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WO2023073450A1 - Engineering of steady topology-controlled nanofibrous structures based on tissue engineering perspective - Google Patents

Engineering of steady topology-controlled nanofibrous structures based on tissue engineering perspective Download PDF

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Publication number
WO2023073450A1
WO2023073450A1 PCT/IB2022/058799 IB2022058799W WO2023073450A1 WO 2023073450 A1 WO2023073450 A1 WO 2023073450A1 IB 2022058799 W IB2022058799 W IB 2022058799W WO 2023073450 A1 WO2023073450 A1 WO 2023073450A1
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exemplary
carbon
nanostructures
substrate
forming
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French (fr)
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Roya Dastjerdi
Zohreh JAFARI VELDANI
Ali Mohammad BAZARGAN
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F2/00Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
    • A61F2/02Prostheses implantable into the body
    • A61F2/28Bones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61FFILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS
    • A61F2/00Filters implantable into blood vessels; Prostheses, i.e. artificial substitutes or replacements for parts of the body; Appliances for connecting them with the body; Devices providing patency to, or preventing collapsing of, tubular structures of the body, e.g. stents
    • A61F2/02Prostheses implantable into the body
    • A61F2/28Bones
    • A61F2002/2835Bone graft implants for filling a bony defect or an endoprosthesis cavity, e.g. by synthetic material or biological material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites

Definitions

  • the present disclosure generally relates to a method for controlling topology of carbon- rich nanostructures, and more particularly, relates to a method for forming and processing an integrated fused carbon-containing fibrous network using thermoplastic connections.
  • Bones are organs of a body which are made of living tissues. Bones are made of calcium salts deposited around protein fibers and can provide a structural support for a living body. Cancellous structure of bones can provide cell migration inside bones and guarantee their viability. Minerals used in cancellous structure of bones can provide rigidity and proteins such as collagen can provide strength and also elasticity of bones. Some diseases associated with bones, like osteonecrosis or cancer can deteriorate bones. Therefore, involved patients may require bone graft. Cancellous bone has an amazing structure with many known and certainly yet unknown mysterious features. Since morphology and topology of a cancellous bone can be detected by cells and mainly effect their behavior, developing cancellous bone-like nanostructure can be a great help especially for hard tissue engineering.
  • Nanofibrous structures suffer from drawbacks such as shrinkage, swelling, and deformation of nanofibrous structures.
  • drawbacks can block pores inside a cancellous structure of bones which can limit cell growth only on a surface of bones. Therefore, a core section of bones may suffer from weakness.
  • fixing topology of fibrous nanostructures via increasing carbon content may be considered to prevent shrinkage, swelling, deformation, etc.
  • engineering topology of a carbon nanostructure especially via a scalable, cost-effective technique, and affordable for public is a great challenge.
  • Li-Heng Kao et al. presented a paper on “Electrospun hierarchical cancellous-bone- like microstructures composed of a crystalline TiO nanonet” vol 82, 2012, 64-66.
  • Li-Heng Kao et al. used titanium dioxide (TiCh) nanoparticles, polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), and titanium isopropoxide (TTIP) in acetic acid and ethanol media to form an electrospinning solution.
  • Li-Heng Kao et al. also used silicate mold to produce bonelike nanostructures. They used a solution of NaOH to dissolve and remove the template.
  • the present disclosure is directed to a method for forming at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bonetissue like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fishlike nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof.
  • an exemplary method may include functionalizing a substrate, forming a plurality of carbon-containing fibers on an exemplary substrate using a mixture containing a carbon fiber precursor, forming a two or multi-phase structure, forming a nanostructured network, and increasing carbon content of an exemplary nanostructured network.
  • an exemplary method may include functionalizing an exemplary substrate by at least one of adding a layer of a resin on an exemplary substrate, adding a layer of at least one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of an electrically conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof.
  • an exemplary method may include forming a two or multi -phase structure by adding at least one thermoplastic material to an exemplary plurality of carbon- containing fibers.
  • an exemplary at least one thermoplastic material may have a melting point below 450 °C.
  • an exemplary method may include forming a nanostructured network by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers.
  • forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon- containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450 °C.
  • an exemplary nano structured network may include a plurality of carbon-containing fibers connected to each other via an exemplary plurality of thermoplastic connections.
  • an exemplary method may include forming a carbon-rich nanostructure by increasing carbon content of an exemplary nanostructured network via removing at least one non-carbon containing element in form of gases from an exemplary nano structured network.
  • removing an exemplary at least one non-carbon containing element may include heating an exemplary nanostructured network to a temperature of 800 °C or more under an inert atmosphere.
  • an exemplary method may include adding an additive to an exemplary carbon-rich nanostructure by coating a layer of an exemplary additive with a thickness up to 1 mm on an exemplary carbon-rich nanostructure.
  • an exemplary additive may include at least one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, an electrolyte, and combinations thereof.
  • an exemplary method may include forming a plurality of carbon-containing fibers using a mixture containing a carbon fiber precursor, forming a two or multi-phase system, forming a nanostructured network, and increasing carbon content of the nano structured network.
  • an exemplary method may include forming a two or multi-phase system by adding at least one thermoplastic material to an exemplary plurality of carbon-containing fibers.
  • an exemplary thermoplastic material may have a melting point below 450 °C.
  • an exemplary method may include forming a nano structured network by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers.
  • forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon-containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450 °C.
  • an exemplary nanostructured network may include a plurality of carbon- containing fibers connected to each other via an exemplary plurality of thermoplastic connections.
  • an exemplary method may include increasing carbon content of an exemplary nano structured network by removing at least one non-carbon containing element in form of gases from an exemplary nanostructured network.
  • removing an exemplary at least one non-carbon containing element may include heating an exemplary nanostructured network to a temperature of at least 800 °C under an inert atmosphere.
  • controlling an exemplary topology of an exemplary carbon-rich nanostructures may include forming one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharpfold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof.
  • an exemplary carbon fiber precursor may include at least one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, and combinations thereof.
  • forming an exemplary plurality of carbon-containing fibers may include forming an exemplary plurality of carbon-containing fibers utilizing a process including at least one of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet- electrospinning, wet or gel electrospinning, and combinations thereof.
  • an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, a poly(amidoamine) (PAMAM), a silicone, a silicone compound, a poysiloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, and combinations thereof.
  • PVA polyvinyl alcohol
  • PVP polyvinylpyrrolidone
  • PEG polyethylene glycol
  • hydrogel polyethylene oxide
  • PEO polyethylene oxide
  • acrylic acid an acrylic acid derivatives
  • an acrylate an acrylic acid derivatives
  • polyester a polyamide
  • PA polyamide
  • adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers may include at least one of adding an exemplary at least one thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers after forming an exemplary plurality of carbon- containing fibers, and combinations thereof.
  • adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process including at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) elctro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented- nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electrocentrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning,
  • heating an exemplary two or multi-phase structure to a temperature up to 450°C may include heating an exemplary two or multi-phase structure to an exemplary temperature up to 450°C under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof.
  • an exemplary inert gas may include at least one noble gas.
  • forming an exemplary plurality of carbon-containing fibers may include forming an exemplary plurality of carbon-containing fibers on a substrate.
  • an exemplary substrate may include at least one of a fabric, a layer, a film, a paper, a sheet, a lace, a web, and combination thereof of a heat resistant material, a carbon-forming material, a graphite-forming material, a carbon/ graphite-forming material, a substrate may be configured to be separated from an exemplary nanostructured network before a heating process to a temperature above 200°C, and combinations thereof.
  • an exemplary substrate may include at least one of a carbon fabric, a micro-carbon fabric, a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a layer of polysaccharide derivatives, lignin, lignocellulose, a carbohydrates, a carbohydrate derivatives, polyacrylonitriles, a metal sheet, a layer of mercerized cellulose, polyester laces, and combinations thereof.
  • forming an exemplary plurality of carbon-containing fibers may further include functionalizing an exemplary substrate by at least one of adding a layer of a resin on an exemplary substrate, adding a layer of an exemplary at least one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of a conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof.
  • an exemplary plurality of nanostructures may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO) a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPS ).
  • Si Silicon
  • B Boron
  • LDHs layered double hydroxides
  • an exemplary plurality of nanostructures may include at least one of a hydroxide, a salt, a composite, an oxide, a framework, and combinations thereof may include at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), chalcogenides, molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof.
  • an exemplary resin may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, a carbohydrates, a polysaccharide, a carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), an acrylic resin, a silicone, a polysiloxane, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, hydrogels, acrylates, poly(sodium acrylate), a polyimide, poly(amidoamine) (PAMAMs), polyaniline, polysiloxane derivatives, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures,
  • PEG polyvinylpyr
  • an exemplary method may further include adding an additive to at least one of an exemplary mixture containing a carbon fiber precursor, an exemplary thermoplastic material, an exemplary carbon-rich nanostructure, and combination thereof.
  • an exemplary additive may include at least one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, a hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, BETS metal compounds, an electrolyte, and combinations thereof.
  • an exemplary additive may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, carbohydrates, polysaccharide, carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), acrylic resins, silicones, poly siloxanes, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, a hydrogels, acrylates, poly(sodium acrylate), polyimides, a poly(amidoamine) (PAMAMs), a polyaniline, polysiloxane derivatives proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials
  • Strontium stannate SrSnos. Tungsten ditelluride (WTe2), Potassium heptafluorotantalate (K ⁇ TaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBi), Niobium disulfide (NbSi), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Lead (Pb), Iridium (Ir), Cobalt (Co), Nickel (Ni), Vanadium (V), tungsten (W), Tin (Sn), molybdenum (Mo), tellurium (Te), niobium (Nb), iron (Fe), palladium (Pd), strontium (Sr), an oxide of at least one of Cu, Zn, Fe, Mn, Ti, Mg, Mo, Si, chalcogenides, a salt comprising at least one of chalcogenides, Ag,
  • an exemplary nanostructured additive may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO) a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPS ).
  • Si Silicon
  • B Phosphorus
  • LDHs layered double hydroxides
  • MXenes carbon nano
  • an exemplary method may further include at least one of washing an exemplary carbon-rich nanostructure with at least one of an organic solvent, an aqueous solution, and combination thereof, washing an exemplary plurality of carbon- containing fibers with at least one of an organic solvent, an aqueous solution, and combination thereof, washing an exemplary nanostructured network with at least one of an organic solvent, an aqueous solution, and combination thereof, purification at least one of an exemplary carbon- rich nanostructure, an exemplary plurality of carbon-containing fibers, an exemplary nanostructured network, and combinations thereof using at least one of an acid solution, a basic solution, an oxidant solution, an organic solution, and combination thereof, in-situ synthesis of a nanostructured additive using at least one of a hydrothermal process, a solvothermal process, a chemical reduction/oxidation, irradiation, a thermal process, and combination thereof, eliminating a component before or after forming an exemplary nanostructured network using at least one of
  • an exemplary carbon-rich nanostructures may include one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially- carbon-rich nanocomposite, and combination thereof.
  • FIG. 1A illustrates a flowchart of a method for controlling topology of carbon-rich nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. IB illustrates a flowchart of a method for controlling topology of carbon-rich nanostructures using a substrate, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 2A illustrates a field emission scanning electron microscopy (FESEM) image of intertwined woven-like nanocomposite nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 2B illustrates a magnified FESEM image of exemplary intertwined woven-like nanocomposite nanostructures shown in FIG. 2A, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 3A illustrates a FESEM image of exemplary dome-shaped intertwined woven- like nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG.3B illustrates a magnified FESEM image of exemplary dome-shaped intertwined woven-like nanostructures shown in FIG. 3A, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 4 illustrates a scanning electron microscopy (SEM) image of exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 5 illustrates an Energy-dispersive X-ray spectroscopy (EDX) diagram for exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 6 illustrates a SEM image of exemplary bone tissue-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 7A illustrates Fourier transform infrared (FTIR) -attenuated total reflection (ATR) (FTIR-ATR) spectrums of exemplary electrospun fibers and nanocomposites after an exemplary fixing and refining process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 7B illustrates FTIR-ATR spectrums of exemplary electrospun bone tissue-like nanostructures before forming an exemplary integrated fused network and after an exemplary fixing process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 8 illustrates a thermogravimetric analysis (TGA) spectrum after an exemplary fixing process in form of carbon nanostructures for exemplary bone tissue-like nanostructure, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 9 illustrates a Raman spectroscopy spectrum for exemplary bone tissue-like nanostructure after an exemplary fixing process in form of carbon, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 10 illustrates a SEM image of a micro carbon fabric substrate modified by clay nano layers, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 11 illustrates a SEM image of an exemplary functionalized micro carbon fabric modified with inorganic nanoparticles and resins, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 12 illustrates a SEM image of exemplary functionalized micro carbon fabric modified with clay nano layers and resins, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 13 illustrates a SEM image of exemplary bone tissue-like nanostructures formed on an exemplary functionalized substrate, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 14 illustrates a SEM image of an exemplary quantum-size fibrous pattern formed on graphitic cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 15 illustrates a SEM image of exemplary fish-like patterns developed on a micro carbon fabric, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 16 illustrates a SEM image of exemplary multiaxial intertwined woven-like nanostructures formed on a circular/radial-patterned substrate, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 17 illustrates a SEM image of exemplary nanoflowers with a carbon shell developed on graphitic cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 18 illustrates a SEM image of exemplary rose-shaped nanostructures, consistent with one or more exemplary embodiments of the present disclosure
  • FIG. 19 illustrates SEM images of exemplary cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 20 illustrates a SEM image of cell attachment on exemplary produced nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • an exemplary topology of an exemplary carbon-rich nanostructures may be controlled by selection of appropriate production/processing parameters and compounds used for producing an exemplary carbon-rich nanostructures.
  • carbon-rich nanostructures refers to compositions containing high percent of at least one of carbon, graphite, graphite/carbon and combinations thereof.
  • Carbon-rich nanostructures may also refer to a carbon-rich nanocomposite.
  • an exemplary carbon-rich component in a carbon-rich nanocomposite may refer to a composition containing high percent of at least one of carbon, graphite, graphite/carbon and combinations thereof.
  • carbon-rich nanostructures may be formed by forming a plurality of carbon-containing structures on a substrate, forming a two or multi-phase system by adding at least one meltable material at temperatures below about 450 °C to exemplary plurality of carbon-containing structures, forming a nanostructured network by melting an exemplary meltable material among exemplary plurality of carbon-containing structures, and increasing carbon content of an exemplary nanostructured network.
  • an exemplary meltable material may include a thermoplastic material.
  • an exemplary plurality of carbon-containing structures may include a plurality of carbon-containing fibers.
  • exemplary carbon-rich nanostructures may include at least one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially-carbon-rich nanocomposite, and combination thereof.
  • exemplary carbon- rich nanostructures may have a convoluted, wavy, spiral, porous, intertwined, angled, branched, networked (integrated network), fibrous, hollow, patterned of nano, micro, meso, and quantum sized structures.
  • exemplary carbon -rich nanostructures may include at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopatterned carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof.
  • exemplary carbon- rich nanostructures may include at least one of woven-like carbon-rich nanocomposite nanostructures, bone-like carbon-rich nanocomposite nanostructures, bone-tissue like carbon- rich nanocomposite nanostructure, multiaxial intertwined woven-like nanocomposite nanostructures, fish-like nanopatterned carbon-rich nanocomposites, dome-shaped intertwined woven-like nanocomposite nanostructures, quantum size fibrous nanocomposite nanostructures, sharp-fold controlled-topology nanocomposite nanostructures, hollow sphere bone-tissue like shell nanocomposites, multi-scaled multilayer micro, nano, meso, quantum sized structures, multi-scaled multilayer nanocomposite, nano-curvature graphitic structures with twisted layers, nano-waved graphitic structures with twisted layers, nano-curvature graphitic integrated network nanocomposites with twisted layers, and nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted layers
  • forming exemplary carbon-rich nanostructures may include forming a plurality of carbon-containing structures.
  • an exemplary carbon containing structure may include a plurality of carbon-containing fibers.
  • forming an exemplary plurality of carbon-containing fibers may be performed by a process including at least one of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel electrospinning, and combinations thereof.
  • an exemplary plurality of carbon-containing fibers may include one of nano, micro, and multiple scaled fibers.
  • one carbon-rich precursor may be used to form an exemplary plurality of carbon-containing fibers.
  • an exemplary carbon-rich precursor may include one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, and combinations thereof.
  • an exemplary polysaccharide may include one of N-[(2-hydroxy-3- trimethyl ammonium) propyl] chitosan (HTCC), lignin, etc., and combinations thereof.
  • Carbohydrates may refer to materials with a molecular structure of carbon, oxygen, and hydrogen where molecular formula of carbohydrates may usually be modeled as C m (H2O)n, like glucose, maltose, mono, oligo or poly saccharides, etc.
  • exemplary carbohydrates may include at least one of glucose amine, chitosan, chitin, alginate, heparin, and combinations thereof.
  • carbohydrate may include synthetic derivatives and natural derivatives of carbohydrates and impure carbohydrates.
  • Saccharides may be the most abundant carbohydrates in nature and in biomolecules (e.g. plants), etc.
  • exemplary natural sources of saccharides or polysaccharides may include starch, cellulose, cotton, glycogens, etc.
  • saccharide may also refer to processed or impure saccharide materials, synthetic saccharide derivatives, and their natural derivatives.
  • an exemplary carbon-containing structure may be formed on a substrate.
  • an exemplary substrate may interact with an exemplary plurality of carbon-containing structures.
  • a heat-compatible substrate may be used.
  • an exemplary heat-compatible substrate may include at least one of heat and shrinkage resistant materials (e.g. a carbon fabric, a micro-carbon fabric, glass fabrics, etc.), a carbon, a graphite-, a carbon/ graphite-forming material and combinations thereof.
  • an exemplary substrate may interact with an exemplary plurality of carbon-containing fibers.
  • an exemplary substrate may include one of acrylic substrates (including polyacrylonitrile and its derivatives, modacrylics, etc.), polysaccharide and mercerized cellulose substrates, such as cotton, viscose, lignin, and lignocellulose, a film of graphene oxide (GO) nano layers/fibers, carbon substrate including fiber and carbon fabric with any biaxial, uniaxial, multiaxial, micro, nano, etc. structure, and their combinations, any forms of fabric, film, paper, lace, etc., in simple, patterned, printed, embossed, etc., which can be combined with an exemplary carbon-containing structure.
  • acrylic substrates including polyacrylonitrile and its derivatives, modacrylics, etc.
  • polysaccharide and mercerized cellulose substrates such as cotton, viscose, lignin, and lignocellulose
  • GO graphene oxide
  • carbon substrate including fiber and carbon fabric with any biaxial, uniaxial, multiaxial, micro, nano, etc. structure,
  • an exemplary substrate with an exemplary carbon-containing structure thereon may be subjected to a thermal procedure.
  • an exemplary interaction of an exemplary substrate with an exemplary plurality of carbon-containing fibers may be in form of physical contact, friction with an exemplary plurality of carbon-containing fibers or a stronger conflict.
  • an exemplary substrate may be functionalized before forming an exemplary plurality of carbon-containing structures on an exemplary substrate.
  • functionalizing a substrate may be designed so that a smart selfactivated micro dynamic control mechanism via nanorough friction and/or resin attachment may be created (added) on an exemplary substrate.
  • a heat-compatible substrate may be used to achieve microdynamic control on thermal shrinkage, topology, and morphology of exemplary carbon- rich nanostructures.
  • an exemplary heat-compatible substrate may include one of a fabric, layer, film, paper, sheet, lace, web, and combinations thereof.
  • an exemplary heat-compatible substrate may include one of a heat resistant material, carbon material, graphite-forming material, carbon/ graphite-forming material, and combinations thereof.
  • an exemplary heat resistant material may include at last one of a carbon fabric, a micro-carbon fabric, a glass fabric, and combinations thereof.
  • an exemplary carbon/ graphite-forming material may include at least one of a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a polysaccharide derivative, lignin, lignocellulose, carbohydrates, carbohydrate derivatives, polyacrylonitriles, a film of graphene oxide (GO), and combinations thereof.
  • an exemplary substrate may include one of a carbon fabric, a micro-carbon fabric, a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a layer of polysaccharide derivatives, lignin, lignocellulose, a carbohydrate, a carbohydrate derivative, polyacrylonitriles, a metal sheet, a layer of mercerized cellulose, polyester laces, and combinations thereof.
  • an exemplary substrate may be functionalized by one of adding a layer of a resin on an exemplary substrate, adding a layer of one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of an electrically conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof.
  • an exemplary nano roughness resulting from coatings created with inorganic nanostructures may be considered to create nano roughness (friction) and use an exemplary friction to control movement, shrinkage, and also keep an exemplary plurality of carbon-containing nanofibers at certain places and prevent them from sticking and uncontrolled clumping. Therefore, an exemplary nano roughness may help to create curves, special spaces between curves, applying tension by dealing with thermal shrinkage microdynamically during an exemplary heating process to increase an exemplary arrangement of chains, etc., and an exemplary guidance of topology and morphology of an exemplary plurality of nano fibers.
  • use of resins and applying changes in thermal processes may also help to control topology of an exemplary plurality of carbon-containing nanofibers.
  • a melting component or a thermoplastic material can also be included during an exemplary thermal process to exemplary carbon-containing nanofibers.
  • the present disclosure may also directed to exemplary dynamic and microdynamic methods of controlling thermal shrinkage of an exemplary plurality of carbon-containing nanofibers as well as thermal processes in nano and atomic scale.
  • a resin may be used for functionalizing an exemplary substrate where an exemplary resin may activate an exemplary microdynamic mechanism at different stages of an exemplary thermal process by intelligently fusing an exemplary carbon-containing nanofibers to surface of an exemplary substrate.
  • an exemplary carbon-containing nanofibers may increase with increasing temperature.
  • a combination of three fusing mechanisms including fusing in nano scale or larger, nano friction and roughness as well as nano fiber entanglement in nanometer spaces between nano structures can be considered together.
  • adding magnetic/nanomagnetic materials on an exemplary substrate may form magnetic/nanomagnetic patterns.
  • magnetic/nanomagnetic patterns formed on an exemplary substrate, etc. may provide a possibility of using magnetic forces to guide and control topology of an exemplary plurality of carbon-containing nanofibers.
  • functionalizing an exemplary substrate with magnetic/nanomagnetic patterns may further include adding magnetic/nanomagnetic materials to an exemplary substrate.
  • exemplary magnetic/nanomagnetic patterns may also be used to control the morphology of an exemplary plurality of carbon- containing nanofibers.
  • an exemplary substrate may be separated from an exemplary plurality of carbon-containing nanofibers or may be processed along with an exemplary plurality of carbon-containing nanofibers.
  • an exemplary plurality of nanostructures added to an exemplary substrate may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphenebased materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPSy).
  • Si Silicon
  • B Boron
  • LDHs layered double hydroxides
  • Strontium stannate SrSnos
  • WTc Tungsten ditelluride
  • KiTaF? Potassium heptafluorotantalate
  • WS2 Tungsten disulfide
  • MgEb magnesium diboride
  • NbSs Niobium disulfide
  • Silver Ag
  • Copper Cu
  • Zinc Zinc
  • Titanium Ti
  • Platinum Pt
  • Gold Au
  • Tin Tin
  • Lead Pb
  • an exemplary plurality of nanostructures may inlcude at least one of a hyroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), chalcogenides, molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof.
  • an exemplary resin may include one of PEG, polyvinylpyrrolidone (PVP), chitosan, a carbohydrates, a polysaccharide, a carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), an acrylic resin, silicone, a poly siloxane, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, hydrogels, acrylates, poly(sodium acrylate), a polyimide, poly(amidoamine) (PAMAMs), polyaniline, polysiloxane derivatives, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BE
  • functionalizing an exemplary substrate may use smartly self-activated microdynamic control mechanism via nanorough friction and/or resin attachment via functionalizing an exemplary substrate by adding one of a layer of a resin, a layer of an exemplary thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, conductive materials, etching an exemplary surface, and combinations thereof on an exemplary substrate.
  • a two or multi-phase structure may be formed by adding at least one thermoplastic material to an exemplary plurality of carbon-containing fibers.
  • an exemplary thermoplastic material may be added before, after, or during production of an exemplary plurality of carbon-containing fibers.
  • an exemplary thermoplastic material may have a melting point below about 450 °C.
  • an exemplary phase made of an exemplary thermoplastic material may make connection sites among an exemplary plurality of carbon-containing nanofibers when an exemplary thermoplastic material melts at the meeting sites of an exemplary plurality of fibers/nanofiber crossing.
  • an exemplary melted thermoplastic material may form connections between an exemplary plurality of carbon-containing nanofibers.
  • a fusible material instead of or together with an exemplary thermoplastic material, a fusible material may be used.
  • melting point of an exemplary fusible material may be below about 450 °C.
  • an exemplary fusible material may include a salt, a nanostructured salt, for example, zinc chloride or zinc nitrate.
  • an exemplary fusible material may include a metal, for example, zinc.
  • an exemplary fusible material may include an oil, for example, a paraffin in form of an emulsion, a dissolvable capsule, or Phase Change Materials (PCMs).
  • type, composition, and percentage of materials, and production conditions may be selected in such a way that an exemplary thermoplastic or an exemplary thermoplastic material in a mixture of an exemplary plurality of nanofibers may have a tendency to form a two-phase system when an exemplary mixture of an exemplary plurality of nanofibers is subjected to an exemplary selected processing condition after leaving a nozzle in a production procedure of an exemplary two or multi-phase structure.
  • an exemplary thermoplastic material or meltable components or elements of an exemplary thermoplastic or an exemplary meltable components may have a tendency to form a two-phase system or to create a two-phase system after an exemplary thermoplastic material or an exemplary meltable component exit a nozzle.
  • an exemplary two-phase system may be formed due to solvent evaporation and/or exposure of an exemplary thermoplastic material or exemplary meltable components to exemplary exiting forces during electrospinning process (or other procedures) with the conditions selected for an exemplary process of electrospinning, etc. and/or exposure to environmental conditions of the process (such as humidity, etc.).
  • an exemplary formed two/multi-phase system may include some elements of at least one of the thermoplastic and/or the meltable materials and combinations thereof.
  • an exemplary substrate may be separated from an exemplary carbon-containing structure before heating to a temperature above 200°C.
  • an exemplary substrate, including polyester laces, may be separated from an exemplary carbon-containing structure before heating to a temperature above 200°C.
  • adding an exemplary thermoplastic material to an exemplary plurality of carbon-containing fibers may include one of adding an exemplary thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary thermoplastic material to an exemplary substrate, adding an exemplary thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers after forming an exemplary plurality of carbon-containing fibers, and combinations thereof.
  • adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process of at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) electro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electroblowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning,
  • a nanostructured network may be formed by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers.
  • forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon- containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450°C.
  • heating an exemplary two or multi-phase structure to a temperature up to 450°C may include heating an exemplary two or multi-phase structure to an exemplary temperature up to 450°C under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof.
  • an exemplary inert gas may include at least one noble gas.
  • an exemplary two or multiphase structure may be separated from an exemplary substrate when applying a temperature of at least 200°C to an exemplary two or multi-phase structure.
  • an exemplary heating process may result in connecting exemplary carbon-containing fibers to each other, and/or connecting exemplary carbon-containing fibers to an exemplary substrate, and combinations thereof via a plurality of connections made by at least one melted component of an exemplary thermoplastic material.
  • an exemplary nanostructured network may include a plurality of carbon-containing fibers connected to each other via an exemplary plurality of thermoplastic connections.
  • an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, apoly(amidoamine) (PAMAM), a silicone, a silicone compound, a poy siloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, poly or oligo or monoacrylates, nanostructures, salts (such as zinc nitrate), elements (such as zinc), mixtures of mentioned materials above with of at least one of protein compounds, oligomers, co- or tri-polymers, amphiphilics, macromolecules, superstructures, biomaterials, metamaterials, softeners, a carbon
  • each of “polyacrylonitriles”, “polyacrylonitrile”, and “PAN” may refer to copolymers, modacrylics, tripolymers, derivatives thereof, and modified materials based on polyacrylonitriles, polyacrylonitrile, and PAN as well as polyacrylonitriles, polyacrylonitrile, and PAN .
  • adding at least one thermoplastic material and/or a meltable material to an exemplary plurality of an exemplary carbon fiber precursor-containing nanofibers, in a way to form a two/multi phased system may include a plurality of at least one of exemplary thermoplastic material elements and/or a meltable material elements along with an exemplary plurality of at least one of the carbon fiber precursor-containing nanofibers elements.
  • an exemplary thermoplastic material and/or a meltable material may have a melting point below 450 °C.
  • an exemplary nanostructured network may be heated to form a carbon-rich nanostructure.
  • an exemplary process of forming a carbon-rich nanostructure by heating an exemplary nano structured network may include a carbonization process.
  • an exemplary nanostructured network may be separated from an exemplary substrate before an exemplary carbonization process when an exemplary substrate undergo undesirable shape changes during an exemplary carbonization process (such as aluminum, polypropylene, polyester).
  • an exemplary nano structured network may be heated after separating an exemplary nanostructured network from an exemplary substrate/functionalized substrate.
  • an exemplary nanostructured network may be heated in a furnace at a temperature of at least 800°C.
  • carbon content of an exemplary nanostructured network may increase by removing at least one non-carbon containing element in form of gases from an exemplary nanostructured network.
  • removing an exemplary at least one non-carbon containing element may include heating an exemplary nanostructured network to a temperature of at least 800 °C under an inert atmosphere.
  • non-carbon elements such as oxygen, nitrogen, hydrogen, halogens, and combinations thereof may be released from an exemplary nanostructured network in form of gases.
  • exemplary released gases may include at least one of hydrogen cyanide (HCN), (nitrogen) N2, water (H2O), and combinations thereof.
  • heating an exemplary nanostructured network may increase carbon content of an exemplary nanostructured network.
  • an exemplary formed carbon-rich nanostructure may include at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon- rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopatterned carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof.
  • an exemplary carbon-rich nanostructure may include at least one of woven-like carbon-rich nanocomposite nanostructures, bone-like carbon-rich nanocomposite nanostructures, bone-tissue like carbon- rich nanocomposite nanostructure, multiaxial intertwined woven-like nanocomposite nanostructures, fish-like nanopattemed carbon-rich nanocomposites, dome-shaped intertwined woven-like nanocomposite nanostructures, quantum size fibrous nanocomposite nanostructures, sharp-fold controlled-topology nanocomposite nanostructures, hollow sphere bone-tissue like shell nanocomposites, multi-scaled multilayer micro, nano, meso, quantum sized structures, multi-scaled multilayer nanocomposite, nano-curvature graphitic structures with twisted layers, nano-waved graphitic structures with twisted layers, nano-curvature graphitic integrated network nanocomposites with twisted layers, nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted
  • bone-like carbon-rich nanostructures may include one of cancellous bone, trabecular bone, cortical bone, and spongy bone-like carbon-rich nanostructures, and combinations thereof.
  • an exemplary heating process for increasing carbon content may lead to fixing topology of an architecture of an exemplary carbon-rich nanostructure by increasing an exemplary carbon content of an exemplary carbon-rich nanostructure and controlling a balance between expansion and tension of an exemplary carbon-rich nanostructure.
  • controlling a balance between expansion and tension of an exemplary carbon-rich nanostructure may be achieved due to release of gases on exemplary fibers in spaces between exemplary connections and tendency to shrink with increasing temperature and plasticizing effect of exemplary melting components.
  • a thermoplastic material with a melting temperature within a temperature range of an exemplary heating process may melt during an exemplary carbonization process; allowing for simultaneously creating connections in an exemplary structure of exemplary carbon-rich nanostructures and plasticizing an exemplary structure of exemplary carbon-rich nanostructures, especially when more than one type of meltable plasticizing agents is used in an exemplary method.
  • an exemplary method may be an efficient method due to using cost-effective easy-scalable materials and steps based on applying plenty and cheap materials; allowing for providing an affordable product.
  • FIG. 1A illustrates a flowchart of a method 100 for controlling topology of carbon-rich nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • method 100 may include a step 102 of forming a plurality of carbon-containing fibers, a step 104 of forming a two or multi-phase system by adding a thermoplastic material to the plurality of carbon-containing fibers, a step 106 of forming a nanostructured network by heating the two or multi-phase system to a temperature up to 450°C, and a step 108 of forming a carbon-rich nanostructure by increasing carbon content of the nanostructured network by heating the nanostructured network to a temperature of at least 800°C under an inert atmosphere.
  • step 102 of forming a plurality of carbon-containing fibers may include using a carbon fiber precursor for producing an exemplary plurality of carbon-containing fibers.
  • an exemplary carbon fiber precursor may form an exemplary plurality of carbon-containing fibers by at least a method of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel electrospinning, and combinations thereof.
  • an exemplary plurality of carbon- containing fibers may include at least one of nano, micro, and multiple scaled fibers.
  • an exemplary carbon-rich precursor may include at least one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, and combinations thereof.
  • an exemplary carbohydrate may include at least one of sucrose, dextrins, starch, glucose, and combinations thereof.
  • an exemplary polysaccharide may include one of N-[(2-hydroxy-3 -trimethyl ammonium) propyl] chitosan (HTCC), lignin, and combinations thereof.
  • step 104 of forming a two or multi-phase system may include adding a thermoplastic material to an exemplary plurality of carbon-containing fibers.
  • at least one thermoplastic material may be added to an exemplary plurality of carbon-containing fibers.
  • adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers may include at least one of adding an exemplary at least one thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers after forming an exemplary plurality of carbon-containing fibers, and combinations thereof.
  • an exemplary thermoplastic/meltable material may be added to an exemplary carbon fiber precursor with a weight ratio in a range of 0.0005:1 to 10:1 (an exemplary thermoplastic material: carbon fiber precursor).
  • an exemplary thermoplastic material may have a melting point below 450°C.
  • adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process of at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) elctro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centr
  • an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, a poly(amidoamine) (PAMAM), a silicone, a silicone compound, a poysiloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, poly or oligo or monoacrylates, nanostructures, salts (such as zinc nitrate), elements (such as zinc), their mixtures with each other or with other materials, their mixtures with of at least one of protein compounds, oligomers, co- or tri-polymers, amphiphilics, macromolecules, superstructures, biomaterials, metamaterial
  • PAN polysaccharides, lignin, lignocellulose
  • PAN polysaccharides, lignin, lignocellulose
  • a polymer a resin, an oligomer, a macromolecule, a capsule, a dendrimer, a liposome, a micelle, a hybrid, a composite, a nanocomposite, an organic/inorganic compound, and combinations thereof.
  • adding at least one thermoplastic material to an exemplary plurality of an exemplary carbon fiber precursor-containing nanofibers, in a way to form a two/multi phased system may include a plurality of at least one of the thermoplastic material elements along with an exemplary plurality of at least one of the carbon fiber precursor-containing nanofibers elements.
  • step 106 of forming a nano structured network may include heating an exemplary two or multi-phase system to a temperature up to 450°C.
  • an exemplary two or multi-phase system may be heated in a heating device for a time period in a range of 10 minutes to 400 minutes.
  • an exemplary heating device may include a heater, a thermal chamber, for example, an oven, a heater, a furnace, etc.
  • an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof.
  • an exemplary inert gas may include at least one noble gas.
  • an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof.
  • heating an exemplary two or multi-phase system may melt an exemplary thermoplastic material.
  • an exemplary thermoplastic material may have a melting point below 450 °C.
  • exemplary elements of an exemplary thermoplastic material may form connections when they melt at an exemplary meeting points of exemplary nanofibers crossing.
  • an exemplary connection between exemplary carbon-containing fibers may form a nanostructured network.
  • a nanostructured network may be formed by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers.
  • forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon-containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450°C.
  • controlling an exemplary temperature may control topology of an exemplary nanostructured network.
  • important factors for controlling topology of carbon rich nanostructures may include duration of an exemplary process of heating, percentage composition of exemplary components, melting point of each of exemplary components, thermal characteristics of each of exemplary components, number and ratio of thermoplastic materials and/or a meltable material, method of adding each component, proximity and frequency of connections, morphology, fineness and abundance and density of fibers between exemplary connections, characteristics and rheology of molten materials, rate of expansion of an exemplary nano structured network, strengthening factors that may create tension, expansion, or prevent shrinking (when using mechanical, magnetic, nano magnetic, smart nano magnetic, etc.
  • step 108 of increasing carbon content of the nanostructured network may include heating an exemplary nanostructured network to a temperature of at least 800°C.
  • heating an exemplary nanostructured network may form carbon-rich nanostructures.
  • an exemplary carbon-rich nanostructures may include one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially-carbon-rich nanocomposite, and combination thereof.
  • an exemplary nano structured network may be heated in a furnace.
  • an exemplary nano structured network may be heated in a furnace.
  • non-carbon elements such as oxygen, nitrogen, hydrogen, halogens, etc.
  • exemplary gases may include hydrogen cyanide (HCN), (nitrogen) N2, water (H2O), etc.
  • HCN hydrogen cyanide
  • an exemplary non-carbon element composition may depend on an exemplary composition of an exemplary nano structured network and chemical structure of an exemplary nanostructured network.
  • an exemplary furnace may include a gas inlet and a gas outlet.
  • exemplary gases leaving an exemplary heating device may include a neutral gas or a predetermined atmosphere.
  • an exemplary predetermined atmosphere may include noble gases.
  • an exemplary nano structured network may be heated under an inert gas atmosphere.
  • an exemplary inert gas may enter from an exemplary gas inlet and may leave an exemplary furnace from an exemplary gas outlet.
  • an exemplary nanostructured network may be heated under an inert gas atmosphere.
  • an exemplary inert gas may include at least a noble gas and/or a mixture of atmospheres.
  • an exemplary heating process may be applied using air atmospheres with a temperature up to 280 °C-300 °C or a combined atmosphere of 5-50% air atmosphere in combination with inert atmosphere d at a temperature up to 300 °C -350 °C.
  • an exemplary nano structured network may be kept for 5 minutes to 20 minutes at a temperature of 350 °C - 380 °C in a mixed atmosphere containing 5-50% air atmosphere, then the air atmosphere may be replaced with a rate of 2- 20% per minute with inert atmosphere and the temperature may be increased with a rate of 2 °C/min. to 20 °C/min. Then, the process may continue at a temperature higher than 400 °C in a completely inert atmosphere.
  • controlled dosing of exemplary combined atmosphere may allow achieving one of forming integrated fused network (IFN), fixing and refining the topology via increasing carbon content (FRIC) thermal steps, and combinations thereof. Both thermal steps of IFN and FRIC can be followed continuously or separately in form of one integrated thermal process or two/multi separated thermal procedures.
  • each of IFN or FRIC steps can include one, two or more continuous or separate steps of a thermal process.
  • exemplary thermoplastic materials with a melting temperature equal or lower than a temperature of FRIC steps may create a new connection or plasticize an exemplary nano structured network or both at the same time by forming carbon rich nanostructures and conducting topology of an exemplary carbon rich nanostructures.
  • conducting topology of an exemplary carbon rich nanostructures may be enhanced when more than one type of thermoplastic material with different melting temperatures are used in an exemplary method.
  • melting of one or more thermoplastic material may be done in an exemplary FRIC stage as well.
  • a thermoplastic component may completely or partially leave an exemplary carbon rich nanostructure during thermal processes, or a small percentage of an exemplary thermoplastic component may remain or an exemplary thermoplastic component may join an exemplary carbon, graphite or carbon/graphite network along with an exemplary carbon rich nanostructure.
  • an exemplary residue of an exemplary thermoplastic component may be removed in following steps such as washing or purification when an exemplary thermoplastic component are not incorporated in one of exemplary carbon, graphite or carbon/graphite nanostructures or exemplary patterns on an exemplary carbon, graphite or carbon/graphite nanostructures.
  • factors considered during an exemplary method for controlling topology of an exemplary carbon rich nanostructures may include controlling balance between thermal expansion, expansion under pressure of exhaust gases and stress, resulting from exhaust gases, on an exemplary plurality of fibers in distances between connections, plasticizing effect of exemplary melting components, tendency to shrinkage with increasing temperature and the type, structure and mechanism of functionalizing an exemplary substrate and thermal and rheological behavior of an exemplary substrate, etc.
  • parameters effecting an exemplary topology of an exemplary carbon rich nanostructure may include one of rate of temperature increase, final temperature, process duration, percentage composition of components, melting point of each component, thermal characteristics of each of exemplary components, number and ratio of exemplary thermoplastic materials, mechanism of adding each component, closeness and frequency of connections, morphology, size (diameter), frequency, density of fibers between connections, rheological properties of molten materials and additives, rheological properties of carbon-containing fibers such as stretchability, extension, modulus, elasticity, and composition of additives, as well as geometry of nanostructures on exemplary carbon-containing fibers, rheological properties of nanocomposites, such as the effect of nanostructures on elasticity, modulus, extension, The rate of gas release, strengthening factors that expand and create tension, or prevent shrinking using mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic and smart microdynamic systems, etc.
  • an exemplary method for controlling tension may work using mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic, thermomicrodynamic, and smart microdynamic methods, etc. and combinations thereof.
  • an exemplary carbon-rich nanostructures may have a convoluted, wavy, spiral, porous, intertwined, angled, branched, networked (integrated network), fibrous, hollow, patterned of nano, micro, meso and quantum sized structures.
  • controlling an exemplary topology of an exemplary carbon-rich nanostructures may include forming at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, nano-curvature graphitic integrated network nanocomposites/nanostructures with twisted layers, nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted layers, and combinations thereof.
  • an additive may be added to at least one of an exemplary mixture containing one of a carbon fiber precursor, an exemplary thermoplastic material, an exemplary carbon-rich nanostructure, and combinations thereof.
  • a layer of an exemplary additive may be formed on an exemplary carbon-rich nanostructures.
  • an exemplary additive may have a thickness of up to 1 mm.
  • an exemplary additive may include one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a surfactant, a catalyst, a hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, BETS, hyroxides, salts, composites, nanostructures of exemplary additives, frameworks of exemplary additives, and combinations thereof.
  • an exemplary additive may include at least one of polyethylene glycol (PEG), polyvinylpyrrolidone (PVP), chitosan, carbohydrates, polysaccharide, carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), acrylic resins, silicones, polysiloxanes, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, a hydrogels, acrylates, poly(sodium acrylate), polyimides, a poly( amidoamine) (PAMAMs), a polyaniline, polysiloxanes, proteins, monomers of exemplary polymers, oligomers, co- or tripolymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials,
  • PEG poly
  • an exemplary nanostructured additive may include at least one of a Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPSa).
  • Si Silicon
  • B Boron
  • Phosphorus P
  • clays hydroxyapatite
  • nanostructured additives may also include one of metals such as Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B).
  • metals such as Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B).
  • a metal oxide or a metal hydroxide such as Titanium dioxide (TiO ).
  • CNT carbon nanofibres
  • CNFs carbon nanofibres
  • fullerene graphene
  • graphene oxide reduced graphene oxide
  • rGO reduced graphene oxide
  • MOFs metal compounds
  • organic/inorganic nanostructures in which the organic component may be one of anhydrides e.g., one of anhydrides
  • maleic anhydride acrylic acid, n-methylols, carbamides, acrylic resins, silicones, poly siloxanes, polyurethanes, aldehydes, PVA, PA, polyols, polyoxides, polyesters, proteins, polycarbonates, polystyrenes, polysaccharides, carbohydrates, poly electrolytes, hydrogels, poly(sodium acrylate), polyimides, PAMAMs, polyaniline, polyvinyls, PVdF, their monomers, ammonias, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, electrolytes, MOFs, drugs, dyes, softeners, antistatic, flame-retardants, etc. derivatives of exemplary additives, mixtures of exemplary additives, co- or tri-polymers of exemplary additives, and combinations thereof.
  • forming an exemplary carbon-rich nanostructures may include intermediate processes such as washing, purification, removal of some components, in-situ synthesis, irradiation, coating, loading additives in the form of combined and sequential processes, etc.
  • washing and purification may be performed due to removing some components, creating porosity, etc.
  • an exemplary carbon-rich nanostructure may be washed with at least one of an organic solvent, an aqueous solution, and combination thereof.
  • an exemplary washing process may be performed via one, two or frequent immersing, dipping, centrifuging steps, in one of an organic solvent, an acid solution, an alkaline solution, an oxidant solution, an enzyme solution, a surfactant solution, a reducing agent solution, an ionic solvent, aqueous solutions, water, and combinations thereof.
  • an exemplary washing process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc. and combinations thereof.
  • an exemplary plurality of carbon-containing fibers may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof.
  • an exemplary nano structured network may be washed with at least one of an organic solvent, an aqueous solution, and combination thereof.
  • at least one of an exemplary carbon-rich nanostructure, an exemplary plurality of carbon-containing fibers, an exemplary nano structured network, and combinations thereof may be purified using at least one of an acid solution, a basic solution, an oxidant solution, an organic solution, and combinations thereof.
  • an exemplary purifying process may include a heating process.
  • an exemplary heating process may be performed in a furnace.
  • an exemplary purifying process may be used for eliminating/reducing dust and impurity of air, environment, and/or undesirable residue /impurity from the procedures, etc., and/or for activation, increasing specific surface area, refining the morphology of an exemplary carbon rich nanostructure, mending defects, covering defects, functionalization, etc.
  • an exemplary purifying process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc., and combinations thereof.
  • an exemplary nanostructured additive may be in-situ synthesized using at least one of a hydrothermal process, a solvothermal process, a chemical reduction/oxidation, irradiation, a thermal process, and combinations thereof.
  • a component may be eliminated before or after forming an exemplary nanostructured network using at least one of an organic solvent, an acid solution, a basic solution, an oxidant solution, water, and combinations thereof.
  • an exemplary component may depend on an exemplary carbon containing precursor, an exemplary thermoplastic material, additives, etc.
  • additives may be added for reinforcement of an exemplary carbon-rich nanostructure, for forming a porous structure, or for synergistic effects, covering defects, improving properties of an exemplary carbon rich nanostructure, improving performance of an exemplary carbon rich nanostructure, surface modifications of an exemplary carbon rich nanostructure, adding a roughness, nano roughness, modifying thermal, rheological, mechanical, tensile properties during or after an exemplary process, forming a composite, nanostructure, superstructure, a metamaterial, a heterostructure, surface modification, conducting fiber morphology, conducting IFN or FRIC adding a feature on an exemplary substrate, achieving a smart, a multi-functional, a multi targeted feature, and combinations thereof, adding a nano, meso, quantum size feature, jagged morphology, increasing the leaving gas volume flow rate, porosity, etc., and combinations thereof.
  • an exemplary IFN or FRIC steps may include designing smart self-activated topology control mechanisms.
  • forming an exemplary smart feature on an exemplary substrate may be used for smart multi-purpose drug delivery, multi targeted drug delivery and cell attachment, bone cement, injectable gel reinforcement, etc.
  • an exemplary eliminated component during an exemplary washing or purification process may include one of exemplary additives e.g. a salt, a softener, an electrolyte, a thermoplastic component, a hydrogel, a resin, a nanostructure, a metal, etc., a byproduct, a precursor or intermediates of an in-situ synthesis, an impurity, an attached substrate which may be designed to be detached before thermal and/or an intermediate process, refining content of a component for special purposes, component which may not be proper or designed to remain during thermal process, creating porosity, hollow fibers, hollow structures, etc.
  • an exemplary byproduct maybe achieved from an in situ synthesis process.
  • an exemplary special purpose may include an additive and/or a thermoplastic and/or a meltable material may be set to achieve an especial morphology through an exemplary carbon-containing fiber production or processing, but an exemplary additive and/or a thermoplastic and/or a meltable content material may be partially or completely removed according to approaches set through a thermal process.
  • FIG. IB illustrates a flowchart of a method 110 for controlling topology of carbon-rich nanostructures using a substrate, consistent with one or more exemplary embodiments of the present disclosure.
  • method 110 may include a step 101 of functionalizing a substrate, a step 102 of forming a plurality of carbon-containing fibers on the functionalized substrate, a step 104 of forming a two or multi-phase system by adding a thermoplastic material to the plurality of carbon-containing fibers, a step 106 of forming a nanostructured network by heating the two or multi-phase system to a temperature up to 450°C, and a step 108 of forming a carbon-rich nanostructure by increasing carbon content of the nanostructured network by heating the nanostructured network to a temperature of at least 800°C under an inert atmosphere.
  • step 101 of functionalizing a substrate may include at least one of forming a rough surface on a substrate, form chemical functional groups on a substrate, and combinations thereof.
  • functionalizing an exemplary substrate may include forming a thermoplastic pattern, a layer of an exemplary thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, electrically conductive materials, etching an exemplary surface, and combinations thereof.
  • a microdynamic control on thermal shrinkage, topology and morphology may be applied via using a heat-compatible substrate at least one of fabric, layer, film, paper, sheet, lace, web, and combinations thereof comprising at least a heat resistant material, a carbon, a graphite, a carbon/graphite-forming material.
  • an exemplary substrate may be designed to be separated before exemplary thermal procedures above 200°C.
  • an exemplary substrate may be made of polyester laces.
  • an exemplary heat resistant material may include carbon fabric, a micro-carbon fabric.
  • an exemplary carbon/graphite-forming material may include cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a polysaccharide derivatives, lignin, lignocellulose, carbohydrates, carbohydrate derivatives, polyacrylonitriles, and combinations thereof.
  • a smart selfactivated microdynamic control mechanism via nanorough friction and/or resin attachment may be devised via functionalizing an exemplary substrate by adding one of a layer of a resin, a layer of an exemplary thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, conductive materials, etching the surface, and combinations thereof on an exemplary substrate.
  • an exemplary functionalized substrate may be designed to undergo an exemplary fixing and refining the topology via increasing carbon content (FRIC) with integrated fused nano structured network of two/multi-phase system and/or designed to undergo through forming integrated fused network (IFN) of two/multi-phase systems.
  • FRIC increasing carbon content
  • IFN integrated fused network
  • an exemplary substrate may be a heat and/or shrinkage resistant substrate, for example, a carbon fabric substrate, glass fabric, etc.
  • an exemplary substrate may be a heat compatible substrate, for example, a carbon- forming material, a graphite-forming material, a carbon/ graphite-forming material.
  • an exemplary plurality of carbon-containing fibers may pass through exemplary thermal treatments (IFN and FRIC) with/without an exemplary functionalized heat resistant substrate.
  • exemplary thermoplastic and/or meltable materials with melting points equal or lower than the temperatures of IFN and FRIC steps may melt and an exemplary plurality of carbon-containing fibers may fuse to an exemplary substrate, functionalized heat resistant, compatible substrate, and/or each other at the connection sites.
  • fused sites may keep an exemplary structure from shrinkage.
  • an exemplary mechanism of forming connections and controlling topology of nanostructures may be smartly self-activated just when an exemplary temperature increase may lead to thermal shrinkage of exemplary structures of exemplary carbon containing fibers or an exemplary nanostructured network.
  • an exemplary mechanism may work more efficient by using a heat and shrinkage resistant substrate.
  • temperature designed for this self-activation mechanism may be controlled by designing exemplary thermoplastic materials and/or exemplary meltable compositions.
  • one, two or multi meltable compositions may be used.
  • an exemplary functionalized substrate may be designed to undergo through one of a fixing and refining the topology via increasing carbon content (FRIC) step with integrated fused nano structured network of two/multi-phase system, designed to undergo through forming integrated fused network (IFN) step of the two/multi-phase system, and/or combinations thereof.
  • an exemplary functionalized substrate may be a heat and/or shrinkage resistant substrate, for example, a carbon fabric substrate, glass fabric, etc.
  • an exemplary functionalized substrate may be a heat compatible substrate, for example, a carbon-forming material, a graphite-forming material, and a carbon/ graphite-forming material.
  • an exemplary thermoplastic and/or meltable materials which melting points of exemplary thermoplastic and/or meltable materials be equal or lower than the temperatures of IFN and FRIOC steps may melt and an exemplary plurality of fibers may fuse to an exemplary substrate and/or each other at the connection sites.
  • fused sites may keep an exemplary structure from shrinkage.
  • an exemplary mechanism may be smartly self-activated just when exemplary structures may be subjected to a thermal shrinkage by increasing temperature.
  • an exemplary mechanism may work more efficient by using an exemplary heat and shrinkage resistant substrate.
  • temperature designed for an exemplary self-activation mechanism may be controlled by designing exemplary thermoplastic materials and/or meltable compositions.
  • one, two or more meltable compositions may be used.
  • effective friction and entanglement of an exemplary network of an exemplary plurality of carbon- containing nanofibers in roughness between exemplary nanostructures may prevent shrinkage of an exemplary network of an exemplary plurality of carbon-containing nanofibers.
  • shrinkage resistance may cause tension and chain alignment and also may boost formation of graphite structures.
  • an exemplary simultaneous fusing of fibers to an exemplary substrate may also have a synergistic effect.
  • an exemplary substrate may include at least one of a fabric, a layer, a film, a paper, a sheet, a lace, a web, and combinations thereof.
  • an exemplary substrate may be made of at least a heat resistant material, a carbon- forming material, a graphite -forming material, and a carbon/ graphite-forming material.
  • an exemplary substrate may be configured to be separated from an exemplary nano structured network before a heating process above 200°C.
  • an exemplary substrate may include at least one of a carbon fabric, a micro- carbon fabric, a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a layer of polysaccharide derivatives, lignin, lignocellulose, a carbohydrates, a carbohydrate derivatives, polyacrylonitriles, a metal sheet, a layer of mercerized cellulose, polyester laces, and combinations thereof.
  • functionalizing an exemplary substrate may include at least one of adding a layer of a resin on an exemplary substrate, adding a layer of an exemplary at least one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of an electrically conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof.
  • one of a substrate, a surface layer, and a sandwich in form of magnetic fibers or patterns with or without nano roughness, fusible component, etc. may be used for a smart and microdynamic topology control system, especially when exemplary fibers and/or connections in an exemplary fiber network include magnetic additives.
  • usage of electrically conductive, electrically non-conductive, magnetic patterns, magnetic fields, magnetic additives, etc., and their combinations for functionalization an exemplary substrate may control morphology of exemplary carbon-containing fibers while producing and collecting an exemplary plurality of carbon-containing fibers from an exemplary functionalized substrate.
  • an exemplary control may be efficient when magnetic fields or magnetic additives may be used simultaneously during one of fiber production process (e.g. a magnetic fields-assisted electrospinning) or in the fibers and/or thermoplastic and/or meltable material mixtures, etc., and combinations thereof.
  • an exemplary fiber production process may include magnetic fields- assisted electrospinning.
  • an exemplary plurality of nanostructures may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphenebased materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide ( FcPSp.
  • Si Silicon
  • B Phosphorus
  • LDHs layered double hydroxides
  • MXenes carbon nano
  • an exemplary plurality of nanostructures may include at least one of a hydroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), chalcogenides, molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof.
  • an exemplary resin may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, a carbohydrates, a polysaccharide, a carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), an acrylic resin, silicone, a polysiloxane, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEG), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, hydrogels, acrylates, poly(sodium acrylate), a polyimide, poly(amidoamine) (PAMAMs), polyaniline, polysiloxanes, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials,
  • step 102 of forming a plurality of carbon-containing fibers may include forming an exemplary plurality of carbon-containing fibers on an exemplary substrate/functionalized substrate.
  • an exemplary plurality of carbon containing fibers may interact with an exemplary functionalized substrate.
  • an exemplary interaction between an exemplary plurality of carbon containing fibers with an exemplary functionalized substrate may effect topology of an exemplary carbon-rich nanostructures.
  • an exemplary plurality of carbon containing fibers may be produced using at least a carbon fiber precursor.
  • an exemplary carbon fiber precursor may form an exemplary plurality of carbon-containing fibers by at least a method of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel electrospinning, and combinations thereof.
  • an exemplary plurality of carbon-containing fibers may include at least one of nano, micro, and multiple scaled fibers.
  • an exemplary carbon-rich precursor may include at least one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, carbon-containing salt, carbon-containing alloy, metal-organic frameworks (MOF), and combinations thereof.
  • MOF metal-organic frameworks
  • an exemplary carbohydrate may include at least one of sucrose, dextrins, starch, glucose, and combinations thereof.
  • an exemplary polysaccharide may include one of N-[(2-hydroxy-3- trimethyl ammonium) propyl] chitosan (HTCC), lignin, and combinations thereof.
  • step 104 of forming a two or multi-phase system may include adding a thermoplastic material to an exemplary plurality of carbon-containing fibers.
  • at least one thermoplastic material may be added to an exemplary plurality of carbon-containing fibers.
  • adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers may include at least one of adding an exemplary at least one thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary at least one thermoplastic material to an exemplary substrate, an exemplary functionalized substrate, one of exemplary composition of an exemplary functionalizing materials for substrate, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers, after forming an exemplary plurality of carbon-containing fibers, and combinations thereof.
  • an exemplary thermoplastic material may be added to an exemplary carbon fiber precursor with a weight ratio in a range of 0.0005:1 to 10:1 an exemplary thermoplastic material: carbon fiber precursor).
  • an exemplary thermoplastic material may have a melting point below 450°C.
  • adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon- containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process of at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) elctro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-
  • an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, a poly( amidoamine) (PAMAM), a silicone, a silicone compound, a poysiloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, poly or oligo or monoacrylates, nanostructures, salts, for example, zinc nitrate, elements for example, zinc, mixtures of exemplary thermoplastic materials with each other or with other materials, mixtures of exemplary thermoplastic materials with of at least one of protein compounds, oligomers, co- or tri-polymers, amphiphilics, macromolecules,
  • PVA poly
  • adding at least one thermoplastic material to an exemplary plurality of an exemplary carbon fiber precursor-containing nanofibers, in a way to form a two/multi phased system may include forming a plurality of at least one of thermoplastic material elements along with an exemplary plurality of carbon fiber precursor-containing nanofibers elements.
  • step 106 of forming a nano structured network may include heating the two or multi-phase system to a temperature up to 450°C.
  • an exemplary two or multi-phase structure may be separated from an exemplary substrate when applying a temperature of at least 200°C to an exemplary two or multi-phase structure.
  • exemplary carbon-containing fibers when an exemplary substrate may be subjected to an exemplary heating process, exemplary carbon-containing fibers may be connected at least to each other, to an exemplary substrate, and combinations thereof via a plurality of connections made by at least one of exemplary melted components.
  • an exemplary nanostructured network may include a plurality of carbon-containing fibers connected to each other via an exemplary plurality of thermoplastic connections.
  • an exemplary two or multi-phase system may be heated in a heating device for a time period in a range of 10 minutes to 400 minutes.
  • an exemplary heating device may include a heater, a thermal chamber such as an oven, a heater, a furnace, etc.
  • an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof.
  • an exemplary inert gas may include at least one noble gas.
  • an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof.
  • heating an exemplary two or multi-phase system may melt an exemplary thermoplastic material.
  • an exemplary thermoplastic material may have a melting point below 450 °C.
  • exemplary elements of an exemplary thermoplastic material may form connections when exemplary elements melt at an exemplary meeting points of exemplary nanofibers crossing and/or substrate.
  • heating an exemplary two or multi-phase system may form connections between carbon-containing fibers via an exemplary melted thermoplastic material.
  • an exemplary connection between exemplary carbon-containing fibers may form a nano structured network.
  • an exemplatry nanostructured network may form by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers.
  • forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon-containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450°C.
  • controlling an exemplary temperature may control topology of an exemplary nanostructured network.
  • important factors for controlling topology of exemplary carbon rich nanostructures may include duration of an exemplary process, percentage composition of exemplary components, melting point of each of exemplary components, thermal characteristics of each of exemplary components, number and ratio of thermoplastic materials and/or a meltable materials, method of adding each, proximity and frequency of connections, morphology, fineness and abundance and density of carbon- containing fibers between joints, characteristics and rheology of molten materials, rate of expansion of an exemplary carbon-rich nanostructure, boosting factors that may create tension, expansion, or prevent shrinking, curie temperature, dosage of atmosphere mixtures, number and temperature of thermal steps, moisture content in an exemplary system for example, " moisture regain of materials" etc.
  • an exemplary control tension system may work in the form of mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic, and smart microdynamic systems, etc. and combinations thereof.
  • an exemplary curie temperature may be important for considering when magnetic, nanomagnetic, or smart and thermodynamic magnetic/nanomagnetic or combined mechanisms, and/or additives containing magnetic materials are used.
  • step 108 of increasing carbon content of the nanostructured network may include heating an exemplary nanostructured network to a temperature of at least 800°C.
  • an exemplary heating process may be used for increasing carbon content of an exemplary nanostructured network.
  • heating an exemplary nano structured network may form carbon-rich nanostructures.
  • an exemplary carbon-rich nanostructures may include one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially- carbon-rich nanocomposite, and combinations thereof.
  • an exemplary nanostructured network may be heated in a furnace.
  • at least a non-carbon containing element may leave an exemplary nano structured network.
  • non-carbon elements such as oxygen, nitrogen and hydrogen, halogens, etc.
  • leaving gasses may include hydrogen cyanide (HCN), (nitrogen) N2, water (H2O), etc.
  • an exemplary non-carbon element composition may depend on the composition of an exemplary nanostructured network and the chemical structure of an exemplary nano structured network.
  • an exemplary furnace may include a gas inlet and a gas outlet.
  • exemplary gases leaving an exemplary heating device may include a neutral gas or a predetermined atmosphere.
  • an exemplary predetermined atmosphere may include noble gases.
  • an exemplary nanostructured network may be heated under an inert gas atmosphere.
  • an exemplary inert gas may enter from an exemplary gas inlet and may leave an exemplary furnace from an exemplary gas outlet.
  • an exemplary nanostructured network may be heated under an inert gas atmosphere with atmospheric pressure.
  • an exemplary inert gas may include at least a noble gas and/or a mixture of atmospheres.
  • an exemplary heating process may be used under air atmospheres at a temperature of 280 °C -300 °C, a combined atmosphere of 5-50% air atmosphere in combination with inert atmosphere may be applied at a temperature up to 300 °C -350 °C.
  • an exemplary nano structured network may be kept for 5 minutes to 20 minutes at a temperature of 350 °C - 380 °C in a mixed atmosphere containing 5-50% air atmosphere, then the air atmospheric atmosphere may be replaced with a rate of 2% per minute to 20% per minute with inert atmosphere and concurrently temperature may be increased with a rate of 2 °C/min. to 20 °C/min.
  • an exemplary heating process may continue at a temperature higher than 400 °C or higher than 450 °C in a completely inert atmosphere.
  • Controlled dosing of an exemplary atmosphere may be followed in any one of an exemplary forming integrated fused network (IFN) step, an exemplary fixing and refining topology of an exemplary carbon-rich nanostructure via increasing carbon content (FRIC) thermal step, and combinations thereof.
  • IFN and FRIC thermal steps may be followed continuously or separately in form of one integrated thermal process or two/multi separated thermal procedures.
  • each of an exemplary IFN or FRIC steps may include one, two or more continuous or separate thermal steps.
  • exemplary thermoplastic materials with melting temperature equal or lower than the temperature of FRIC step may create a new connection or plasticize an exemplary nano structured network or both at the same time by forming carbon rich nanostructures and conducting and refining topology of an exemplary carbon rich nanostructures especially when more than one type of thermoplastic material with different melting temperatures may be used in an exemplary method.
  • melting of one or more thermoplastic material may also be performed in an exemplary FRIC step.
  • a thermoplastic component may completely or partially leave an exemplary carbon rich nanostructure during thermal processes, or a small percentage of an exemplary thermoplastic component may remain or an exemplary thermoplastic component may join an exemplary carbon, graphite or carbon/graphite network along with an exemplary carbon rich nanostructure.
  • residue of an exemplary thermoplastic component may be removed in following steps of washing or purification when an exemplary thermoplastic component may not be incorporated in an exemplary carbon, graphite or carbon/graphite structure and/or the patterns on an exemplary carbon, graphite or carbon/graphite structure.
  • factors considered during an exemplary method for controlling topology of an exemplary carbon rich nanostructures may include controlling balance between thermal expansion, expansion under pressure of exhaust gases and stress resulting from exhaust gases on an exemplary plurality of carbon-containing fibers in distances between connections, plasticizing effect of exemplary melting components, plasticizing, tendency to shrinkage with increasing temperature and structure, and type of functionalization an exemplary substrate and thermal and rheological behavior of an exemplary substrate, and stability of topology by increasing carbon content, etc., and the combinations thereof.
  • parameters effecting topology of an exemplary carbon rich nanostructure may include temperature increase rate, maximum temperature, process duration, percentage composition of components, melting point of each component, thermal characteristics of each of exemplary components, number and ratio of exemplary thermoplastic materials, mechanism of adding each component, closeness and frequency of joints, morphology, elegance and frequency and density of fibers between joints, rheological properties of molten materials and additives, rheological properties of cabon-contanining fibers such as stretchability, modulus, elasticity, and composition of additives, as well as geometry of nanostructures on exemplary cabon-contanining fibers, rheological properties of nanocomposites, such as effect of nanostructures on elasticity, modulus, elasticity, rate of gas release, strengthening of factors that may expand and create tension, or prevent shrinkage of an exemplary carbon-rich nanostructure using mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic and smart microdynamic systems, etc., curie temperature when magnetic, nanomagnetic
  • an exemplary carbon-rich nanostructures may have a convoluted, wavy, spiral, porous, intertwined, angled, branched, networked (integrated network), fibrous, hollow, patterned of nano, micro, meso and quantum sized structures.
  • controlling an exemplary topology of an exemplary carbon-rich nanostructures may include forming at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, nano-curvature graphitic integrated network nanocomposites/nanostructures with twisted layers, nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted layers, and combinations thereof.
  • an exemplary nanostructured network may be heated to form a carbon-rich nanostructure (heating process).
  • an exemplary nano structured network may be separated from an exemplary substrate before an exemplary heating process when an exemplary substrate undergo undesirable shape changes during an exemplary heating process.
  • an exemplary substrate may include aluminum, polypropylene, and polyester.
  • an exemplary nano structured network may be heated after separating an exemplary nanostructured network from an exemplary substrate/functionalized substrate.
  • an exemplary nanostructured network may be heated in a furnace at a temperature of at least 800°C.
  • an additive may be added to at least one of an exemplary mixture containing a carbon fiber precursor, an exemplary thermoplastic material, an exemplary carbon-rich nanostructure, and combinations thereof.
  • a layer of an exemplary additive may be formed on an exemplary carbon-rich nanostructures.
  • an exemplary additive may have a thickness of up to 1 mm.
  • an exemplary additive may include at least one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, a hydrogel, a vitamin, a softener agent, a surfactant, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, BETS, hyroxides, salts, composites, nanostructures of an exemplary additive, frameworks of an exemplary additive, and combinations thereof.
  • an exemplary additive may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, carbohydrates, polysaccharide, carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), acrylic resins, silicones, poly siloxanes, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, a hydrogels, acrylates, poly(sodium acrylate), polyimides, a poly(amidoamine) (PAM AMs), a polyaniline, poly siloxanes, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, metal-
  • an exemplary nanostructured additive may include at least one of a Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene-based materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPS ).
  • Si Silicon
  • B Boron
  • LDHs layered double hydroxides
  • nanostructure additives may also include one of metals such as Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B).
  • metals such as Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B).
  • CNT carbon nanofibres
  • CNFs carbon nanofibres
  • fullerene graphene
  • graphene oxide reduced graphene oxide
  • MOFs MOFs
  • hBN borophene
  • Bismuth strontium calcium copper oxide BSCCO
  • kagome lattices e.g. kagome (BETS) 2 GaC14
  • BETS metal compounds e.g.
  • organic/inorganic nanostructures in which the organic component may be one of anhydrides e.g., one of anhydrides
  • Maleic anhydride acrylic acid, n-methylols, carbamides, acrylic resins, silicones, poly siloxanes, polyurethanes, aldehydes, PVA, PA, polyols, polyoxides, polyesters, proteins, polycarbonates, polystyrenes, polysaccharides, carbohydrates, poly electrolytes, hydrogels, poly(sodium acrylate), polyimides, PAMAMs, polyaniline, polyvinyls, PVdF, their monomers, ammonias, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, electrolytes, MOFs, drugs, dyes, softeners, antistatic, flame-retardants, etc.
  • forming an exemplary carbon-rich nanostructures may include intermediate processes such as washing, purification, in-situ synthesis, irradiation, coating, loading additives in the form of combined and sequential processes, etc.
  • exemplary washing and purification processes may be performed due to removing some components, creating porosity, improving the thermal, mechanical, rheological properties, etc.
  • an exemplary carbon-rich nanostructure may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof.
  • an exemplary plurality of carbon- containing fibers may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof.
  • an exemplary nanostructured network may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof.
  • an exemplary washing process may be performed via one, two, or frequent immersing, dipping, centrifuging, in one of an organic solvent, an acid solution, an alkaline solution, an oxidant solution, an enzyme solution, a surfactant solution, reducing agent solution, an ionic solvent, aqueous solutions, water, and combinations thereof.
  • an exemplary washing process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc. and combinations thereof.
  • an exemplary carbon-rich nanostructure, an exemplary plurality of carbon-containing fibers, an exemplary nanostructured network, and combinations thereof may be purified using at least one of an acid solution, a basic solution, an oxidant solution, an organic solution, and combinations thereof.
  • an exemplary purifying process may include applying heat, for example, in a furnace.
  • an exemplary purifying process may be used for eliminating/reducing dust and impurity from air and environment, for activation, increasing specific surface area, refining morphology of an exemplary carbon rich nanostructure, mending defects, covering defects, functionalization, etc.
  • an exemplary purifying process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc., and combinations thereof
  • an exemplary nano structured additive may be in-situ synthesized using at least one of a hydrothermal process, a solvothermal process, a chemical reduction/oxidation, irradiation, a thermal process, and combinations thereof.
  • a component may be eliminated before or after forming an exemplary nanostructured network using at least one of an organic solvent, an acid solution, a basic solution, an oxidant solution, water, and combinations thereof.
  • an exemplary component may depend on an exemplary carbon containing precursor, an exemplary thermoplastic material, additives, etc.
  • additives may be added for reinforcement of an exemplary carbon-rich nanostructure, forming a porous structure, or for synergistic effects, covering defects, improving properties of an exemplary carbon rich nanostructure, improving performance of an exemplary carbon rich nanostructure, surface modifications of an exemplary carbon rich nanostructure, adding a roughness, nano roughness, modifying the thermal, rheological, mechanical, tensile properties during or after an exemplary process, forming a composite, nanostructure, superstructure, a metamaterial, a heterostructure, surface modification, conducting fiber morphology, conducting IFN or FRIC steps, adding a feature on an exemplary substrate, achieving a smart, a multi-functional, a multi targeted feature, and combinations thereof, adding a nano, meso, quantum size feature, jagged morphology, increasing exemplary leaving gas flow rate, porosity, etc.
  • conducting IFN or FRIC steps may include designing smart self-activated topology control mechanisms.
  • achieving a smart, a multi-functional, a multi targeted feature may include a smart multi-purpose drug delivery, multi targeted drug delivery and cell attachment, bone cement/injectable gel reinforcement, etc.
  • an exemplary eliminated component may include one of exemplary additives, for example, a salt, a softener, an electrolyte, a thermoplastic component, a hydrogel, a resin, a nanostructure, a metal, etc., a byproduct (for instance achieved from an in situ synthesis), precursor or intermediates of an in-situ synthesis, an impurity, an attached substrate which may be designed to be detached before, component which may not be proper or designed to remain during a thermal process, creating porosity, hollow fibers, hollow structures, etc.
  • exemplary additives for example, a salt, a softener, an electrolyte, a thermoplastic component, a hydrogel, a resin, a nanostructure, a metal, etc.
  • a byproduct for instance achieved from an in situ synthesis
  • an exemplary special approaches may include an additive and/or a thermoplastic and/or a meltable content material may be set to achieve an especial morphology through fiber production or processing, but it may be partially or completely removed according to approaches set through an exemplary thermal process.
  • Example 1 Producing intertwined woven-like nanocomposites with control on topology in sharp folded edges
  • a method similar to method 100 or method 110 may be used.
  • a polymer solution of PEG/PAN and a nanocomposite solution of PEG/TiCb were electrospun alternatively.
  • two polymer solutions were prepared.
  • a nanocomposite polymer solution was prepared.
  • titanium dioxide (TiCh) and PEG were dissolved in distilled water at room temperature.
  • FIG. 2A illustrates a field emission scanning electron microscopy (FESEM) image of exemplary intertwined woven-like nanocomposite nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 2B illustrates a magnified FESEM image of intertwined woven-like nanocomposite nanostructures shown in FIG. 2A, consistent with one or more exemplary embodiments of the present disclosure.
  • the nanocomposite polymer solution contained 100-150 wt. %, here for the exemplary structure shown in FIG. 2A and 2B, 120 wt. % PEG and 1-5 wt%, here for the exemplary structure shown in FIG. 2A and 2B, 1 wt. % TiCE.
  • the nanocomposite polymer solution was homogenized for 0.2-24 hour here for the exemplary structure shown in FIG. 2A and 2B, 1 hour using a magnetic stirrer. Then, the nanocomposite polymer solution may be sonicated for 0-5 minute (here for the exemplary structure shown in FIG. 2A and 2B, it was sonicated for 1 minute) using an ultrasound probe at ambient temperature before the electrospinning process.
  • the nanocomposite polymer solution was injected using a dual-nozzle pump syringe. A voltage of 15-22 kV was be applied, here for the structure shown in FIG. 2A and 2B, a voltage of 18 kV was applied to the nozzle tips.
  • Pump syringe may set with a flow rate of 0.08-0.4 mL/h, here for the exemplary structure shown in FIG. 2A and 2B, 0.1-0.3 mL/h for 0.5-20 minutes (here for the exemplary structure shown in FIG. 2A and 2B 1-10 minutes) in each turn.
  • the polymer solution may be injected using a single, dual-nozzle or multi-nozzle.
  • a distance between a collector and a tip of the dual-nozzle pump syringe may be set at 14-25 cm (here for the exemplary structure shown in FIG. 2A and 2B, 20 cm).
  • polyethylene glycol (PEG) and polyacrylonitrile (PAN) were mixed with dimethylformamide (DMF).
  • the polymer solution may contain 4-9 wt. %, (here for the exemplary structure shown in FIG. 2A and 2B, 5 wt. %) PAN and 10-17 wt. % PEG (here for the exemplary structure shown in FIG. 2A and 2B, 15% PEG) in DMF solvent.
  • the polymer solution may be homogenized using a homogenizer at room temperature for 30 minutes to 24 hours (here for the exemplary structure shown in FIG. 2A and 2B, 1 hour).
  • the polymer solution may be injected using a single, dual-nozzle or multinozzle pump syringe with flow rate of 0.1 -0.4 mL/h (here for the exemplary structure shown in FIG. 2A and 2B, 0.1-0.3 mL/h) (accuracy of 0.01 mL/h).
  • the applied voltage to the dualnozzle pump syringe may be set 16-22 kV (here for the exemplary structure shown in FIG. 2A and 2B, applied voltage was 18 kV) and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe may be considered 10-27 cm (here for the exemplary structure shown in FIG. 2A and 2B, applied voltage was 20 cm) for 10-540 min (here for the exemplary structure shown in FIG. 2A and 2B, 60-180 min in each trun).
  • the polymer solution of PEG/PAN and the nanocomposite solution of PEG/TiO were electrospun alternatively.
  • the nanocomposite solution of PEG/TiCh was electrospun for 10 minutes on a collector covered with an aluminum foil.
  • the polymer solution of PEG/PAN was electrospun for (60-180 minutes).
  • the collector may be covered with a lace fabric e.g. a PET lace fabric.
  • the collector may be made of a metallic or conductive lace, a magnetic or conductive pattern, etc.
  • a rotary collector may be used.
  • a traverse (partial movement) can be applied between the nozzle tip and the collector.
  • a simple collector covered with an aluminum sheet was used for the structure shown in FIG 2A and 2B .
  • the electrospun nanofibers was collected from the collector and transferred on a titanium sheet.
  • a thermal process to form integrated fused network (IFN) and a process of fixing and refining the topology via increasing the carbon content (FRIC) were applied on the electrospun nanofibers.
  • the electrospun nanofibers were heated at 220-300 °C, here for the exemplary structure shown in FIG. 2A and 2B, 230°C for 0.5-2 hour, here for the exemplary structure shown in FIG. 2A and 2B, 1 hour under ambient atmosphere.
  • the electrospun nanofibers were heated at 1000 °C under nitrogen atmosphere for 0.5-2 hour (for the exemplary structure shown in FIG. 2A and 2B, 1 hour).
  • the integrated fused network was fixed and refined via increasing carbon content and the topology fixed in the form of carbon-rich nanostructure nanocomposite.
  • the heating rate may be 3-15 °C/min, here for an exemplary structure shown in FIG. 2A and 2B, it was 10 °C/min.
  • thermoplastic component with a high ratio in this example may also have the role of a plasticizer and it may help to bring closer the distances of connections and thermal shrinkage to some extent.
  • the thermoplastic component in this example melts in the initial stages of the thermal process and guides the control of the structure.
  • the thermoplastic component may leave the final structure almost completely or partially, or a small percentage of it may remain. The residue may join the carbon-rich nanostructure.
  • Example 2 Creating dome-shaped intertwined woven-like nanostructures on sharp micro-size curvatures
  • a method similar to method 100 or method 110 may be used.
  • a polymer solution was produced.
  • PEG polyethylene glycol
  • PAN polyacrylonitrile
  • DMF dimethylformamide
  • the type and composition and the percentage of materials along with the production conditions are selected in such a way that the mixture after leaving the nozzle have a tendency to form a two-phase system comprising elements of thermoplastic or fusible components when the mixture is subjected to solvent evaporation, exposure to the electrospinning process forces with the controlled and selected conditions and/or spinning environment conditions (such as humidity, etc.).
  • FIG. 3A illustrates a FESEM image of exemplary dome-shaped intertwined woven-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 3B illustrates a magnified FESEM image of exemplary dome-shaped intertwined woven-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • the polymer solution for an exemplary sample shown in FIG 3 A and 3B, contained 5 wt. % PAN and 15 wt. % PEG in DMF solvent.
  • the polymer solution was homogenized using a homogenizer at room temperature for 1 hour.
  • the polymer solution was injected using a dual-nozzle pump syringe with flow rate of 0.1 mL/h (accuracy of 0.01-0.3 mL/h).
  • the applied voltage to the dual-nozzle pump syringe was 18 kV and a distance between a collector (substrate) and a tip of the dualnozzle pump syringe was 20 cm for an exemplary sample.
  • the electrospun nanofibers were collected from the collector and transferred on a titanium sheet. Then, a thermal process (IFN) and a process of increasing carbon content (FRIC) were applied on the electrospun nanofibers.
  • the electrospun nanofibers were heated at 220 °C -300 °C, for an exemplary sample shown in FIG. 3A and 3B, 230°C for 30 minutes to 2 hours, here for the exemplary structure shown in FIG. 3A and 3B, 1 hour under ambient atmosphere.
  • the electrospun nanofibers may be heated at 1000 °C under nitrogen atmosphere for 30 minutes to 2 hours (here, for the exemplary structure shown in FIG. 3A and 3B, was 1 hour).
  • the process of increasing the carbon content may include forming the integrated fused network (IFN) and fixing and refining the structure via increasing carbon content (FRIC) of the electrospun nanofibers.
  • the process of increasing the carbon content may include increasing carbon content, fixing, and forming the topology of the integrated fused network.
  • the heating rate may be set 5-10 °C/min, here for the exemplary structure shown in FIG. 3A and 3B, it was 10 °C/min.
  • inorganic or polymeric microspheres may be added on the surface of the collector.
  • Inorganic microspheres such as titanium dioxide, silicon dioxide, zinc oxide or salts such as zinc sulfide, zinc nitrate, etc., carbon structures, metallic and organic/ inorganic structures such as MOFs, etc., can be loaded, coated, sputtered, and/or sprayed on the surface through one of the surface modification methods. They can be sprayed or coated, or they can be sprayed or added at the same time as spinning of fibers.
  • Polymeric microspheres can also be added by the same usual methods or be formed simultaneously with the process of producing nanofibers, for example, by an electrospray process. This process can also include spraying capsules, etc.
  • the polymer may be include for example one of materials mentioned for carbon precursor and/or thermoplastic components, etc. such as polyacrylonitrile and its derivatives, chitosan, PVA, PEG, etc. and combinations thereof.
  • the spheres can leave the structure during the process, for example, during the thermal process, to increase porosity of structure or remain and join the carbon structure or a combination of these options may be used.
  • the simultaneous production of polymer micro sphere and their spraying during the electrospinning of carbon-containing nanofibers was used while designing an electrospray process through a separate nozzle.
  • a PAN polymer/mixture electro spraying may be used as one of the cheapest options.
  • PAN polymer may be homogenized with a concentration of 2.5-3.5% in DMF for 30 minutes-24 hours, and electrospray with a feed rate 0.5-1 ml/hour, a distance of 10-13 cm, a voltage of 6.5-8.5kV (for instance an AC voltage) may be used.
  • the nozzle may traverse to cover the entire sample.
  • the electrospun nanofibers were heated at 230°C for 1 hour under ambient atmosphere. Then, the electrospun nanofibers were heated at 1000°C under nitrogen atmosphere. The heating rate was 10°C/minute for the exemplary structure (shown in FIG. 3A and 3B.
  • Example 3 Producing bone tissue-like nanocomposites nanostructures
  • FIG. 4 illustrates a scanning electron microscopy (SEM) image of exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • the nanocomposite polymer solution may contain 100- 150 wt. %, here for the exemplary structure shown in FIG. 4, 120 wt. % PEG and 1-5 wt. % here for the exemplary structure shown in FIG. 4, 1 wt. % TiCF.
  • the nanocomposite polymer solution was homogenized for 0.2-24 hour here for the exemplary structure shown in FIG. 4, 1 hour using a magnetic stirrer. Then, the nanocomposite polymer solution may be sonicated or not.
  • the nanocomposite polymer solution may be sonicated for 0.1-5 minute (here for the exemplary structure shown in FIG. 4, it was sonicated for 1 minute) using an ultrasound probe at ambient temperature before the electrospinning process.
  • the nanocomposite polymer solution was injected using a dual-nozzle pump syringe.
  • a voltage of 15-22 kV, here for the structure shown in FIG. 4, 18 kV was applied to the nozzle tips, the pump syringe may run with a flow rate of 0.02-0.5 mL/h, here for the exemplary structure shown in FIG. 4, 0.1 mL/h for 0.5-20 minutes (here for the exemplary structure shown in FIG. 4, 10 minutes) in each turn.
  • a distance between a collector and a tip of the dual-nozzle pump syringe may be set 15-25 cm (here for the exemplary structure shown in FIG. 4, it was 20cm).
  • polyethylene glycol (PEG) and polyacrylonitrile (PAN) were mixed with dimethylformamide (DMF).
  • the polymer solution may contain (7-16 wt. %) (here, for the exemplary structure shown in FIG. 4, 11 wt. %) PAN and 0.1-4.5 wt. % PEG, here, for the exemplary structure shown in FIG. 4, 1 wt. % PEG in DMF solvent.
  • the polymer solution was homogenized using a homogenizer at room temperature for (0.5-24 h) (here for the exemplary structure shown in FIG. 4, 1 hour).
  • the polymer solution was injected using a dual-nozzle pump syringe with flow rate of 0.15-0.6 mL/h, here for the exemplary structure shown in FIG. 4, 0.5 mL/h) (accuracy of 0.01 mL/h).
  • the applied voltage to the nozzles tips pump syringe may be 10-16 kV (here for the exemplary structure shown in FIG. 4, it was 12 kV) and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe may be set 10-17 cm (here for the exemplary structure shown in FIG. 4, it was set 12 cm) for 3-60 min (here for the exemplary structure shown in FIG. 4, 60 min).
  • the collector may be covered with a lace fabric e.g. a PET lace fabric.
  • the collector may be made of a metallic or conductive lace, a magnetic or conductive patterns, etc. for especial approaches.
  • a rotary collector may be used.
  • a traverse (partial movement) can be considered between the nozzle tip and the collector.
  • a simple collector covered with an aluminum sheet was used.
  • the system may include at least one nozzle.
  • the polymer solution of PEG/PAN and the nanocomposite solution of PEG/TiCh may be electrospun alternatively.
  • the nanocomposite solution of PEG/TiCh was electrospun for 10 minutes on a collector covered with an aluminum foil. Then, the polymer solution of PEG/PAN was electrospun for 60 minutes. After that, the nanocomposite solution of PEG/TiO was electrospun for 10 minutes, the polymer solution of PEG/PAN was electrospun for 60 minutes and for the last step the nanocomposite solution of PEG/TiOi was electrospun for 10 minutes.
  • the electrospun nanofibers were collected from the collector and transferred on a titanium sheet. Then, a thermal process (IFN) and a process for increasing carbon content of the integrated fused network were applied on the electrospun nanofibers.
  • the process of increasing the carbon content may include forming the integrated fused network (FIN) and fixing and refining the structure via increasing carbon content (FRIC) of the electrospun nanofibers.
  • the process of increasing the carbon content may include increasing carbon content, fixing, and conducting formation the topology of the integrated fused network.
  • the electrospun nanofibers may be heated at (220-300 °C, here for the exemplary sample in FIG.
  • the electrospun nanofibers were heated at 1000 °C under nitrogen atmosphere for 0.5-2 hour (here for the exemplary sample in FIG 4, 1 hour).
  • the heating rate may be set at 10-20 °C/min, here for the exemplary sample in FIG 4, it was 10 °C/min.
  • the fibers between the connections are subjected to tension during the expansion of the system due to the outflow of gases when exposure to the flow of exhaust gases. Since the fibers are connected with different directions and angles, as a result of the tension, due to the outgoing flow of gases, curves, twists, waves, pores and an amazing architecture, for example, resemble the architecture of bone tissue can be formed.
  • the thermoplastic material may help to boost flexibility, extension, elasticity and/or elongation of the fiber between the connections just when they are subjected to the tension by the outgoing gases flow, align the polymer chains more effectively and arrange them more by plasticizing the structure.
  • FIG. 5 illustrates an Energy-dispersive X-ray spectroscopy (EDX) diagram for exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • EDX Energy-dispersive X-ray spectroscopy
  • FIG. 6 illustrates a SEM image of exemplary bone tissue-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • the polymer solution may contain (7-16 wt. %) (here for the exemplary sample shown in FIG. 6, it was 13.25 wt. %) PAN and 0.1-4.5 wt. % PEG, here for this exemplary sample, (0.1-1 wt. %) PEG in DMF solvent.
  • the polymer solution was homogenized using a homogenizer at room temperature for 30 minutes to 24 hours (here for this exemplary sample shown in FIG. 6, 2 hour).
  • the polymer solution was injected using a dual, single or multi-nozzle pump syringe with flow rate of 0.1-0.6 mL/h, here for the exemplary sample in FIG. 6, a single-nozzle syringe with flow rate of 0.22 mL/h (accuracy of 0.01 mL/h) was applied.
  • the applied voltage to the nozzles tips pump syringe may be set 10-16 kV (here for the exemplary sample in FIG. 6, 12 kV) and a distance between a collector and a tip of the dual-nozzle pump syringe may set 10-17 cm (here for the exemplary sample in FIG. 6, 10 cm) for 3-60 min (here 20-45 min).
  • the collector may cover with a metal sheet, a fabric, lace fabric, e.g. a PET lace fabric.
  • a rotary collector may be used.
  • a traverse can be considered between the nozzle tip and the collector.
  • a simple collector was applied for the structure shown in FIG. 6, a simple collector was applied.
  • the electrospun nanofibers were collected from the collector and transferred on a titanium sheet. Then, a thermal process to form the integrated fused nano structured network and a process of conducting, refining and fixing the topology via increasing carbon content were applied on the electrospun nanofibers.
  • the process of increasing the carbon content may include forming the integrated fused network (IFN) and fixing and refining the structure via increasing carbon content (FRIC) of the electrospun nanofibers.
  • the process of increasing the carbon content may include increasing carbon content, conducting and refining the topology and fixing, of the integrated fused network in form of a topology-controlled carbon-rich nanostructure.
  • the electrospun nanofibers were heated at 220 °C -300 °C, (here for the exemplary sample in FIG. 6, at 230 °C) for 30 minutes to 2 hours, (here for the exemplary sample in FIG. 5, 1 hour) under ambient atmosphere. Then, the electrospun nanofibers were heated at 1000 °C under nitrogen atmosphere for 30 minutes to 2 hours (here for the exemplary sample in FIG. 6, 1 hour).
  • the heating rate may be set at 10 °C/min -20 °C/min, here for the exemplary sample in FIG. 6, 10°C/min,
  • the bone tissue-like nanostructures were hollow sphere-like with spongy cancellous bone-like nano structured shell. It is highly similar to human shin bone tissue structure.
  • the invention of such a topology can simultaneously bring many advantages of natural bone tissue, only two of which include a special architecture, to withstand pressure and to provide the possibility of producing a scaffold with proper porosity and open pores with appropriate size with the advantage of providing (creating) the possibility of cell penetration and compatibility.
  • Cell penetration into the scaffold is one of the biggest challenges of nanofibrous scaffolds, while the problem of shrinkage and swelling in biological fluids intense this challenge, which in most scaffolds causes the pores to close and become inaccessible.
  • This invention response to these challenges by engineering such biomimetic steady topologies resistant also to deformation. It seems that the bone topology may play a remarkable role to provide bones with an amazing resistance to pressure.
  • FIG. 7A illustrates Fourier transform infrared (FTIR)-attenuated total reflection (ATR) (FTIR-ATR) spectrums of exemplary nanostructures (spectrum 702) and nanocomposites nanostructures (spectrum 704) after an exemplary fixing and refining process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • Diagram 701 shows magnified view of curve 704 shown in diagram 700.
  • FIG. 7B illustrates FTIR-ATR spectrums of exemplary electrospun bone tissue-like nanostructures before an exemplary heating process for forming integrated fused network (IFN) (spectrum 708) and after an exemplary fixing process in form of carbon nanostructures (spectrum 706), consistent with one or more exemplary embodiments of the present disclosure.
  • IFN integrated fused network
  • FIG. 7A curve 702 shows PEG/PAN nanofiber after an exemplary fixing and refining process in form of carbon nanostructures.
  • Curve 704a shows magnified curve 704 of TiCF/PEG/PAN nanofiber after an exemplary fixing and refining process in form of carbon nanostructures.
  • FIG. 8 illustrates a thermogravimetric analysis (TGA) spectrum after an exemplary fixing process in form of exemplary carbon nanostructures for an exemplary bone tissue-like composite, consistent with one or more exemplary embodiments of the present disclosure.
  • TGA thermogravimetric analysis
  • the weight loss in the sample was recorded up to a temperature of about 700 °C and after that the weight loss was stopped.
  • the weight loss up to 200 °C is usually related to the removal of moisture regains and water molecules may be trapped in the structure, which in this case includes about one percent of the weight loss, after that it is about 3.5 percent.
  • the percentage of weight loss is related to the removal of non-carbon impurities of functional groups connected to structural defects. This analysis also confirms the previous analysis and the results of FTIR-ATR spectroscopy, showing the formation of an almost complete carbon structure in this process.
  • FIG. 9 illustrates a Raman spectroscopy spectrum for an exemplary bone tissue-like nanostructure after an exemplary fixing process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • the peak related to the ordered graphite structures is very dominant in the Raman spectrum and it has recorded a significant difference with the peak related to the disordered structures, which shows that the dominant structure even in the sample after leaving the furnace (without any post-treatments is the ordered graphite structure. Therefore, it is easy to achieve a structure with more structural order via various methods of washing or treating with other materials and/or subsequent thermal procedures.
  • the structural order of graphite can perform better in terms of characteristics and strength. These results show that especially tension applied to the structure under the gases outflow exposure in wavy and curved areas have increased the ordered graphite structure. Especially considering the rate of temperature increase. Change the angle of the graphene layers in the wavy and curvature graphite structure is formed in the curves. In this way nanocurvature graphitic nanostructures/ nanocomposites with a twisted layered structure and nanowaved graphitic nanostructures/nanocomposites with twisted graphene layers may be formed. The results for the topology of woven-like structures also showed the graphitic structure, but this structure was more dominant in the bone-like structures.
  • the carbon precursor selected for the examples is the cheapest, most available and most abundant precursor on a commercial scale. This selection is due to prove the performance of strategy of this invention to engineer architecture, topology, geometry and morphology based on fibrous or nano-fibrous structures awarding also the unique feature of axial arrangement of the polymeric chains of the precursor in form of fibrous structure and all the advantages resulting from it with the cheap and plenty precursors providing the patients with affordable products.
  • the present method is not limited to expensive materials or biomaterials (with the limitation of rare and expensive sources/processing procedures or biomaterials (with further limitations such as high price, limited storage time, storage conditions, unpleasant odor, risk of transmission or absorption and spread of biological pollution, costly and time-consuming multi-step procedures for their extraction, processing and/or use, low chemical, thermal, biological and mechanical resistance (at least for the precursor), etc.) but the method can be used for producing such structures with abundant and cheap materials.
  • DMF Dimethylformamide
  • DMAc dimethylacetamide
  • 6-butyrolactone dimethylsulfoxide
  • DMSO dimethyl sulfone
  • DMSO dimethyl sulfonate
  • DMF/urea DMSO/urea
  • m-nitrophenol carbonates (ethylene carbonate), N -methyl-2-pyrrolidone (NMP), NaScN(aq), LiBr(aq) and ZnC12(aq)
  • NMP N -methyl-2-pyrrolidone
  • NaScN(aq) LiBr(aq) and ZnC12(aq) concentrate water solutions, ionic liquids (e.g.
  • pyridinium benzylchloride aqueous acid solutions (e.g. nitric acid and sulfuric acid), other polar organic solvents, hydroxy acetonitrile and mixtures (e.g. hydroxy acetonitrile/ethyl alcohol), etc. and combinations thereof.
  • Example 5 Creating a smart self-activated microdynamic topology-control mechanism using functionalized substrates and/or post treatments
  • a method similar to method 110 was used by adding one of a layer of a resin, a layer of the thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, conductive materials, etching the surface, and combinations thereof on the substrate.
  • a bone tissue-like topology were produced by spinning a solution of 7-16 wt. % PAN (for the exemplary sample here about 13%) in DMF (without PEG) to form the plurality of carbon-containing fibers.
  • the plurality of carbon-containing fibers were collected on the functionalized substrate and passed through the thermal treatments (Forming IFN and FRIC) with the functionalized heat resistant substrate.
  • the thermoplastic and/or meltable materials which their melting points meet the temperatures of the heating process will melt and the fibers may fuse to the substrate and/or each other at the connection sites.
  • the carbon nanostructures further may treat with the nanostructures to produce a nanocomposite.
  • patterned carbon nanostructured were devised via applying a resin post treatment after collecting the plurality of carbon-containing fibers on a functionalized heat resistance substrate.
  • FIGs 16- 19 Several other exemplary topology-controlled nanostructures have been introduced in FIGs 16- 19 via using a functionalized substrates for collecting nano fibers according to a method similar to method 110.
  • an exemplary nanoroughness resulting from the coating created with inorganic nanostructures may be considered to create nano roughness and use the resulting friction or nano friction to control movement, shrinkage, and also keep an exemplary plurality of carbon-containing nanofibers at certain places and prevent them from sticking and uncontrolled clumping. Therefore, an exemplary nano roughness may help to create curves, special spaces between curves, applying tension by dealing with thermal shrinkage microdynamically during an exemplary heating process to increase an exemplary arrangement of polymer chains, etc., and an exemplary microdynamic management on topology and morphology of an exemplary plurality of nano fibers.
  • the use of resins and applying changes in thermal processes may also help to control topology of an exemplary plurality of carbon-containing nanofibers.
  • melting components or thermoplastic materials can also be included in this functionalization.
  • the present disclosure may also establish the dynamic microdynamic, intelligent/microdynamic, intelligent/thermomicrodynamic, methods, etc. and combination thereof to control the thermal shrinkage through the thermal processes in the nano and atomic scale.
  • the combination of these three fusing mechanisms in a scale of nano or larger), nano friction of roughness as well as nano fiber entanglement in nanometer spaces between nano structures may be considered together.
  • the substrate for electrospinning the spinning solution was treated before the electrospinning process.
  • the functionalized substrate designed to go through the fixing and refining the topology via increasing carbon content (FRIC) with the integrated fused nanostructured network of two/multi-phase system and/or designed to go through the forming integrated fused network (IFN) of the two/multi-phase system may be a heat and or shrinkage resistant substrate e.g. a carbon fabric substrate, glass fabric, and so on.
  • the substrate may be a carbon-forming material, a graphite- forming material, a carbon/ graphite-forming material. Carbon forming substrate e.g.
  • the micro carbon fabrics were immersed inside the aqueous colloidal solutions for 10 seconds to 60 seconds. Then, the carbon fabrics were padded with 50% to 100% wet-pick up. The padded fabrics were then dried at a temperature of 10°C to 100°C. Some fabrics were also treated with a resin. Some resin e.g. PVA, PEG, etc.
  • the nanofunctionalized micro carbon fabrics with the nanostructures or the untreated micro carbon fabrics were immersed inside a potassium persulfate aqueous solution (K2S2O8, 0.4 wt. %) for 10 seconds. Then, the functionalized carbon fabrics were padded and dried. After that, the padded functionalized micro carbon fabrics were immersed inside an aqueous solution of disodium hydrogen phosphate (8 wt. %) and acrylic acid monomer (8 wt.
  • the fabrics may be also functionalized using at least a polymer, a resin, and combinations thereof.
  • the polymer and the resin may be in-situ polymerized on a substrate or may be added on the substrate using spray coating, impregnation, brushing, exhaustion, coating, dipping, impregnation, roll coating, padding, electro spraying, sputtering, etc.
  • One of resin used for functionalizing the fabric was self-cross-linkable amino-functionalized polysiloxane resin with a weight ratio of 0.06 wt. % to 10 wt. %.
  • the applied weight percent for the exemplary reported samples was 1.7 wt. % of the resin.
  • the fabrics (the nanofunctionalized or untreated ones) was impregnated with the resin for 3 seconds to 10 seconds.
  • the impregnated fabric was padded with 50% to 100% wet-pick- up.
  • the padded fabric was dried at a temperature of 10°C to 200°C.
  • the functionalized fabrics were washed to remove unreacted materials.
  • the functionalized fabrics were subjected to a fastness evaluation process to investigate the efficiency of the crosslinking and/or in-situ formed linkages through the in-situ polymerization to prevent leaching of nanostructures out.
  • the washing process was performed in 40 cycles with 5g/L detergent in water at a temperature of 60 °C.
  • Each cycle of the washing process was elongated for 30 minutes of treating the functionalized fabric with the detergent solution, the 40 cycles washing, then, followed by 200 hours immersing the fabric in the solution on the shaker + neutralization, rinsing with distilled water, 30 minutes immersing in the ultrasonic bath with detergent + 200 hours immersing in the solution on the shaker, rinsing and drying.
  • the washing process was performed for evaluating the stability in different conditions. Nanostructures released from the functionalized fabric into the washing solution was a measure of resistance to leaching. To this end, effluents gained from the washing process were examined using inductively coupled plasma (ICP) spectroscopy.
  • ICP inductively coupled plasma
  • FIG. 10 illustrates a SEM image of a micro carbon fabric substrate modified by exemplary clay nano layers on, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 11 illustrates a SEM image of functionalized micro carbon fabric modified with exemplary inorganic nanoparticles and resins after the fastness evaluation procedures, consistent with one or more exemplary embodiments of the present disclosure.
  • micro carbon fabric modified with inorganic nanoparticles and resin compounds which shows the successful transfer of nanostructures on the surface and their stability after successive washing procedures and exposure to various acute conditions, which is used in this disclosure as a suitable method for the functionalization of the carbon fabric substrate.
  • the micro carbon fabric was selected due to its shrinkage resistance and thermal resistance as the substrate to collect the nanofibers.
  • the micro carbon fabric was functionalized with inorganic nanoparticles and resins.
  • the SEM image shows nanofunctionalized micro carbon fabric subjected to the fastness evaluation procedures including the frequent washing process, etc. after functionalizing the micro carbon fabric.
  • FIG. 12 illustrates a SEM image of functionalized micro carbon fabric modified with exemplary clay nano layers and resins, consistent with one or more exemplary embodiments of the present disclosure.
  • the SEM image shows nanofunctionalized micro carbon subjected to the fastness evaluation procedures including frequent washing process, etc.
  • Microscopic evidence of functionalization the substrate of micro carbon fabric modified with clay nanolayers with a higher percentage than in FIG. 10 along with resin compounds (according to method 110) shows successful transfer of nanostructures on the surface of the carbon fabric and their stability after successive washings and exposure to various acute conditions.
  • As a suitable method for the functionalization of the carbon substrate which is also used in this disclosure.
  • a resin or a plurality of resins may be used to coat the plurality of collected fibers before the thermal procedures to form the integrated fused networks (IFN) and fixing and refining the topology via increasing carbon content (FRTC).
  • the polymer and the resin may be added on the fibers using spray coating, impregnation, brushing, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, etc.
  • the resin including the thermoplastic components may be applied at least with a molecular thickness. Resins e.g.
  • PVA (aq 1-10%), mixture of PVA (aq) and (0.1-2% HTCC(aq), mixture of PVA (aq) and/or PEG and (0.1-2% glucose), etc. and combination thereof were applied with brushing, spraying and/or electro spraying for the exemplary reported samples with a resin post- treatment in the examples (e.g. FIG 14, etc.).
  • Self cross-linkable polysiloxane resin was used as one of the resin for producing functionalized fabrics.
  • the in-situ synthesized resins and the cross-linkable resins especially self cross-linkable ones are especially efficient when an intermediate process e.g. washing, functionalization, hydro/solvo thermal synthesis are performed.
  • the use of resins or acrylate hydrogel also provides the possibility of relative movement of fibers for nano-size displacement and trapping between nanometer roughness, and if the melting of thermoplastic resins takes place in the initial stages and also at higher temperatures (when more than one meltable/ thermoplastic component is included), it is possible to enhance the efficiency.
  • silicone resins may melt at higher temperatures, and may strengthening the connection of the fiber with the substrate at their melting point, simultaneously they may have a plasticizing effect on the fiber, they improve the effect of tension (by the outflow gasses) on the fiber and may result in the polymer chain arrangement, while thermal expansion and exposing to the outflow of gases.
  • the functionalizations presented in the examples of this disclosure has been done in an aqueous environment and neutral pH as a green process.
  • the resins can be also coated on the carbon-rich nanostructures to fix the nanostructures on the fabric which is desirable for filtration applications, etc. and/or for their surface modification e.g. for controlled cell attachment approaches.
  • acrylate coatings in addition to the mentioned cases, in terms of similarity to the carbon fiber precursor in this example, and its graft (chemical bonds and linkages) for reasons such as providing proper stability, on the other hand, because of providing more effective control of fibers on the substrate with considering the high capacity of keeping moisture (especially in the form of nanocomposite with inorganic nanostructures), it was designed as a nonsolvent for PAN and compatible surface feature with PEG.
  • FIG. 13 illustrates a SEM image of exemplary bone tissue-like nanostructures formed on an exemplary functionalized substrate, consistent with one or more exemplary embodiments of the present disclosure.
  • the substrate was a carbon fabric functionalized by a resin including a thermoplastic resin component and the nanostructures.
  • the bone-like structures have been produced via electrospinning pure PAN (13 wt. %) in DMF without PEG, thermoplastic component is only included in the resin treatment of the substrate for this exemplary sample.
  • a bone tissue-like topology were produced by spinning a solution of 7-16 wt. % PAN (for the exemplary sample here 13%) in DMF (without PEG) to form the plurality of carbon-containing fibers.
  • the plurality of carbon-containing fibers were collected on the functionalized substrate and passed through the heat treatments with the functionalized heat resistant substrate. Through the heating process the thermoplastic and/or meltable materials which their melting points meet the temperatures will melt and the fibers may fuse to the substrate and/or each other at the connection sites.
  • the carbon nanostructures exemplary sample further was treated with nanoparticles to produce a nanocomposite.
  • the polymer solution (13% PAN in DMF) was homogenized using a homogenizer at room temperature for (30 minutes -24 hours) (here 2 hours).
  • the polymer solution was injected using a dual, single or multi-nozzle pump syringe with flow rate of 0.2-0.6 mL/h, here a dual-nozzle syringe with flow rate of 0.2 mL/h (accuracy of 0.01 mL/h) was applied.
  • the applied voltage to the nozzles tips pump syringe was 11-13 kV and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe was 10-14 cm the fibers were collected for 10-20 min.
  • the electrospun nanofibers were heated at (220-300 °C, here for the exemplary sample 230°C here for the exemplary sample 1 hour under ambient atmosphere. Then, the integrated connected network fixed via increasing carbon content and the topology formed and refined at 1000 °C under nitrogen atmosphere for 0.5-2 hour (here for the exemplary sample, 1 hour). The heating rate may be set at 10-20 °C/min, here for the exemplary sample, it was 10°C/min
  • FIG. 14 illustrates a SEM image of an exempalry quantum-size fibrous pattern formed on graphitic cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • the quantum-size fibrous pattern formed on the graphitic cancellous bone-like structures are multilayered porous multiple-scaled of micro, nano, meso and quantum size structures.
  • the patterned bone -like structures have been produced via the post resin treatment on the electrospun pure PAN (13.5 wt. %) in DMF.
  • the substrate of the micro carbon fabric was functionalized by a resin including a thermoplastic resin component and the nanostructures.
  • the bone-like structures have been produced via electrospinning pure PAN (13.5 wt. %) in DMF without PEG, thermoplastic component was included in the resin treatment of the substrate and post resin treatment on the electrospun fibers for this exemplary sample.
  • thermoplastic component was included in the resin treatment of the substrate and post resin treatment on the electrospun fibers for this exemplary sample.
  • a bone tissue-like topology were produced by spinning a solution of 7-16 wt. % PAN (for the exemplary sample here 13.5%) in DMF (without PEG) to form the plurality of carbon-containing fibers.
  • the plurality of carbon-containing fibers were collected on the functionalized substrate and passed through the heat treatments with the functionalized heat resistant and shrinkage resistant substrate (micro carbon fabric).
  • the polymer solution was homogenized using a gentle homogenizer (here, a magnetic stirrer) at room temperature for (0.5-24 h) (here 2 hour).
  • the polymer solution was injected using a dual, single or multi-nozzle pump syringe with flow rate of 0.2-0.6 mL/h, here for the exemplary topology shown in FIG 14, a dual-nozzle syringe with flow rate of 0.26 mL/h (accuracy of 0.01 mL/h) was applied.
  • the applied voltage to the nozzles tips pump syringe was 11-14 kV and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe was 10-14 cm.
  • the process was performed for 20-40 min.
  • a resin post-treatment of one of PVA (aq 5-10%), mixture of the PVA (aq) and (0.1-2% HTCC (aq), mixture of PVA (aq) and/or PEG and (0.1-2% glucose), and combination thereof was applied, consistent with one or more exemplary embodiments of the present disclosure.
  • the integrated fused network and after that fixing and refining the topology via increasing carbon content were applied on the electrospun nanofibers on the functionalized substrate.
  • the electrospun nanofibers were heated at (220-300 °C, here for the exemplary sample shown in FIG 14, 230°C here for the exemplary sample shown in FIG 14, 1 hour under ambient atmosphere.
  • the integrated fused network fixed via increasing carbon content and the topology formed at 1000 °C under nitrogen atmosphere for 0.5-2 hour (here for the exemplary sample shown in FIG 14, 1 hour).
  • the heating rate may be set at 7-20 °C/min, here for the exemplary sample shown in FIG 14, it was 10°C/min.
  • FIG. 15 illustrates a SEM image of exemplary fish-like patterns developed on a micro carbon fabric, consistent with one or more exemplary embodiments of the present disclosure.
  • the micro carbon fabric was nanofunctionalized and the electrospun fibers were also post treated using a layer of resins.
  • FIG. 16 illustrates a SEM image of exemplary multiaxial intertwined woven-like nanostructures formed on a circular/radial-patterned substrate, consistent with one or more exemplary embodiments of the present disclosure.
  • the fibrous nanostructures were formed according to the general method of Example 3.
  • FIG. 17 illustrates a SEM image of exemplary nanoflowers with a carbon shell, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 18 illustrates a SEM image of exemplary rose-shaped nanostructures, consistent with one or more exemplary embodiments of the present disclosure including an intermediate washing performed after electrospinning process on a patterned substrate.
  • FIG. 19 illustrates SEM images of exemplary cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • the cancellous bone-like nanostructures were produced by reducing electrospinning time.
  • the innovative engineered strategies of this invention also include changing various factors such as the type of precursor, polymer mixtures or simple and single-component types, etc., their ratio, adding additives, substrate structures and types, pre-treatments and/or treatments on substrate, application of nanostructures, resins or nanocomposites pre-, after- and/or post-treatments, the production methods and conditions (for instance in the reported examples production methods are based on nanofiber production and production variants are including solution and processing parameters, humidity and ambient conditions, etc. e.g.
  • the products of this method can be converted and used in the form of powder or colloidal solution, gel, paste, etc., which can be easily transferred to other surfaces and goods, and can also be used in the structure or precursor of other products, for example, in mixing with solutions or molten polymers or monomeric materials during in-situ synthesis, and in the same way precursors or intermediary materials for the process of metals, metal alloys, glass, ceramics, rubber, plastic, etc.
  • in-situ synthesis of polymers, alloys, hybrids, different types of composites and modification of the surface or bulk of materials can also be integrated with various molding processes (melt, solution, etc.), such as the production of fibers, nanofibers, films and thin layers, coating, etc., different types of carbon-containing nanofibers including hybrid, multicomponent, hollow, porous, etc., alone or together with other nano, micro, meso, quantumsized, multi-scale structures, etc.
  • the present method disclosed herein may be used for the functionalization of any type of product or material such as hydrogels, resins, polymers, polymer mixtures, micro or non-nano carbon structures, porous, quantum-size, nanoscale or non-nano structures, carriers, carriers, capsules, resin, spinning oil, polymer synthesis precursor, paper, rubber, plastic, banknote, glass, ceramic, and various materials, paste, melt, solution, etc.
  • product or material such as hydrogels, resins, polymers, polymer mixtures, micro or non-nano carbon structures, porous, quantum-size, nanoscale or non-nano structures, carriers, carriers, capsules, resin, spinning oil, polymer synthesis precursor, paper, rubber, plastic, banknote, glass, ceramic, and various materials, paste, melt, solution, etc.
  • the present method disclosed herein may be used with other methods, for example, gel-spinning, dry-spinning, all kinds of melting processes, solution, etc., pad-dry, pad-dry-cure, exhaustion , spraying, printing nanostructures, synthesis, in situ synthesis, spin coating, sol-gel, various spinning process, ultrasound, irradiation, etc.
  • the present method disclosed herein may be used, followed or integrated. In polymer, inorganic, glass, ceramic, metal, alloy and hybrid substrates, hybrid, composite, alloy, porous, patterned, functionalized and/or untreated, template, etc. and in a combination or any set of combinations and synergistic structures with any scale and feature.
  • All components of products based on this disclosure and their direct and indirect effects can be green, safe, renewable, sustainable, eco-friendly, bioinspired, and/or biomimetic. Any additive can be added to the carbon or graphite structures of this invention by developing or growth other materials, such as the production of carbon, graphite, carbon/graphite nanoflowers, etc.
  • Example 6 Analyzing cell viability and biocompatibility of produced nanostructures
  • ELISA readers or micro plate readers is an analytical instrument for spectrophotometry and evaluation the color difference values which is compatible with a 96- well plate. The evaluation is based on emitting a light beam at the specific wavelength, and recording the density of the absorbed beam by the sample in each well.
  • FIG. 20 illustrates a SEM image of cell attachment on exemplary produced nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
  • TCPs tissue culture polystyrene
  • the architectural effect (the effect of topology) of the porous scaffold is so dominant in this disclosure that even with the relative hydrophobicity of the surface and without any subsequent process, coating, or surface modification, it has led to excellent cell adhesion. It is obvious that the use of appropriate biopolymer coatings and other biomaterials, etc., can significantly improve these unique results and mark a new era in biomedical applications with a perspective to help the patients. At the same time, due to simulating bone tissue, the structures based on it can meet the amazing properties of bone, such as bearing load and pressure, and response the challenge of the weakness of biomaterials in tissue engineering, especially load-bearing hard tissue engineering.
  • Nanostructures may be applicable for different applications such as medicine (such as drug delivery, bone tissue engineering, etc.), agriculture, water purification, etc. Designing the process of synthesizing nanostructures by changing the thermoplastic material, the temperature of curing, functionalizing the substrate, adding additives, engineering of solution and production parameters, etc. can change the topology of nanostructures.

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Abstract

Disclosed herein is a method for controlling topology of carbon-rich nanostructures. The method includes forming a plurality of carbon-containing fibers using a mixture containing a carbon fiber precursor, forming a two or multi-phase system by adding at least one thermoplastic material with a melting point below 450 ºC to the plurality of carbon-containing fibers, forming a nanostructured network by forming a plurality of thermoplastic connections among the plurality of carbon-containing fibers, and increasing carbon content of the nanostructured network by removing at least one non-carbon containing element in form of gases from the nanostructured network. Forming the nanostructured network includes melting the thermoplastic material among the plurality of carbon-containing fibers. Removing the non-carbon containing element includes heating the nanostructured network to a temperature of at least 800 ºC under an inert atmosphere.

Description

ENGINEERING OF STEADY TOPOLOGY-CONTROLLED NANOFIBROUS
STRUCTURES BASED ON TISSUE ENGINEERING PERSPECTIVE
TECHNICAL FIELD
[0001] The present disclosure generally relates to a method for controlling topology of carbon- rich nanostructures, and more particularly, relates to a method for forming and processing an integrated fused carbon-containing fibrous network using thermoplastic connections.
BACKGROUND ART
[0002] Fabrication of intertwined woven-like nanostructures is an ideal vision for reinforcement of bone-cements especially for regenerating of load-bearing bones’ defects. Bones are organs of a body which are made of living tissues. Bones are made of calcium salts deposited around protein fibers and can provide a structural support for a living body. Cancellous structure of bones can provide cell migration inside bones and guarantee their viability. Minerals used in cancellous structure of bones can provide rigidity and proteins such as collagen can provide strength and also elasticity of bones. Some diseases associated with bones, like osteonecrosis or cancer can deteriorate bones. Therefore, involved patients may require bone graft. Cancellous bone has an amazing structure with many known and certainly yet unknown mysterious features. Since morphology and topology of a cancellous bone can be detected by cells and mainly effect their behavior, developing cancellous bone-like nanostructure can be a great help especially for hard tissue engineering.
[0003] Production of bio-tissue-like structures may be done by forming nanofibrous structures. Nanofibrous structures suffer from drawbacks such as shrinkage, swelling, and deformation of nanofibrous structures. The mentioned drawbacks can block pores inside a cancellous structure of bones which can limit cell growth only on a surface of bones. Therefore, a core section of bones may suffer from weakness. Considering biocompatibility of carbon nanostructures, fixing topology of fibrous nanostructures via increasing carbon content may be considered to prevent shrinkage, swelling, deformation, etc. However, engineering topology of a carbon nanostructure especially via a scalable, cost-effective technique, and affordable for public is a great challenge.
[0004] Nowadays one of the most exciting challenges is using a method to produce bone-like structures. Li-Heng Kao et al. presented a paper on “Electrospun hierarchical cancellous-bone- like microstructures composed of a crystalline TiO nanonet” vol 82, 2012, 64-66. Li-Heng Kao et al. used titanium dioxide (TiCh) nanoparticles, polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), and titanium isopropoxide (TTIP) in acetic acid and ethanol media to form an electrospinning solution. Li-Heng Kao et al. also used silicate mold to produce bonelike nanostructures. They used a solution of NaOH to dissolve and remove the template. Removing the template has been followed by filtration, rinsing and drying at the end of their procedures. Aref Fakhrali et al. presented a paper on “Electrospun PGS/PCL nanofibers: From straight to sponge and spring-like morphology” in Journal of Polymer Advanced Technologies, 2020, 1-16. Aref Fakhrali et al. used polycaprolactone (PCL) and polyglycerol sebacate (PGS) and acetic acid as a solvent to produce bone-like structures. They used an electrospinning method to produce the bone-like structures. However, these proposed methods suffer from shrinkage, swelling, and deformation of the produced structures, and/or require a template for producing bone-like structures.
[0005] There is, therefore, a need for a method to control topology of carbon-rich nanostructures. There is further a need for a cost-effective and easy-scalable method to produce safe and biocompatible controlled-topology carbon-rich nanostructures without shrinkage, swelling, and deformation of nanostructures.
SUMMARY OF THE DISCLOSURE
[0006] This summary is intended to provide an overview of the subject matter of this patent, and is not intended to identify essential elements or key elements of the subject matter, nor is it intended to be used to determine the scope of the claimed implementations. The proper scope of this patent may be ascertained from the claims set forth below in view of the detailed description below and the drawings.
[0007] In one general aspect, the present disclosure is directed to a method for forming at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bonetissue like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fishlike nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof. In an exemplary embodiment, an exemplary method may include functionalizing a substrate, forming a plurality of carbon-containing fibers on an exemplary substrate using a mixture containing a carbon fiber precursor, forming a two or multi-phase structure, forming a nanostructured network, and increasing carbon content of an exemplary nanostructured network. In an exemplary embodiment, an exemplary method may include functionalizing an exemplary substrate by at least one of adding a layer of a resin on an exemplary substrate, adding a layer of at least one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of an electrically conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof. In an exemplary embodiment, an exemplary method may include forming a two or multi -phase structure by adding at least one thermoplastic material to an exemplary plurality of carbon- containing fibers. In an exemplary embodiment, an exemplary at least one thermoplastic material may have a melting point below 450 °C. In an exemplary embodiment, an exemplary method may include forming a nanostructured network by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon- containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450 °C. In an exemplary embodiment, an exemplary nano structured network may include a plurality of carbon-containing fibers connected to each other via an exemplary plurality of thermoplastic connections. In an exemplary embodiment, an exemplary method may include forming a carbon-rich nanostructure by increasing carbon content of an exemplary nanostructured network via removing at least one non-carbon containing element in form of gases from an exemplary nano structured network. In an exemplary embodiment, removing an exemplary at least one non-carbon containing element may include heating an exemplary nanostructured network to a temperature of 800 °C or more under an inert atmosphere. In an exemplary embodiment, an exemplary method may include adding an additive to an exemplary carbon-rich nanostructure by coating a layer of an exemplary additive with a thickness up to 1 mm on an exemplary carbon-rich nanostructure. In an exemplary embodiment, an exemplary additive may include at least one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, an electrolyte, and combinations thereof.
[0008] In a more general aspect, the present disclosure is directed to a method for controlling topology of carbon-rich nanostructures. In an exemplary embodiment, an exemplary method may include forming a plurality of carbon-containing fibers using a mixture containing a carbon fiber precursor, forming a two or multi-phase system, forming a nanostructured network, and increasing carbon content of the nano structured network. In an exemplary embodiment, an exemplary method may include forming a two or multi-phase system by adding at least one thermoplastic material to an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, an exemplary thermoplastic material may have a melting point below 450 °C. In an exemplary embodiment, an exemplary method may include forming a nano structured network by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon-containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450 °C. In an exemplary embodiment, an exemplary nanostructured network may include a plurality of carbon- containing fibers connected to each other via an exemplary plurality of thermoplastic connections. In an exemplary embodiment, an exemplary method may include increasing carbon content of an exemplary nano structured network by removing at least one non-carbon containing element in form of gases from an exemplary nanostructured network. In an exemplary embodiment, removing an exemplary at least one non-carbon containing element may include heating an exemplary nanostructured network to a temperature of at least 800 °C under an inert atmosphere.
[0009] In an exemplary embodiment, controlling an exemplary topology of an exemplary carbon-rich nanostructures may include forming one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharpfold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof.
[0010] In an exemplary embodiment, an exemplary carbon fiber precursor may include at least one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, and combinations thereof.
[0011] In an exemplary embodiment, forming an exemplary plurality of carbon-containing fibers may include forming an exemplary plurality of carbon-containing fibers utilizing a process including at least one of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet- electrospinning, wet or gel electrospinning, and combinations thereof.
[0012] In an exemplary embodiment, an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, a poly(amidoamine) (PAMAM), a silicone, a silicone compound, a poysiloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, and combinations thereof.
[0013] In an exemplary embodiment, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers may include at least one of adding an exemplary at least one thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers after forming an exemplary plurality of carbon- containing fibers, and combinations thereof.
[0014] In an exemplary embodiment, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process including at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) elctro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented- nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electrocentrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel-electro/spinning, sequential layer by layer fiber forming/electrospinning, a post- electrospinning, and combinations thereof.
[0015] In an exemplary embodiment, heating an exemplary two or multi-phase structure to a temperature up to 450°C may include heating an exemplary two or multi-phase structure to an exemplary temperature up to 450°C under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof. In an exemplary embodiment, an exemplary inert gas may include at least one noble gas.
[0016] In an exemplary embodiment, forming an exemplary plurality of carbon-containing fibers may include forming an exemplary plurality of carbon-containing fibers on a substrate. In an exemplary embodiment, an exemplary substrate may include at least one of a fabric, a layer, a film, a paper, a sheet, a lace, a web, and combination thereof of a heat resistant material, a carbon-forming material, a graphite-forming material, a carbon/ graphite-forming material, a substrate may be configured to be separated from an exemplary nanostructured network before a heating process to a temperature above 200°C, and combinations thereof.
[0017] In an exemplary embodiment, an exemplary substrate may include at least one of a carbon fabric, a micro-carbon fabric, a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a layer of polysaccharide derivatives, lignin, lignocellulose, a carbohydrates, a carbohydrate derivatives, polyacrylonitriles, a metal sheet, a layer of mercerized cellulose, polyester laces, and combinations thereof.
[0018] In an exemplary embodiment, forming an exemplary plurality of carbon-containing fibers may further include functionalizing an exemplary substrate by at least one of adding a layer of a resin on an exemplary substrate, adding a layer of an exemplary at least one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of a conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof.
[0019] In an exemplary embodiment, an exemplary plurality of nanostructures may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO) a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPS ). Strontium stannate (SrSnos), Tungsten ditelluride (WTc ). Potassium heptafluorotantalate (TGTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBs), Niobium disulfide (NbSi), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof.
[0020] In an exemplary embodiment, an exemplary plurality of nanostructures may include at least one of a hydroxide, a salt, a composite, an oxide, a framework, and combinations thereof may include at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), chalcogenides, molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof.
[0021] In an exemplary embodiment, an exemplary resin may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, a carbohydrates, a polysaccharide, a carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), an acrylic resin, a silicone, a polysiloxane, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, hydrogels, acrylates, poly(sodium acrylate), a polyimide, poly(amidoamine) (PAMAMs), polyaniline, polysiloxane derivatives, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS metal compounds, an electrolyte, MOFs, softeners, and combinations thereof.
[0022] In an exemplary embodiment, an exemplary method may further include adding an additive to at least one of an exemplary mixture containing a carbon fiber precursor, an exemplary thermoplastic material, an exemplary carbon-rich nanostructure, and combination thereof. In an exemplary embodiment, an exemplary additive may include at least one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, a hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, BETS metal compounds, an electrolyte, and combinations thereof.
[0023] In an exemplary embodiment, an exemplary additive may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, carbohydrates, polysaccharide, carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), acrylic resins, silicones, poly siloxanes, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, a hydrogels, acrylates, poly(sodium acrylate), polyimides, a poly(amidoamine) (PAMAMs), a polyaniline, polysiloxane derivatives proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS metal compounds, an electrolyte, metal-organic frameworks (MOFs), softeners, a metal oxide, Silicon (Si), Boron (B), phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanotubes (CNTs), fullerene, graphene and graphene-based materials, graphene oxide (GO), a magnetic material, hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPSs). Strontium stannate (SrSnos). Tungsten ditelluride (WTe2), Potassium heptafluorotantalate (K^TaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBi), Niobium disulfide (NbSi), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Lead (Pb), Iridium (Ir), Cobalt (Co), Nickel (Ni), Vanadium (V), tungsten (W), Tin (Sn), molybdenum (Mo), tellurium (Te), niobium (Nb), iron (Fe), palladium (Pd), strontium (Sr), an oxide of at least one of Cu, Zn, Fe, Mn, Ti, Mg, Mo, Si, chalcogenides, a salt comprising at least one of chalcogenides, Ag, Cu, Zn, Fe, V, Ni, Co, Ir, Pb, Mn, Au, Pt, Ti, W, Sn, Mo, Te, Nb, Pd, and Sr, and combinations thereof.
[0024] In an exemplary embodiment, an exemplary nanostructured additive may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO) a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPS ). Strontium stannate (SrSnos), Tungsten ditelluride (WTc ). Potassium heptafluorotantalate (KiTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBs), Niobium disulfide (NbSi), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), at least one of a hyroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), chalcogenides, Vanadium (V), Tungsten (W), and combinations thereof.
[0025] In an exemplary embodiment, an exemplary method may further include at least one of washing an exemplary carbon-rich nanostructure with at least one of an organic solvent, an aqueous solution, and combination thereof, washing an exemplary plurality of carbon- containing fibers with at least one of an organic solvent, an aqueous solution, and combination thereof, washing an exemplary nanostructured network with at least one of an organic solvent, an aqueous solution, and combination thereof, purification at least one of an exemplary carbon- rich nanostructure, an exemplary plurality of carbon-containing fibers, an exemplary nanostructured network, and combinations thereof using at least one of an acid solution, a basic solution, an oxidant solution, an organic solution, and combination thereof, in-situ synthesis of a nanostructured additive using at least one of a hydrothermal process, a solvothermal process, a chemical reduction/oxidation, irradiation, a thermal process, and combination thereof, eliminating a component before or after forming an exemplary nanostructured network using at least one of an organic solvent, an acid solution, a basic solution, an oxidant solution, water, and combination thereof, and combination thereof.
[0026] In an exemplary embodiment, an exemplary carbon-rich nanostructures may include one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially- carbon-rich nanocomposite, and combination thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The drawing figures depict one or more implementations in accord with the present teachings, by way of example only, not by way of limitation. In the figures, like reference numerals refer to the same or similar elements.
[0028] FIG. 1A illustrates a flowchart of a method for controlling topology of carbon-rich nanostructures, consistent with one or more exemplary embodiments of the present disclosure; [0029] FIG. IB illustrates a flowchart of a method for controlling topology of carbon-rich nanostructures using a substrate, consistent with one or more exemplary embodiments of the present disclosure;
[0030] FIG. 2A illustrates a field emission scanning electron microscopy (FESEM) image of intertwined woven-like nanocomposite nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0031] FIG. 2B illustrates a magnified FESEM image of exemplary intertwined woven-like nanocomposite nanostructures shown in FIG. 2A, consistent with one or more exemplary embodiments of the present disclosure;
[0032] FIG. 3A illustrates a FESEM image of exemplary dome-shaped intertwined woven- like nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0033] FIG.3B illustrates a magnified FESEM image of exemplary dome-shaped intertwined woven-like nanostructures shown in FIG. 3A, consistent with one or more exemplary embodiments of the present disclosure;
[0034] FIG. 4 illustrates a scanning electron microscopy (SEM) image of exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure; [0035] FIG. 5 illustrates an Energy-dispersive X-ray spectroscopy (EDX) diagram for exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0036] FIG. 6 illustrates a SEM image of exemplary bone tissue-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0037] FIG. 7A illustrates Fourier transform infrared (FTIR) -attenuated total reflection (ATR) (FTIR-ATR) spectrums of exemplary electrospun fibers and nanocomposites after an exemplary fixing and refining process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0038] FIG. 7B illustrates FTIR-ATR spectrums of exemplary electrospun bone tissue-like nanostructures before forming an exemplary integrated fused network and after an exemplary fixing process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0039] FIG. 8 illustrates a thermogravimetric analysis (TGA) spectrum after an exemplary fixing process in form of carbon nanostructures for exemplary bone tissue-like nanostructure, consistent with one or more exemplary embodiments of the present disclosure;
[0040] FIG. 9 illustrates a Raman spectroscopy spectrum for exemplary bone tissue-like nanostructure after an exemplary fixing process in form of carbon, consistent with one or more exemplary embodiments of the present disclosure;
[0041] FIG. 10 illustrates a SEM image of a micro carbon fabric substrate modified by clay nano layers, consistent with one or more exemplary embodiments of the present disclosure;
[0042] FIG. 11 illustrates a SEM image of an exemplary functionalized micro carbon fabric modified with inorganic nanoparticles and resins, consistent with one or more exemplary embodiments of the present disclosure;
[0043] FIG. 12 illustrates a SEM image of exemplary functionalized micro carbon fabric modified with clay nano layers and resins, consistent with one or more exemplary embodiments of the present disclosure;
[0044] FIG. 13 illustrates a SEM image of exemplary bone tissue-like nanostructures formed on an exemplary functionalized substrate, consistent with one or more exemplary embodiments of the present disclosure; [0045] FIG. 14 illustrates a SEM image of an exemplary quantum-size fibrous pattern formed on graphitic cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0046] FIG. 15 illustrates a SEM image of exemplary fish-like patterns developed on a micro carbon fabric, consistent with one or more exemplary embodiments of the present disclosure;
[0047] FIG. 16 illustrates a SEM image of exemplary multiaxial intertwined woven-like nanostructures formed on a circular/radial-patterned substrate, consistent with one or more exemplary embodiments of the present disclosure;
[0048] FIG. 17 illustrates a SEM image of exemplary nanoflowers with a carbon shell developed on graphitic cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0049] FIG. 18 illustrates a SEM image of exemplary rose-shaped nanostructures, consistent with one or more exemplary embodiments of the present disclosure;
[0050] FIG. 19 illustrates SEM images of exemplary cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure; and
[0051] FIG. 20 illustrates a SEM image of cell attachment on exemplary produced nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
DESCRIPTION OF EMBODIMENTS
[0052] In the following detailed description, numerous specific details are set forth by way of examples in order to provide a thorough understanding of the relevant teachings. However, it should be apparent that the present teachings may be practiced without such details. In other instances, well known methods, procedures, components, and/or circuitry have been described at a relatively high-level, without detail, in order to avoid unnecessarily obscuring aspects of the present teachings. The novel features which are believed to be characteristic of the present disclosure, as to its structure, organization, use and method of operation, together with further objectives and advantages thereof, will be better understood from the following discussion. In the following detailed description, numerous specific details are set forth by way of examples in order to provide a thorough understanding of the relevant teachings. However, it should be apparent that the present teachings may be practiced without such details. In other instances, well known methods, procedures, components, and/or circuitry have been described at a relatively high-level, without detail, in order to avoid unnecessarily obscuring aspects of the present teachings. The following detailed description is presented to enable a person skilled in the art to make and use the methods and devices disclosed in exemplary embodiments of the present disclosure. For purposes of explanation, specific nomenclature is set forth to provide a thorough understanding of the present disclosure. However, it will be apparent to one skilled in the art that these specific details are not required to practice the disclosed exemplary embodiments. Descriptions of specific exemplary embodiments are provided only as representative examples. Various modifications to the exemplary implementations will be readily apparent to one skilled in the art, and the general principles defined herein may be applied to other implementations and applications without departing from the scope of the present disclosure. The present disclosure is not intended to be limited to the implementations shown, but is to be accorded the widest possible scope consistent with the principles and features disclosed herein.
[0053] The present disclosure is directed to exemplary embodiments of a method for controlling topology of carbon-rich nanostructures. In an exemplary embodiment, an exemplary topology of an exemplary carbon-rich nanostructures may be controlled by selection of appropriate production/processing parameters and compounds used for producing an exemplary carbon-rich nanostructures. Herein, “carbon-rich nanostructures” refers to compositions containing high percent of at least one of carbon, graphite, graphite/carbon and combinations thereof. “Carbon-rich nanostructures” may also refer to a carbon-rich nanocomposite. In this case, an exemplary carbon-rich component in a carbon-rich nanocomposite may refer to a composition containing high percent of at least one of carbon, graphite, graphite/carbon and combinations thereof. In an exemplary embodiment, carbon-rich nanostructures may be formed by forming a plurality of carbon-containing structures on a substrate, forming a two or multi-phase system by adding at least one meltable material at temperatures below about 450 °C to exemplary plurality of carbon-containing structures, forming a nanostructured network by melting an exemplary meltable material among exemplary plurality of carbon-containing structures, and increasing carbon content of an exemplary nanostructured network. In an exemplary embodiment, an exemplary meltable material may include a thermoplastic material. In an exemplary embodiment, an exemplary plurality of carbon-containing structures may include a plurality of carbon-containing fibers. In an exemplary embodiment, exemplary carbon-rich nanostructures may include at least one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially-carbon-rich nanocomposite, and combination thereof. In an exemplary embodiment, exemplary carbon- rich nanostructures may have a convoluted, wavy, spiral, porous, intertwined, angled, branched, networked (integrated network), fibrous, hollow, patterned of nano, micro, meso, and quantum sized structures. In an exemplary embodiment, exemplary carbon -rich nanostructures may include at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopatterned carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof. In an exemplary embodiment, exemplary carbon- rich nanostructures may include at least one of woven-like carbon-rich nanocomposite nanostructures, bone-like carbon-rich nanocomposite nanostructures, bone-tissue like carbon- rich nanocomposite nanostructure, multiaxial intertwined woven-like nanocomposite nanostructures, fish-like nanopatterned carbon-rich nanocomposites, dome-shaped intertwined woven-like nanocomposite nanostructures, quantum size fibrous nanocomposite nanostructures, sharp-fold controlled-topology nanocomposite nanostructures, hollow sphere bone-tissue like shell nanocomposites, multi-scaled multilayer micro, nano, meso, quantum sized structures, multi-scaled multilayer nanocomposite, nano-curvature graphitic structures with twisted layers, nano-waved graphitic structures with twisted layers, nano-curvature graphitic integrated network nanocomposites with twisted layers, and nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted layers.
[0054] In an exemplary embodiment, forming exemplary carbon-rich nanostructures may include forming a plurality of carbon-containing structures. In an exemplary embodiment, an exemplary carbon containing structure may include a plurality of carbon-containing fibers. In an exemplary embodiment, forming an exemplary plurality of carbon-containing fibers may be performed by a process including at least one of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel electrospinning, and combinations thereof. In an exemplary embodiment, an exemplary plurality of carbon-containing fibers may include one of nano, micro, and multiple scaled fibers. In an exemplary embodiment, one carbon-rich precursor may be used to form an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, an exemplary carbon-rich precursor may include one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, and combinations thereof. In an exemplary embodiment, an exemplary polysaccharide may include one of N-[(2-hydroxy-3- trimethyl ammonium) propyl] chitosan (HTCC), lignin, etc., and combinations thereof. Carbohydrates may refer to materials with a molecular structure of carbon, oxygen, and hydrogen where molecular formula of carbohydrates may usually be modeled as Cm(H2O)n, like glucose, maltose, mono, oligo or poly saccharides, etc. In an exemplary embodiment, exemplary carbohydrates may include at least one of glucose amine, chitosan, chitin, alginate, heparin, and combinations thereof. In an exemplary embodiment, carbohydrate may include synthetic derivatives and natural derivatives of carbohydrates and impure carbohydrates. Saccharides may be the most abundant carbohydrates in nature and in biomolecules (e.g. plants), etc. In an exemplary embodiment, exemplary natural sources of saccharides or polysaccharides may include starch, cellulose, cotton, glycogens, etc. As used herein, the word “saccharide” may also refer to processed or impure saccharide materials, synthetic saccharide derivatives, and their natural derivatives.
[0055] In an exemplary embodiment, an exemplary carbon-containing structure may be formed on a substrate. In an exemplary embodiment, an exemplary substrate may interact with an exemplary plurality of carbon-containing structures. In an exemplary embodiment, to achieve a microdynamic control on thermal shrinkage, topology, and morphology of exemplary carbon- rich nanostructures, a heat-compatible substrate may be used. In an exemplary embodiment, an exemplary heat-compatible substrate may include at least one of heat and shrinkage resistant materials (e.g. a carbon fabric, a micro-carbon fabric, glass fabrics, etc.), a carbon, a graphite-, a carbon/ graphite-forming material and combinations thereof. In an exemplary embodiment, an exemplary substrate may interact with an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, an exemplary substrate may include one of acrylic substrates (including polyacrylonitrile and its derivatives, modacrylics, etc.), polysaccharide and mercerized cellulose substrates, such as cotton, viscose, lignin, and lignocellulose, a film of graphene oxide (GO) nano layers/fibers, carbon substrate including fiber and carbon fabric with any biaxial, uniaxial, multiaxial, micro, nano, etc. structure, and their combinations, any forms of fabric, film, paper, lace, etc., in simple, patterned, printed, embossed, etc., which can be combined with an exemplary carbon-containing structure. In an exemplary embodiment, an exemplary substrate with an exemplary carbon-containing structure thereon may be subjected to a thermal procedure. In an exemplary embodiment, an exemplary interaction of an exemplary substrate with an exemplary plurality of carbon-containing fibers may be in form of physical contact, friction with an exemplary plurality of carbon-containing fibers or a stronger conflict.
[0056] In an exemplary embodiment, an exemplary substrate may be functionalized before forming an exemplary plurality of carbon-containing structures on an exemplary substrate. In an exemplary embodiment, functionalizing a substrate may be designed so that a smart selfactivated micro dynamic control mechanism via nanorough friction and/or resin attachment may be created (added) on an exemplary substrate. In an exemplary embodiment, to achieve microdynamic control on thermal shrinkage, topology, and morphology of exemplary carbon- rich nanostructures, a heat-compatible substrate may be used. In an exemplary embodiment, an exemplary heat-compatible substrate may include one of a fabric, layer, film, paper, sheet, lace, web, and combinations thereof. In an exemplary embodiment, an exemplary heat-compatible substrate may include one of a heat resistant material, carbon material, graphite-forming material, carbon/ graphite-forming material, and combinations thereof. In an exemplary embodiment, an exemplary heat resistant material may include at last one of a carbon fabric, a micro-carbon fabric, a glass fabric, and combinations thereof. In an exemplary embodiment, an exemplary carbon/ graphite-forming material may include at least one of a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a polysaccharide derivative, lignin, lignocellulose, carbohydrates, carbohydrate derivatives, polyacrylonitriles, a film of graphene oxide (GO), and combinations thereof. In an exemplary embodiment, an exemplary substrate may include one of a carbon fabric, a micro-carbon fabric, a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a layer of polysaccharide derivatives, lignin, lignocellulose, a carbohydrate, a carbohydrate derivative, polyacrylonitriles, a metal sheet, a layer of mercerized cellulose, polyester laces, and combinations thereof. In an exemplary embodiment, an exemplary substrate may be functionalized by one of adding a layer of a resin on an exemplary substrate, adding a layer of one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of an electrically conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof. In an exemplary embodiment, an exemplary nano roughness resulting from coatings created with inorganic nanostructures may be considered to create nano roughness (friction) and use an exemplary friction to control movement, shrinkage, and also keep an exemplary plurality of carbon-containing nanofibers at certain places and prevent them from sticking and uncontrolled clumping. Therefore, an exemplary nano roughness may help to create curves, special spaces between curves, applying tension by dealing with thermal shrinkage microdynamically during an exemplary heating process to increase an exemplary arrangement of chains, etc., and an exemplary guidance of topology and morphology of an exemplary plurality of nano fibers. In an exemplary embodiment, use of resins and applying changes in thermal processes (such as temperature and duration of an exemplary thermal process) may also help to control topology of an exemplary plurality of carbon-containing nanofibers. In addition, a melting component or a thermoplastic material can also be included during an exemplary thermal process to exemplary carbon-containing nanofibers. The present disclosure may also directed to exemplary dynamic and microdynamic methods of controlling thermal shrinkage of an exemplary plurality of carbon-containing nanofibers as well as thermal processes in nano and atomic scale. In an exemplary embodiment, a resin may be used for functionalizing an exemplary substrate where an exemplary resin may activate an exemplary microdynamic mechanism at different stages of an exemplary thermal process by intelligently fusing an exemplary carbon-containing nanofibers to surface of an exemplary substrate. Therefore, tendency of an exemplary carbon-containing nanofibers to thermal shrinkage may increase with increasing temperature. In an exemplary embodiment, a combination of three fusing mechanisms including fusing in nano scale or larger, nano friction and roughness as well as nano fiber entanglement in nanometer spaces between nano structures can be considered together. [0057] Moreover, adding magnetic/nanomagnetic materials on an exemplary substrate may form magnetic/nanomagnetic patterns. In an exemplary embodiment, magnetic/nanomagnetic patterns formed on an exemplary substrate, etc., may provide a possibility of using magnetic forces to guide and control topology of an exemplary plurality of carbon-containing nanofibers. In an exemplary embodiment, functionalizing an exemplary substrate with magnetic/nanomagnetic patterns may further include adding magnetic/nanomagnetic materials to an exemplary substrate. In an exemplary embodiment, exemplary magnetic/nanomagnetic patterns may also be used to control the morphology of an exemplary plurality of carbon- containing nanofibers. In these cases, an exemplary substrate may be separated from an exemplary plurality of carbon-containing nanofibers or may be processed along with an exemplary plurality of carbon-containing nanofibers.
[0058] In an exemplary embodiment, an exemplary plurality of nanostructures added to an exemplary substrate may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphenebased materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPSy). Strontium stannate (SrSnos). Tungsten ditelluride (WTc ). Potassium heptafluorotantalate (KiTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgEb), Niobium disulfide (NbSs), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof. In an exemplary embodiment, an exemplary plurality of nanostructures may inlcude at least one of a hyroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), chalcogenides, molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof. In an exemplary embodiment, an exemplary resin may include one of PEG, polyvinylpyrrolidone (PVP), chitosan, a carbohydrates, a polysaccharide, a carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), an acrylic resin, silicone, a poly siloxane, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, hydrogels, acrylates, poly(sodium acrylate), a polyimide, poly(amidoamine) (PAMAMs), polyaniline, polysiloxane derivatives, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, MOFs, softeners, and combinations thereof. In an exemplary embodiment, functionalizing an exemplary substrate may use smartly self-activated microdynamic control mechanism via nanorough friction and/or resin attachment via functionalizing an exemplary substrate by adding one of a layer of a resin, a layer of an exemplary thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, conductive materials, etching an exemplary surface, and combinations thereof on an exemplary substrate.
[0059] In an exemplary embodiment, a two or multi-phase structure may be formed by adding at least one thermoplastic material to an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, an exemplary thermoplastic material may be added before, after, or during production of an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, an exemplary thermoplastic material may have a melting point below about 450 °C. In an exemplary embodiment, an exemplary phase made of an exemplary thermoplastic material may make connection sites among an exemplary plurality of carbon-containing nanofibers when an exemplary thermoplastic material melts at the meeting sites of an exemplary plurality of fibers/nanofiber crossing. In an exemplary embodiment, an exemplary melted thermoplastic material may form connections between an exemplary plurality of carbon-containing nanofibers. In an exemplary embodiment, instead of or together with an exemplary thermoplastic material, a fusible material may be used. In an exemplary embodiment, melting point of an exemplary fusible material may be below about 450 °C. In an exemplary embodiment, an exemplary fusible material may include a salt, a nanostructured salt, for example, zinc chloride or zinc nitrate. In an exemplary embodiment, an exemplary fusible material may include a metal, for example, zinc. In an exemplary embodiment, an exemplary fusible material may include an oil, for example, a paraffin in form of an emulsion, a dissolvable capsule, or Phase Change Materials (PCMs). In an exemplary embodiment, type, composition, and percentage of materials, and production conditions may be selected in such a way that an exemplary thermoplastic or an exemplary thermoplastic material in a mixture of an exemplary plurality of nanofibers may have a tendency to form a two-phase system when an exemplary mixture of an exemplary plurality of nanofibers is subjected to an exemplary selected processing condition after leaving a nozzle in a production procedure of an exemplary two or multi-phase structure. In an exemplary embodiment, an exemplary thermoplastic material or meltable components or elements of an exemplary thermoplastic or an exemplary meltable components may have a tendency to form a two-phase system or to create a two-phase system after an exemplary thermoplastic material or an exemplary meltable component exit a nozzle. In an exemplary embodiment, an exemplary two-phase system may be formed due to solvent evaporation and/or exposure of an exemplary thermoplastic material or exemplary meltable components to exemplary exiting forces during electrospinning process (or other procedures) with the conditions selected for an exemplary process of electrospinning, etc. and/or exposure to environmental conditions of the process (such as humidity, etc.). In an exemplary embodiment, an exemplary formed two/multi-phase system may include some elements of at least one of the thermoplastic and/or the meltable materials and combinations thereof.
[0060] In an exemplary embodiment, an exemplary substrate may be separated from an exemplary carbon-containing structure before heating to a temperature above 200°C. In an exemplary embodiment, an exemplary substrate, including polyester laces, may be separated from an exemplary carbon-containing structure before heating to a temperature above 200°C. In an exemplary embodiment, adding an exemplary thermoplastic material to an exemplary plurality of carbon-containing fibers may include one of adding an exemplary thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary thermoplastic material to an exemplary substrate, adding an exemplary thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers after forming an exemplary plurality of carbon-containing fibers, and combinations thereof. In an exemplary embodiment, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process of at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) electro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electroblowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel-electro/spinning, sequential layer by layer fiber forming/electrospinning, a post-electrospinning, and combinations thereof. In an exemplary embodiment, a nanostructured network may be formed by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon- containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450°C. In an exemplary embodiment, heating an exemplary two or multi-phase structure to a temperature up to 450°C may include heating an exemplary two or multi-phase structure to an exemplary temperature up to 450°C under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof. In an exemplary embodiment, an exemplary inert gas may include at least one noble gas. In an exemplary embodiment, an exemplary two or multiphase structure may be separated from an exemplary substrate when applying a temperature of at least 200°C to an exemplary two or multi-phase structure. In an exemplary embodiment, an exemplary heating process may result in connecting exemplary carbon-containing fibers to each other, and/or connecting exemplary carbon-containing fibers to an exemplary substrate, and combinations thereof via a plurality of connections made by at least one melted component of an exemplary thermoplastic material. In an exemplary embodiment, an exemplary nanostructured network may include a plurality of carbon-containing fibers connected to each other via an exemplary plurality of thermoplastic connections. In an exemplary embodiment, an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, apoly(amidoamine) (PAMAM), a silicone, a silicone compound, a poy siloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, poly or oligo or monoacrylates, nanostructures, salts (such as zinc nitrate), elements (such as zinc), mixtures of mentioned materials above with of at least one of protein compounds, oligomers, co- or tri-polymers, amphiphilics, macromolecules, superstructures, biomaterials, metamaterials, softeners, a carbon fiber precursor, (e.g. PAN, polysaccharides, lignin, lignocellulose), and combinations thereof in form of polymer, resin, oligomer, macromolecule, capsule, dendrimer, liposome, micelle, hybrid, composite, nanocomposite, organic/mineral compound, and combinations thereof. In an exemplary embodiment, each of “polyacrylonitriles”, “polyacrylonitrile”, and “PAN” may refer to copolymers, modacrylics, tripolymers, derivatives thereof, and modified materials based on polyacrylonitriles, polyacrylonitrile, and PAN as well as polyacrylonitriles, polyacrylonitrile, and PAN .
[0061] In an exemplary embodiment, adding at least one thermoplastic material and/or a meltable material to an exemplary plurality of an exemplary carbon fiber precursor-containing nanofibers, in a way to form a two/multi phased system may include a plurality of at least one of exemplary thermoplastic material elements and/or a meltable material elements along with an exemplary plurality of at least one of the carbon fiber precursor-containing nanofibers elements. In an exemplary embodiment, an exemplary thermoplastic material and/or a meltable material may have a melting point below 450 °C. In an exemplary embodiment, while a melting process exemplary elements of an exemplary thermoplastic material and/or a meltable material may form connections at an exemplary meeting points of exemplary nanofibers crossing [0062] In an exemplary embodiment, an exemplary nanostructured network may be heated to form a carbon-rich nanostructure. In an exemplary embodiment, an exemplary process of forming a carbon-rich nanostructure by heating an exemplary nano structured network may include a carbonization process. In an exemplary embodiment, an exemplary nanostructured network may be separated from an exemplary substrate before an exemplary carbonization process when an exemplary substrate undergo undesirable shape changes during an exemplary carbonization process (such as aluminum, polypropylene, polyester). In an exemplary embodiment, an exemplary nano structured network may be heated after separating an exemplary nanostructured network from an exemplary substrate/functionalized substrate. In an exemplary embodiment, an exemplary nanostructured network may be heated in a furnace at a temperature of at least 800°C. In an exemplary embodiment, carbon content of an exemplary nanostructured network may increase by removing at least one non-carbon containing element in form of gases from an exemplary nanostructured network. In an exemplary embodiment, removing an exemplary at least one non-carbon containing element may include heating an exemplary nanostructured network to a temperature of at least 800 °C under an inert atmosphere. In an exemplary embodiment, during an exemplary heating process, non-carbon elements such as oxygen, nitrogen, hydrogen, halogens, and combinations thereof may be released from an exemplary nanostructured network in form of gases. In an exemplary embodiment, exemplary released gases may include at least one of hydrogen cyanide (HCN), (nitrogen) N2, water (H2O), and combinations thereof. In an exemplary embodiment, heating an exemplary nanostructured network may increase carbon content of an exemplary nanostructured network. In an exemplary embodiment, an exemplary formed carbon-rich nanostructure may include at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon- rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopatterned carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof. In an exemplary embodiment, an exemplary carbon-rich nanostructure may include at least one of woven-like carbon-rich nanocomposite nanostructures, bone-like carbon-rich nanocomposite nanostructures, bone-tissue like carbon- rich nanocomposite nanostructure, multiaxial intertwined woven-like nanocomposite nanostructures, fish-like nanopattemed carbon-rich nanocomposites, dome-shaped intertwined woven-like nanocomposite nanostructures, quantum size fibrous nanocomposite nanostructures, sharp-fold controlled-topology nanocomposite nanostructures, hollow sphere bone-tissue like shell nanocomposites, multi-scaled multilayer micro, nano, meso, quantum sized structures, multi-scaled multilayer nanocomposite, nano-curvature graphitic structures with twisted layers, nano-waved graphitic structures with twisted layers, nano-curvature graphitic integrated network nanocomposites with twisted layers, nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted layers, and combinations thereof. In an exemplary embodiment, bone-like carbon-rich nanostructures may include one of cancellous bone, trabecular bone, cortical bone, and spongy bone-like carbon-rich nanostructures, and combinations thereof. In an exemplary embodiment, an exemplary heating process for increasing carbon content may lead to fixing topology of an architecture of an exemplary carbon-rich nanostructure by increasing an exemplary carbon content of an exemplary carbon-rich nanostructure and controlling a balance between expansion and tension of an exemplary carbon-rich nanostructure. In an exemplary embodiment, controlling a balance between expansion and tension of an exemplary carbon-rich nanostructure may be achieved due to release of gases on exemplary fibers in spaces between exemplary connections and tendency to shrink with increasing temperature and plasticizing effect of exemplary melting components. In an exemplary embodiment, a thermoplastic material with a melting temperature within a temperature range of an exemplary heating process, may melt during an exemplary carbonization process; allowing for simultaneously creating connections in an exemplary structure of exemplary carbon-rich nanostructures and plasticizing an exemplary structure of exemplary carbon-rich nanostructures, especially when more than one type of meltable plasticizing agents is used in an exemplary method. In an exemplary embodiment, an exemplary method may be an efficient method due to using cost-effective easy-scalable materials and steps based on applying plenty and cheap materials; allowing for providing an affordable product.
[0063] FIG. 1A illustrates a flowchart of a method 100 for controlling topology of carbon-rich nanostructures, consistent with one or more exemplary embodiments of the present disclosure. In an exemplary embodiment, method 100 may include a step 102 of forming a plurality of carbon-containing fibers, a step 104 of forming a two or multi-phase system by adding a thermoplastic material to the plurality of carbon-containing fibers, a step 106 of forming a nanostructured network by heating the two or multi-phase system to a temperature up to 450°C, and a step 108 of forming a carbon-rich nanostructure by increasing carbon content of the nanostructured network by heating the nanostructured network to a temperature of at least 800°C under an inert atmosphere.
[0064] In an exemplary embodiment, step 102 of forming a plurality of carbon-containing fibers may include using a carbon fiber precursor for producing an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, an exemplary carbon fiber precursor may form an exemplary plurality of carbon-containing fibers by at least a method of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel electrospinning, and combinations thereof. In an exemplary embodiment, an exemplary plurality of carbon- containing fibers may include at least one of nano, micro, and multiple scaled fibers. In an exemplary embodiment, an exemplary carbon-rich precursor may include at least one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, and combinations thereof. In an exemplary embodiment, an exemplary carbohydrate may include at least one of sucrose, dextrins, starch, glucose, and combinations thereof. In an exemplary embodiment, an exemplary polysaccharide may include one of N-[(2-hydroxy-3 -trimethyl ammonium) propyl] chitosan (HTCC), lignin, and combinations thereof.
[0065] In an exemplary embodiment, step 104 of forming a two or multi-phase system may include adding a thermoplastic material to an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, at least one thermoplastic material may be added to an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers may include at least one of adding an exemplary at least one thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers after forming an exemplary plurality of carbon-containing fibers, and combinations thereof. In an exemplary embodiment, an exemplary thermoplastic/meltable material may be added to an exemplary carbon fiber precursor with a weight ratio in a range of 0.0005:1 to 10:1 (an exemplary thermoplastic material: carbon fiber precursor).
[0066] In an exemplary embodiment, an exemplary thermoplastic material may have a melting point below 450°C. In an exemplary embodiment, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process of at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) elctro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel-electro/spinning, sequential layer by layer fiber forming/electrospinning, a post- electrospinning, and combinations thereof. In an exemplary embodiment, an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, a poly(amidoamine) (PAMAM), a silicone, a silicone compound, a poysiloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, poly or oligo or monoacrylates, nanostructures, salts (such as zinc nitrate), elements (such as zinc), their mixtures with each other or with other materials, their mixtures with of at least one of protein compounds, oligomers, co- or tri-polymers, amphiphilics, macromolecules, superstructures, biomaterials, metamaterials, softeners, a carbon fiber precursor, (e.g. PAN, polysaccharides, lignin, lignocellulose), and combinations thereof in a form of a polymer, a resin, an oligomer, a macromolecule, a capsule, a dendrimer, a liposome, a micelle, a hybrid, a composite, a nanocomposite, an organic/inorganic compound, and combinations thereof.
[0067] In an exemplary embodiment, adding at least one thermoplastic material to an exemplary plurality of an exemplary carbon fiber precursor-containing nanofibers, in a way to form a two/multi phased system may include a plurality of at least one of the thermoplastic material elements along with an exemplary plurality of at least one of the carbon fiber precursor-containing nanofibers elements.
[0068] In an exemplary embodiment, step 106 of forming a nano structured network may include heating an exemplary two or multi-phase system to a temperature up to 450°C. In an exemplary embodiment, an exemplary two or multi-phase system may be heated in a heating device for a time period in a range of 10 minutes to 400 minutes. In an exemplary embodiment, an exemplary heating device may include a heater, a thermal chamber, for example, an oven, a heater, a furnace, etc. In an exemplary embodiment, an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof. In an exemplary embodiment, an exemplary inert gas may include at least one noble gas. In an exemplary embodiment, an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof. In an exemplary embodiment, heating an exemplary two or multi-phase system may melt an exemplary thermoplastic material. In an exemplary embodiment, an exemplary thermoplastic material may have a melting point below 450 °C. In an exemplary embodiment, exemplary elements of an exemplary thermoplastic material may form connections when they melt at an exemplary meeting points of exemplary nanofibers crossing. In an exemplary embodiment, an exemplary connection between exemplary carbon-containing fibers may form a nanostructured network. In an exemplary embodiment, a nanostructured network may be formed by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon-containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450°C. In an exemplary embodiment, controlling an exemplary temperature may control topology of an exemplary nanostructured network. In an exemplary embodiment, important factors for controlling topology of carbon rich nanostructures may include duration of an exemplary process of heating, percentage composition of exemplary components, melting point of each of exemplary components, thermal characteristics of each of exemplary components, number and ratio of thermoplastic materials and/or a meltable material, method of adding each component, proximity and frequency of connections, morphology, fineness and abundance and density of fibers between exemplary connections, characteristics and rheology of molten materials, rate of expansion of an exemplary nano structured network, strengthening factors that may create tension, expansion, or prevent shrinking (when using mechanical, magnetic, nano magnetic, smart nano magnetic, etc. systems), curie temperature when using magnetic, nanomagnetic, or smart and microdynamic magnetic/nanomagnetic system, etc., and combinations thereof are used, additives containing magnetic materials), dosage of atmosphere mixtures, number and temperature of thermal processes, moisture content in an exemplary structure for example, "moisture regain of materials" etc.
[0069] In an exemplary embodiment, step 108 of increasing carbon content of the nanostructured network may include heating an exemplary nanostructured network to a temperature of at least 800°C. In an exemplary embodiment, heating an exemplary nanostructured network may form carbon-rich nanostructures. In an exemplary embodiment, an exemplary carbon-rich nanostructures may include one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially-carbon-rich nanocomposite, and combination thereof. In an exemplary embodiment, an exemplary nano structured network may be heated in a furnace. In an exemplary embodiment, an exemplary nano structured network may be heated in a furnace. In an exemplary embodiment, during an exemplary heating process for increasing carbon content of an exemplary nano structured network, at least a non-carbon containing element may leave an exemplary nanostructured network. In an exemplary embodiment, during an exemplary thermal process, non-carbon elements such as oxygen, nitrogen, hydrogen, halogens, etc., may be released in form of gases. In an exemplary embodiment, exemplary gases may include hydrogen cyanide (HCN), (nitrogen) N2, water (H2O), etc. In an exemplary embodiment, an exemplary non-carbon element composition may depend on an exemplary composition of an exemplary nano structured network and chemical structure of an exemplary nanostructured network. In an exemplary embodiment, an exemplary furnace may include a gas inlet and a gas outlet. In an exemplary embodiment, exemplary gases leaving an exemplary heating device, for example, a furnace may include a neutral gas or a predetermined atmosphere. In an exemplary embodiment, an exemplary predetermined atmosphere may include noble gases. In an exemplary embodiment, an exemplary nano structured network may be heated under an inert gas atmosphere. In an exemplary embodiment, an exemplary inert gas may enter from an exemplary gas inlet and may leave an exemplary furnace from an exemplary gas outlet. In an exemplary embodiment, an exemplary nanostructured network may be heated under an inert gas atmosphere. In an exemplary embodiment, an exemplary inert gas may include at least a noble gas and/or a mixture of atmospheres. For example, an exemplary heating process may be applied using air atmospheres with a temperature up to 280 °C-300 °C or a combined atmosphere of 5-50% air atmosphere in combination with inert atmosphere d at a temperature up to 300 °C -350 °C. In an exemplary embodiment, an exemplary nano structured network may be kept for 5 minutes to 20 minutes at a temperature of 350 °C - 380 °C in a mixed atmosphere containing 5-50% air atmosphere, then the air atmosphere may be replaced with a rate of 2- 20% per minute with inert atmosphere and the temperature may be increased with a rate of 2 °C/min. to 20 °C/min. Then, the process may continue at a temperature higher than 400 °C in a completely inert atmosphere. In an exemplary embodiment, controlled dosing of exemplary combined atmosphere may allow achieving one of forming integrated fused network (IFN), fixing and refining the topology via increasing carbon content (FRIC) thermal steps, and combinations thereof. Both thermal steps of IFN and FRIC can be followed continuously or separately in form of one integrated thermal process or two/multi separated thermal procedures. In an exemplary embodiment, each of IFN or FRIC steps can include one, two or more continuous or separate steps of a thermal process.
[0070] In an exemplary embodiment, exemplary thermoplastic materials with a melting temperature equal or lower than a temperature of FRIC steps may create a new connection or plasticize an exemplary nano structured network or both at the same time by forming carbon rich nanostructures and conducting topology of an exemplary carbon rich nanostructures. In an exemplary embodiment, conducting topology of an exemplary carbon rich nanostructures may be enhanced when more than one type of thermoplastic material with different melting temperatures are used in an exemplary method. In an exemplary embodiment, melting of one or more thermoplastic material may be done in an exemplary FRIC stage as well. In an exemplary embodiment, a thermoplastic component may completely or partially leave an exemplary carbon rich nanostructure during thermal processes, or a small percentage of an exemplary thermoplastic component may remain or an exemplary thermoplastic component may join an exemplary carbon, graphite or carbon/graphite network along with an exemplary carbon rich nanostructure. In an exemplary embodiment, an exemplary residue of an exemplary thermoplastic component may be removed in following steps such as washing or purification when an exemplary thermoplastic component are not incorporated in one of exemplary carbon, graphite or carbon/graphite nanostructures or exemplary patterns on an exemplary carbon, graphite or carbon/graphite nanostructures. In an exemplary embodiment, factors considered during an exemplary method for controlling topology of an exemplary carbon rich nanostructures may include controlling balance between thermal expansion, expansion under pressure of exhaust gases and stress, resulting from exhaust gases, on an exemplary plurality of fibers in distances between connections, plasticizing effect of exemplary melting components, tendency to shrinkage with increasing temperature and the type, structure and mechanism of functionalizing an exemplary substrate and thermal and rheological behavior of an exemplary substrate, etc.
[0071] In an exemplary embodiment, parameters effecting an exemplary topology of an exemplary carbon rich nanostructure may include one of rate of temperature increase, final temperature, process duration, percentage composition of components, melting point of each component, thermal characteristics of each of exemplary components, number and ratio of exemplary thermoplastic materials, mechanism of adding each component, closeness and frequency of connections, morphology, size (diameter), frequency, density of fibers between connections, rheological properties of molten materials and additives, rheological properties of carbon-containing fibers such as stretchability, extension, modulus, elasticity, and composition of additives, as well as geometry of nanostructures on exemplary carbon-containing fibers, rheological properties of nanocomposites, such as the effect of nanostructures on elasticity, modulus, extension, The rate of gas release, strengthening factors that expand and create tension, or prevent shrinking using mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic and smart microdynamic systems, etc. curie temperature when using magnetic, nanomagnetic, or smart and thermomicrodynamic/ microdynamic magnetic/nanomagnetic or combined mechanisms, and/or additives containing magnetic materials, etc., dosage of atmosphere mixtures, number and temperature of thermal steps, moisture content in an exemplary method, for example, " moisture regained of materials" etc. In an exemplary embodiment, an exemplary method for controlling tension may work using mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic, thermomicrodynamic, and smart microdynamic methods, etc. and combinations thereof.
[0072] In an exemplary embodiment, an exemplary carbon-rich nanostructures may have a convoluted, wavy, spiral, porous, intertwined, angled, branched, networked (integrated network), fibrous, hollow, patterned of nano, micro, meso and quantum sized structures. In an exemplary embodiment, controlling an exemplary topology of an exemplary carbon-rich nanostructures may include forming at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, nano-curvature graphitic integrated network nanocomposites/nanostructures with twisted layers, nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted layers, and combinations thereof. [0073] In an exemplary embodiment, an additive may be added to at least one of an exemplary mixture containing one of a carbon fiber precursor, an exemplary thermoplastic material, an exemplary carbon-rich nanostructure, and combinations thereof. In an exemplary embodiment, a layer of an exemplary additive may be formed on an exemplary carbon-rich nanostructures. In an exemplary embodiment, an exemplary additive may have a thickness of up to 1 mm. In an exemplary embodiment, an exemplary additive may include one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a surfactant, a catalyst, a hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, BETS, hyroxides, salts, composites, nanostructures of exemplary additives, frameworks of exemplary additives, and combinations thereof. In an exemplary embodiment, an exemplary additive may include at least one of polyethylene glycol (PEG), polyvinylpyrrolidone (PVP), chitosan, carbohydrates, polysaccharide, carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), acrylic resins, silicones, polysiloxanes, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, a hydrogels, acrylates, poly(sodium acrylate), polyimides, a poly( amidoamine) (PAMAMs), a polyaniline, polysiloxanes, proteins, monomers of exemplary polymers, oligomers, co- or tripolymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, metal-organic frameworks (MOFs), softeners, a metal oxide, Silicon (Si), Boron (B), phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanotubes (CNTs), fullerene, graphene and graphene-based materials, a magnetic material, hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPS ). Strontium stannate (SrSnos), Tungsten ditelluride (WTei), Potassium heptafluorotantalate (FCTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBi), Niobium disulfide (NbSz), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Lead (Pb), Iridium (Ir), Cobalt (Co), Nickel (Ni), Vanadium (V), tungsten (W), Tin (Sn), molybdenum (Mo), tellurium (Te), niobium (Nb), iron (Fe), palladium (Pd), strontium (Sr), an oxide of at least one of Cu, Zn, Fe, Mn, Ti, Mg, Mo, Si, chalcogenides, a salt comprising at least one of chalcogenides, Ag, Cu, Zn, Fe, V, Ni, Co, Ir, Pb, Mn, Au, Pt, Ti, W, Sn, Mo, Te, Nb, Pd, and Sr, and combinations thereof. In an exemplary embodiment, an exemplary nanostructured additive may include at least one of a Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPSa). Strontium stannate (SrSnos), Tungsten ditelluride (WTc ). Potassium heptafluorotantalate (KiTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBi), Niobium disulfide (NbSz), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), at least one of a hydroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), chalcogenides, Vanadium (V), Tungsten (W), and combinations thereof. In another exemplary embodiment, nanostructured additives may also include one of metals such as Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B). Oxides/ hyroxides of Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B), a metal oxide or a metal hydroxide such as Titanium dioxide (TiO ). Zinc oxide (ZnO), Copper oxide (CuO), Silicon dioxide (SiOi), Iron oxide (FeiOs), Iron oxide (FesO^, Magnesium oxide (MgO), and Magnesium hydroxide (MgOH), Salts of Titanium (Ti), Calcium (Ca), Sodium (Na), Tellurium (Te), Copper (Cu), Selenium (Se), Iron (Fe), Carbon (C), Zinc (Zn), Silicon (Si), Titanium (Ti), Germanium (Ge), Gallium (Ga), Cobalt (Co), Cerium (Ce), Iridium (Ir), Vanadium (V), Strontium (Sr), Tantalum (Ta), Cadmium (Cd), Manganese (Mn), Magnesium (Mg), Tin (Sn), Niobium (Nb), Antimony (Sb), Lead (Pb), Platinum (Pt), Gold (Au), Silver (Ag), Aluminum (AL), Tungsten (W), , Molybdenum (Mo), Potassium (K), transition metal cholcogenides, etc., with one another and/or with Chlorine (Cl), Fluorine (F), Sulfur (S), Iodine (I), Boron (B), Nitrogen (N), Phosphorus (P), Sulfate (SO4), Nitrate (NO3), Carbonate (CO3), Bicarbonate (HCO3), Periodate (IO4), Phosphate (PO4), etc, and combinations thereof, Multi and bimetals with one of Ti, Ca, Te, Cu, Se, Fe, C, Zn, Si, Ge, Ga, Co, Ce, Ir, Sr, Ta, V, Cd, Mn, Mg, Sn, Nb, Sb, Pb, Pt, Au, Ag, W, Te, Na, K and combinations thereof, carbon structures (e.g. CNT, carbon nanofibres (CNFs), fullerene, graphene, graphene oxide, reduced graphene oxide (rGO), MOFs, hBN, borophene, Bismuth strontium calcium copper oxide (BSCCO), kagome lattices (e.g. kagome (BETS GaCk), BETS metal compounds (e.g. (BETS GaCU), hydroxyapatite, phosphosilicates, Composites of SiO2, TiO2, MgO, MgOH, CuO, ZnO, Fe2O3, Fe3O4, Ag, Ce, Cu, Pt, Au, V, Ca, Mg, Mn, Mg, Sn, Ga, Fe, Pb, Al, Cd, Si, Co, Te, B, SrSno3. MgB2, WTe2, WS2, Ag/ ZnO, Ag/SiO2, Ag/TiO2, NbS2, FePS3, clays, CaCO3, SiC, LDH, Na3N, MXenes, magnetites, hBN, borophene, CNFs, CNT, fullerene, carbon structures, MOFs, Ir, Mo, Ni, SiC, Sn, Pd, Nb, , W, Sr, Si, Potassium heptafluorotantalate (K2TaF?), Bismuth strontium calcium copper oxide (BSCCO), kagome lattices, hydroxyapatite, bioglass, biomaterials, their oxygen compounds, etc., such as Ag/TiO2, Au/SiO2, Ag/ZnO, Ag/SiO2, Ag/TiO2, including core-shells, etc., Ion loaded nanostructures by Cl, F, S, Fe, I, B, N, P, Te, Cu, Se, C, Zn, Si, Ti, Ge, Ga, Co, Ce, Ir, Sr, Ta, Cd, Mn, Se, Mg, Sn, Nb, Sb, Pb, Pt, Au, Ag, W, Mo, Te, Na, K, their anionic species for example with O (e.g. Sulfate (SO4), Nitrate (NO3), Carbonate (CO3), Bicarbonate (HCO3), Periodate (IO4), Phosphate (PO4)), etc. Nanostructures treated, activated, and/or etched via one of methods of treating, activating, coating, etching, patterning, and/or decorating using chemical methods (oxidants, acids, alkalis, organic solvents, etc.), irradiation based methods e.g. laser, plasma, gamma, rays ultraviolet (UV) electronic waves, magnetron, microwave, lithography, ion etching pretreatments, atomic force microscopy, PVD, CVD, sputtering, electrospray, etc., and combinations thereof, organic/inorganic nanostructures in which the organic component may be one of anhydrides (e.g. Maleic anhydride), acrylic acid, n-methylols, carbamides, acrylic resins, silicones, poly siloxanes, polyurethanes, aldehydes, PVA, PA, polyols, polyoxides, polyesters, proteins, polycarbonates, polystyrenes, polysaccharides, carbohydrates, poly electrolytes, hydrogels, poly(sodium acrylate), polyimides, PAMAMs, polyaniline, polyvinyls, PVdF, their monomers, ammonias, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, electrolytes, MOFs, drugs, dyes, softeners, antistatic, flame-retardants, etc. derivatives of exemplary additives, mixtures of exemplary additives, co- or tri-polymers of exemplary additives, and combinations thereof.
[0074] In an exemplary embodiment, forming an exemplary carbon-rich nanostructures may include intermediate processes such as washing, purification, removal of some components, in-situ synthesis, irradiation, coating, loading additives in the form of combined and sequential processes, etc. In an exemplary embodiment, washing and purification may be performed due to removing some components, creating porosity, etc. In an exemplary embodiment, an exemplary carbon-rich nanostructure may be washed with at least one of an organic solvent, an aqueous solution, and combination thereof. In an exemplary embodiment, an exemplary washing process may be performed via one, two or frequent immersing, dipping, centrifuging steps, in one of an organic solvent, an acid solution, an alkaline solution, an oxidant solution, an enzyme solution, a surfactant solution, a reducing agent solution, an ionic solvent, aqueous solutions, water, and combinations thereof. In an exemplary embodiment, an exemplary washing process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc. and combinations thereof.
[0075] In an exemplary embodiment, an exemplary plurality of carbon-containing fibers may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof. In an exemplary embodiment, an exemplary nano structured network may be washed with at least one of an organic solvent, an aqueous solution, and combination thereof. In an exemplary embodiment, at least one of an exemplary carbon-rich nanostructure, an exemplary plurality of carbon-containing fibers, an exemplary nano structured network, and combinations thereof may be purified using at least one of an acid solution, a basic solution, an oxidant solution, an organic solution, and combinations thereof. In an exemplary embodiment, an exemplary purifying process may include a heating process. In an exemplary embodiment, an exemplary heating process may be performed in a furnace. In an exemplary embodiment, an exemplary purifying process may be used for eliminating/reducing dust and impurity of air, environment, and/or undesirable residue /impurity from the procedures, etc., and/or for activation, increasing specific surface area, refining the morphology of an exemplary carbon rich nanostructure, mending defects, covering defects, functionalization, etc. In an exemplary embodiment, an exemplary purifying process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc., and combinations thereof. [0076] In an exemplary embodiment, an exemplary nanostructured additive may be in-situ synthesized using at least one of a hydrothermal process, a solvothermal process, a chemical reduction/oxidation, irradiation, a thermal process, and combinations thereof. In an exemplary embodiment, a component may be eliminated before or after forming an exemplary nanostructured network using at least one of an organic solvent, an acid solution, a basic solution, an oxidant solution, water, and combinations thereof. In an exemplary embodiment, an exemplary component may depend on an exemplary carbon containing precursor, an exemplary thermoplastic material, additives, etc. In an exemplary embodiment, additives may be added for reinforcement of an exemplary carbon-rich nanostructure, for forming a porous structure, or for synergistic effects, covering defects, improving properties of an exemplary carbon rich nanostructure, improving performance of an exemplary carbon rich nanostructure, surface modifications of an exemplary carbon rich nanostructure, adding a roughness, nano roughness, modifying thermal, rheological, mechanical, tensile properties during or after an exemplary process, forming a composite, nanostructure, superstructure, a metamaterial, a heterostructure, surface modification, conducting fiber morphology, conducting IFN or FRIC adding a feature on an exemplary substrate, achieving a smart, a multi-functional, a multi targeted feature, and combinations thereof, adding a nano, meso, quantum size feature, jagged morphology, increasing the leaving gas volume flow rate, porosity, etc., and combinations thereof. In an exemplary embodiment, an exemplary IFN or FRIC steps may include designing smart self-activated topology control mechanisms. In an exemplary embodiment, forming an exemplary smart feature on an exemplary substrate may be used for smart multi-purpose drug delivery, multi targeted drug delivery and cell attachment, bone cement, injectable gel reinforcement, etc.
[0077] In an exemplary embodiment, an exemplary eliminated component during an exemplary washing or purification process may include one of exemplary additives e.g. a salt, a softener, an electrolyte, a thermoplastic component, a hydrogel, a resin, a nanostructure, a metal, etc., a byproduct, a precursor or intermediates of an in-situ synthesis, an impurity, an attached substrate which may be designed to be detached before thermal and/or an intermediate process, refining content of a component for special purposes, component which may not be proper or designed to remain during thermal process, creating porosity, hollow fibers, hollow structures, etc. In an exemplary embodiment, an exemplary byproduct maybe achieved from an in situ synthesis process. In an exemplary embodiment, an exemplary special purpose may include an additive and/or a thermoplastic and/or a meltable material may be set to achieve an especial morphology through an exemplary carbon-containing fiber production or processing, but an exemplary additive and/or a thermoplastic and/or a meltable content material may be partially or completely removed according to approaches set through a thermal process.
[0078] FIG. IB illustrates a flowchart of a method 110 for controlling topology of carbon-rich nanostructures using a substrate, consistent with one or more exemplary embodiments of the present disclosure. In an exemplary embodiment, method 110 may include a step 101 of functionalizing a substrate, a step 102 of forming a plurality of carbon-containing fibers on the functionalized substrate, a step 104 of forming a two or multi-phase system by adding a thermoplastic material to the plurality of carbon-containing fibers, a step 106 of forming a nanostructured network by heating the two or multi-phase system to a temperature up to 450°C, and a step 108 of forming a carbon-rich nanostructure by increasing carbon content of the nanostructured network by heating the nanostructured network to a temperature of at least 800°C under an inert atmosphere.
[0079] In an exemplary embodiment, step 101 of functionalizing a substrate may include at least one of forming a rough surface on a substrate, form chemical functional groups on a substrate, and combinations thereof. In an exemplary embodiment, functionalizing an exemplary substrate may include forming a thermoplastic pattern, a layer of an exemplary thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, electrically conductive materials, etching an exemplary surface, and combinations thereof. A microdynamic control on thermal shrinkage, topology and morphology may be applied via using a heat-compatible substrate at least one of fabric, layer, film, paper, sheet, lace, web, and combinations thereof comprising at least a heat resistant material, a carbon, a graphite, a carbon/graphite-forming material. In an exemplary embodiment, an exemplary substrate may be designed to be separated before exemplary thermal procedures above 200°C. In an exemplary embodiment, an exemplary substrate may be made of polyester laces. In an exemplary embodiment, an exemplary heat resistant material may include carbon fabric, a micro-carbon fabric. In an exemplary embodiment, an exemplary carbon/graphite-forming material may include cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a polysaccharide derivatives, lignin, lignocellulose, carbohydrates, carbohydrate derivatives, polyacrylonitriles, and combinations thereof. In an exemplary embodiment, a smart selfactivated microdynamic control mechanism via nanorough friction and/or resin attachment may be devised via functionalizing an exemplary substrate by adding one of a layer of a resin, a layer of an exemplary thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, conductive materials, etching the surface, and combinations thereof on an exemplary substrate. In an exemplary embodiment, an exemplary functionalized substrate may be designed to undergo an exemplary fixing and refining the topology via increasing carbon content (FRIC) with integrated fused nano structured network of two/multi-phase system and/or designed to undergo through forming integrated fused network (IFN) of two/multi-phase systems. In an exemplary embodiment, an exemplary substrate may be a heat and/or shrinkage resistant substrate, for example, a carbon fabric substrate, glass fabric, etc. In an exemplary embodiment, an exemplary substrate may be a heat compatible substrate, for example, a carbon- forming material, a graphite-forming material, a carbon/ graphite-forming material. In an exemplary embodiment, after collecting an exemplary plurality of carbon-containing fibers from an exemplary functionalized substrate, an exemplary plurality of carbon-containing fibers may pass through exemplary thermal treatments (IFN and FRIC) with/without an exemplary functionalized heat resistant substrate. In an exemplary embodiment, through an exemplary heating process, exemplary thermoplastic and/or meltable materials with melting points equal or lower than the temperatures of IFN and FRIC steps may melt and an exemplary plurality of carbon-containing fibers may fuse to an exemplary substrate, functionalized heat resistant, compatible substrate, and/or each other at the connection sites. In an exemplary embodiment, fused sites may keep an exemplary structure from shrinkage. In an exemplary embodiment, an exemplary mechanism of forming connections and controlling topology of nanostructures may be smartly self-activated just when an exemplary temperature increase may lead to thermal shrinkage of exemplary structures of exemplary carbon containing fibers or an exemplary nanostructured network. In an exemplary embodiment, an exemplary mechanism may work more efficient by using a heat and shrinkage resistant substrate. In an exemplary embodiment, temperature designed for this self-activation mechanism may be controlled by designing exemplary thermoplastic materials and/or exemplary meltable compositions. In an exemplary embodiment, one, two or multi meltable compositions may be used.
[0080] In an exemplary embodiment, an exemplary functionalized substrate may be designed to undergo through one of a fixing and refining the topology via increasing carbon content (FRIC) step with integrated fused nano structured network of two/multi-phase system, designed to undergo through forming integrated fused network (IFN) step of the two/multi-phase system, and/or combinations thereof. In an exemplary embodiment, an exemplary functionalized substrate may be a heat and/or shrinkage resistant substrate, for example, a carbon fabric substrate, glass fabric, etc. In an exemplary embodiment, an exemplary functionalized substrate may be a heat compatible substrate, for example, a carbon-forming material, a graphite-forming material, and a carbon/ graphite-forming material. After collecting an exemplary plurality of carbon-containing fibers on an exemplary functionalized substrate and passing through thermal treatments, for example, IFN and FRIC steps with an exemplary functionalized heat resistant substrate, during an exemplary heating process, an exemplary thermoplastic and/or meltable materials which melting points of exemplary thermoplastic and/or meltable materials be equal or lower than the temperatures of IFN and FRIOC steps may melt and an exemplary plurality of fibers may fuse to an exemplary substrate and/or each other at the connection sites. In an exemplary embodiment, fused sites may keep an exemplary structure from shrinkage. In an exemplary embodiment, an exemplary mechanism may be smartly self-activated just when exemplary structures may be subjected to a thermal shrinkage by increasing temperature. In an exemplary embodiment, an exemplary mechanism may work more efficient by using an exemplary heat and shrinkage resistant substrate. In an exemplary embodiment, temperature designed for an exemplary self-activation mechanism may be controlled by designing exemplary thermoplastic materials and/or meltable compositions. In an exemplary embodiment, one, two or more meltable compositions may be used. In an exemplary embodiment, effective friction and entanglement of an exemplary network of an exemplary plurality of carbon- containing nanofibers in roughness between exemplary nanostructures may prevent shrinkage of an exemplary network of an exemplary plurality of carbon-containing nanofibers. In an exemplary embodiment, shrinkage resistance may cause tension and chain alignment and also may boost formation of graphite structures. In an exemplary embodiment, an exemplary simultaneous fusing of fibers to an exemplary substrate may also have a synergistic effect.
[0081] In an exemplary embodiment, an exemplary substrate may include at least one of a fabric, a layer, a film, a paper, a sheet, a lace, a web, and combinations thereof. In an exemplary embodiment, an exemplary substrate may be made of at least a heat resistant material, a carbon- forming material, a graphite -forming material, and a carbon/ graphite-forming material. In an exemplary embodiment, an exemplary substrate may be configured to be separated from an exemplary nano structured network before a heating process above 200°C. In an exemplary embodiment, an exemplary substrate may include at least one of a carbon fabric, a micro- carbon fabric, a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a layer of polysaccharide derivatives, lignin, lignocellulose, a carbohydrates, a carbohydrate derivatives, polyacrylonitriles, a metal sheet, a layer of mercerized cellulose, polyester laces, and combinations thereof. In an exemplary embodiment, functionalizing an exemplary substrate may include at least one of adding a layer of a resin on an exemplary substrate, adding a layer of an exemplary at least one thermoplastic material on an exemplary substrate, adding a layer of a plurality of nanostructures on an exemplary substrate, forming a pattern of a magnetic material on an exemplary substrate, adding a layer of an electrically conductive material on an exemplary substrate, adding a patterned layer of an electrically conductive material on an exemplary substrate, etching surface of an exemplary substrate, and combinations thereof. In an exemplary embodiment, one of a substrate, a surface layer, and a sandwich in form of magnetic fibers or patterns with or without nano roughness, fusible component, etc., may be used for a smart and microdynamic topology control system, especially when exemplary fibers and/or connections in an exemplary fiber network include magnetic additives. In an exemplary embodiment, usage of electrically conductive, electrically non-conductive, magnetic patterns, magnetic fields, magnetic additives, etc., and their combinations for functionalization an exemplary substrate may control morphology of exemplary carbon-containing fibers while producing and collecting an exemplary plurality of carbon-containing fibers from an exemplary functionalized substrate. In an exemplary embodiment, an exemplary control may be efficient when magnetic fields or magnetic additives may be used simultaneously during one of fiber production process (e.g. a magnetic fields-assisted electrospinning) or in the fibers and/or thermoplastic and/or meltable material mixtures, etc., and combinations thereof. In an exemplary embodiment, an exemplary fiber production process may include magnetic fields- assisted electrospinning. In an exemplary embodiment, an exemplary plurality of nanostructures may include at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphenebased materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide ( FcPSp. Strontium stannate (SrSnos), Tungsten ditelluride (WTc ). Potassium heptafluorotantalate (FGTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgEL), Niobium disulfide (NbS ), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof. In an exemplary embodiment, an exemplary plurality of nanostructures may include at least one of a hydroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), chalcogenides, molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof. In an exemplary embodiment, an exemplary resin may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, a carbohydrates, a polysaccharide, a carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), an acrylic resin, silicone, a polysiloxane, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEG), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, hydrogels, acrylates, poly(sodium acrylate), a polyimide, poly(amidoamine) (PAMAMs), polyaniline, polysiloxanes, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, MOFs, softeners, and combinations thereof.
[0082] In an exemplary embodiment, step 102 of forming a plurality of carbon-containing fibers may include forming an exemplary plurality of carbon-containing fibers on an exemplary substrate/functionalized substrate. In an exemplary embodiment, an exemplary plurality of carbon containing fibers may interact with an exemplary functionalized substrate. In an exemplary embodiment, an exemplary interaction between an exemplary plurality of carbon containing fibers with an exemplary functionalized substrate may effect topology of an exemplary carbon-rich nanostructures. In an exemplary embodiment, an exemplary plurality of carbon containing fibers may be produced using at least a carbon fiber precursor. In an exemplary embodiment, an exemplary carbon fiber precursor may form an exemplary plurality of carbon-containing fibers by at least a method of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel electrospinning, and combinations thereof. In an exemplary embodiment, an exemplary plurality of carbon-containing fibers may include at least one of nano, micro, and multiple scaled fibers. In an exemplary embodiment, an exemplary carbon-rich precursor may include at least one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, carbon-containing salt, carbon-containing alloy, metal-organic frameworks (MOF), and combinations thereof. In an exemplary embodiment, an exemplary carbohydrate may include at least one of sucrose, dextrins, starch, glucose, and combinations thereof. In an exemplary embodiment, an exemplary polysaccharide may include one of N-[(2-hydroxy-3- trimethyl ammonium) propyl] chitosan (HTCC), lignin, and combinations thereof.
[0083] In an exemplary embodiment, step 104 of forming a two or multi-phase system may include adding a thermoplastic material to an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, at least one thermoplastic material may be added to an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers may include at least one of adding an exemplary at least one thermoplastic material to an exemplary mixture containing an exemplary carbon fiber precursor, adding an exemplary at least one thermoplastic material to an exemplary substrate, an exemplary functionalized substrate, one of exemplary composition of an exemplary functionalizing materials for substrate, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers while forming an exemplary plurality of carbon-containing fibers, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers, after forming an exemplary plurality of carbon-containing fibers, and combinations thereof. In an exemplary embodiment, an exemplary thermoplastic material may be added to an exemplary carbon fiber precursor with a weight ratio in a range of 0.0005:1 to 10:1 an exemplary thermoplastic material: carbon fiber precursor). In an exemplary embodiment, an exemplary thermoplastic material may have a melting point below 450°C. In an exemplary embodiment, adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon- containing fibers while forming an exemplary plurality of carbon-containing fibers or after forming an exemplary plurality of carbon-containing fibers may include adding an exemplary at least one thermoplastic material to an exemplary plurality of carbon-containing fibers utilizing a process of at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, a fiber/nanofiber co(parallel) elctro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet- electrospinning, wet or gel-electro/spinning, sequential layer by layer fiber forming/electrospinning, a post- electrospinning, and combinations thereof. In an exemplary embodiment, an exemplary thermoplastic material may include at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, a poly( amidoamine) (PAMAM), a silicone, a silicone compound, a poysiloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, poly or oligo or monoacrylates, nanostructures, salts, for example, zinc nitrate, elements for example, zinc, mixtures of exemplary thermoplastic materials with each other or with other materials, mixtures of exemplary thermoplastic materials with of at least one of protein compounds, oligomers, co- or tri-polymers, amphiphilics, macromolecules, superstructures, biomaterials, metamaterials, softeners, a carbon fiber precursor, and combinations thereof in a form of polymer, resin, oligomer, macromolecule, capsule, dendrimer, liposome, micelle, hybrid, composite, nanocomposite, organic/mineral compound, and combinations thereof. In an exemplary embodiment, an exemplary carbon fiber precursor may include PAN, polysaccharides, lignin, and lignocellulose.
[0084] In an exemplary embodiment, adding at least one thermoplastic material to an exemplary plurality of an exemplary carbon fiber precursor-containing nanofibers, in a way to form a two/multi phased system may include forming a plurality of at least one of thermoplastic material elements along with an exemplary plurality of carbon fiber precursor-containing nanofibers elements. [0085] In an exemplary embodiment, step 106 of forming a nano structured network may include heating the two or multi-phase system to a temperature up to 450°C. In an exemplary embodiment, an exemplary two or multi-phase structure may be separated from an exemplary substrate when applying a temperature of at least 200°C to an exemplary two or multi-phase structure. In an exemplary embodiment, when an exemplary substrate may be subjected to an exemplary heating process, exemplary carbon-containing fibers may be connected at least to each other, to an exemplary substrate, and combinations thereof via a plurality of connections made by at least one of exemplary melted components. In an exemplary embodiment, an exemplary nanostructured network may include a plurality of carbon-containing fibers connected to each other via an exemplary plurality of thermoplastic connections. In an exemplary embodiment, an exemplary two or multi-phase system may be heated in a heating device for a time period in a range of 10 minutes to 400 minutes. In an exemplary embodiment, an exemplary heating device may include a heater, a thermal chamber such as an oven, a heater, a furnace, etc. In an exemplary embodiment, an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof. In an exemplary embodiment, an exemplary inert gas may include at least one noble gas. In an exemplary embodiment, an exemplary two or multi-phase system may be heated under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof. In an exemplary embodiment, heating an exemplary two or multi-phase system may melt an exemplary thermoplastic material. In an exemplary embodiment, an exemplary thermoplastic material may have a melting point below 450 °C. In an exemplary embodiment, exemplary elements of an exemplary thermoplastic material may form connections when exemplary elements melt at an exemplary meeting points of exemplary nanofibers crossing and/or substrate. In an exemplary embodiment, heating an exemplary two or multi-phase system may form connections between carbon-containing fibers via an exemplary melted thermoplastic material. In an exemplary embodiment, an exemplary connection between exemplary carbon-containing fibers may form a nano structured network. In an exemplary embodiment, an exemplatry nanostructured network may form by forming a plurality of thermoplastic connections among an exemplary plurality of carbon-containing fibers. In an exemplary embodiment, forming an exemplary nano structured network may include melting an exemplary at least one thermoplastic material among an exemplary plurality of carbon-containing fibers by heating an exemplary two or multi-phase system to a temperature up to 450°C. In an exemplary embodiment, controlling an exemplary temperature may control topology of an exemplary nanostructured network. In an exemplary embodiment, important factors for controlling topology of exemplary carbon rich nanostructures may include duration of an exemplary process, percentage composition of exemplary components, melting point of each of exemplary components, thermal characteristics of each of exemplary components, number and ratio of thermoplastic materials and/or a meltable materials, method of adding each, proximity and frequency of connections, morphology, fineness and abundance and density of carbon- containing fibers between joints, characteristics and rheology of molten materials, rate of expansion of an exemplary carbon-rich nanostructure, boosting factors that may create tension, expansion, or prevent shrinking, curie temperature, dosage of atmosphere mixtures, number and temperature of thermal steps, moisture content in an exemplary system for example, " moisture regain of materials" etc. In an exemplary embodiment, an exemplary control tension system may work in the form of mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic, and smart microdynamic systems, etc. and combinations thereof. In an exemplary embodiment, an exemplary curie temperature may be important for considering when magnetic, nanomagnetic, or smart and thermodynamic magnetic/nanomagnetic or combined mechanisms, and/or additives containing magnetic materials are used.
[0086] In an exemplary embodiment, step 108 of increasing carbon content of the nanostructured network may include heating an exemplary nanostructured network to a temperature of at least 800°C. In an exemplary embodiment, an exemplary heating process may be used for increasing carbon content of an exemplary nanostructured network. In an exemplary embodiment, heating an exemplary nano structured network may form carbon-rich nanostructures. In an exemplary embodiment, an exemplary carbon-rich nanostructures may include one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially- carbon-rich nanocomposite, and combinations thereof. In an exemplary embodiment, an exemplary nanostructured network may be heated in a furnace. In an exemplary embodiment, during an exemplary heating process at least a non-carbon containing element may leave an exemplary nano structured network. In an exemplary embodiment, during an exemplary thermal process, non-carbon elements such as oxygen, nitrogen and hydrogen, halogens, etc., may be released in form of gases. In an exemplary embodiment, leaving gasses may include hydrogen cyanide (HCN), (nitrogen) N2, water (H2O), etc. In an exemplary embodiment, an exemplary non-carbon element composition may depend on the composition of an exemplary nanostructured network and the chemical structure of an exemplary nano structured network. In an exemplary embodiment, an exemplary furnace may include a gas inlet and a gas outlet. In an exemplary embodiment, exemplary gases leaving an exemplary heating device, for example, a furnace may include a neutral gas or a predetermined atmosphere. In an exemplary embodiment, an exemplary predetermined atmosphere may include noble gases. In an exemplary embodiment, an exemplary nanostructured network may be heated under an inert gas atmosphere. In an exemplary embodiment, an exemplary inert gas may enter from an exemplary gas inlet and may leave an exemplary furnace from an exemplary gas outlet. In an exemplary embodiment, an exemplary nanostructured network may be heated under an inert gas atmosphere with atmospheric pressure. In an exemplary embodiment, an exemplary inert gas may include at least a noble gas and/or a mixture of atmospheres.
[0087] For example, an exemplary heating process may be used under air atmospheres at a temperature of 280 °C -300 °C, a combined atmosphere of 5-50% air atmosphere in combination with inert atmosphere may be applied at a temperature up to 300 °C -350 °C. In an exemplary embodiment, an exemplary nano structured network may be kept for 5 minutes to 20 minutes at a temperature of 350 °C - 380 °C in a mixed atmosphere containing 5-50% air atmosphere, then the air atmospheric atmosphere may be replaced with a rate of 2% per minute to 20% per minute with inert atmosphere and concurrently temperature may be increased with a rate of 2 °C/min. to 20 °C/min. Then, an exemplary heating process may continue at a temperature higher than 400 °C or higher than 450 °C in a completely inert atmosphere. Controlled dosing of an exemplary atmosphere may be followed in any one of an exemplary forming integrated fused network (IFN) step, an exemplary fixing and refining topology of an exemplary carbon-rich nanostructure via increasing carbon content (FRIC) thermal step, and combinations thereof. Both IFN and FRIC thermal steps may be followed continuously or separately in form of one integrated thermal process or two/multi separated thermal procedures. In an exemplary embodiment, each of an exemplary IFN or FRIC steps may include one, two or more continuous or separate thermal steps.
[0088] In an exemplary embodiment, exemplary thermoplastic materials with melting temperature equal or lower than the temperature of FRIC step may create a new connection or plasticize an exemplary nano structured network or both at the same time by forming carbon rich nanostructures and conducting and refining topology of an exemplary carbon rich nanostructures especially when more than one type of thermoplastic material with different melting temperatures may be used in an exemplary method. In an exemplary embodiment, melting of one or more thermoplastic material may also be performed in an exemplary FRIC step. In an exemplary embodiment, a thermoplastic component may completely or partially leave an exemplary carbon rich nanostructure during thermal processes, or a small percentage of an exemplary thermoplastic component may remain or an exemplary thermoplastic component may join an exemplary carbon, graphite or carbon/graphite network along with an exemplary carbon rich nanostructure. In an exemplary embodiment, residue of an exemplary thermoplastic component may be removed in following steps of washing or purification when an exemplary thermoplastic component may not be incorporated in an exemplary carbon, graphite or carbon/graphite structure and/or the patterns on an exemplary carbon, graphite or carbon/graphite structure. In an exemplary embodiment, factors considered during an exemplary method for controlling topology of an exemplary carbon rich nanostructures may include controlling balance between thermal expansion, expansion under pressure of exhaust gases and stress resulting from exhaust gases on an exemplary plurality of carbon-containing fibers in distances between connections, plasticizing effect of exemplary melting components, plasticizing, tendency to shrinkage with increasing temperature and structure, and type of functionalization an exemplary substrate and thermal and rheological behavior of an exemplary substrate, and stability of topology by increasing carbon content, etc., and the combinations thereof.
[0089] In an exemplary embodiment, parameters effecting topology of an exemplary carbon rich nanostructure may include temperature increase rate, maximum temperature, process duration, percentage composition of components, melting point of each component, thermal characteristics of each of exemplary components, number and ratio of exemplary thermoplastic materials, mechanism of adding each component, closeness and frequency of joints, morphology, elegance and frequency and density of fibers between joints, rheological properties of molten materials and additives, rheological properties of cabon-contanining fibers such as stretchability, modulus, elasticity, and composition of additives, as well as geometry of nanostructures on exemplary cabon-contanining fibers, rheological properties of nanocomposites, such as effect of nanostructures on elasticity, modulus, elasticity, rate of gas release, strengthening of factors that may expand and create tension, or prevent shrinkage of an exemplary carbon-rich nanostructure using mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic and smart microdynamic systems, etc., curie temperature when magnetic, nanomagnetic, or smart and thermodynamic magnetic/nanomagnetic or composite mechanisms may be used, or additives containing magnetic materials, dosage of atmosphere mixtures, number and temperature of thermal steps, moisture content in an exemplary system for example, "recycled moisture of materials" etc. In an exemplary embodiment, an exemplary system may work in form of mechanical, magnetic, nanomagnetic, smart nanomagnetic, microdynamic, and smart microdynamic systems, etc., and combinations thereof.
[0090] In an exemplary embodiment, an exemplary carbon-rich nanostructures may have a convoluted, wavy, spiral, porous, intertwined, angled, branched, networked (integrated network), fibrous, hollow, patterned of nano, micro, meso and quantum sized structures. In an exemplary embodiment, controlling an exemplary topology of an exemplary carbon-rich nanostructures may include forming at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, flower-like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopattemed carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled-topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, nano-curvature graphitic integrated network nanocomposites/nanostructures with twisted layers, nano-waved graphitic integrated network nanocomposites/ nanostructures with twisted layers, and combinations thereof.
[0091] In an exemplary embodiment, an exemplary nanostructured network may be heated to form a carbon-rich nanostructure (heating process). In an exemplary embodiment, an exemplary nano structured network may be separated from an exemplary substrate before an exemplary heating process when an exemplary substrate undergo undesirable shape changes during an exemplary heating process. In an exemplary embodiment, an exemplary substrate may include aluminum, polypropylene, and polyester. In an exemplary embodiment, an exemplary nano structured network may be heated after separating an exemplary nanostructured network from an exemplary substrate/functionalized substrate. In an exemplary embodiment, an exemplary nanostructured network may be heated in a furnace at a temperature of at least 800°C.
[0092] In an exemplary embodiment, an additive may be added to at least one of an exemplary mixture containing a carbon fiber precursor, an exemplary thermoplastic material, an exemplary carbon-rich nanostructure, and combinations thereof. In an exemplary embodiment, a layer of an exemplary additive may be formed on an exemplary carbon-rich nanostructures. In an exemplary embodiment, an exemplary additive may have a thickness of up to 1 mm. In an exemplary embodiment, an exemplary additive may include at least one of an exemplary thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, a hydrogel, a vitamin, a softener agent, a surfactant, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, BETS, hyroxides, salts, composites, nanostructures of an exemplary additive, frameworks of an exemplary additive, and combinations thereof. In an exemplary embodiment, an exemplary additive may include at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, carbohydrates, polysaccharide, carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), acrylic resins, silicones, poly siloxanes, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, a hydrogels, acrylates, poly(sodium acrylate), polyimides, a poly(amidoamine) (PAM AMs), a polyaniline, poly siloxanes, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, metal-organic frameworks (MOFs), softeners, a metal oxide, Silicon (Si), Boron (B), phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanotubes (CNTs), fullerene, graphene and graphene-based materials, a magnetic material, hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPSa). Strontium stannate (SrSnos). Tungsten ditelluride (WTc ). Potassium heptafluorotantalate (KsTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBi), Niobium disulfide (NbSi), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Lead (Pb), Iridium (Ir), Cobalt (Co), Nickel (Ni), Vanadium (V), tungsten (W), Tin (Sn), molybdenum (Mo), tellurium (Te), niobium (Nb), iron (Fe), palladium (Pd), strontium (Sr), an oxide of at least one of Cu, Zn, Fe, Mn, Ti, Mg, Mo, Si, chalcogenides, a salt comprising at least one of chalcogenides, Ag, Cu, Zn, Fe, V, Ni, Co, Ir, Pb, Mn, Au, Pt, Ti, W, Sn, Mo, Te, Nb, Pd, and Sr, and combinations thereof. In an exemplary embodiment, an exemplary nanostructured additive may include at least one of a Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene-based materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FcPS ). Strontium stannate (SrSnos), Tungsten ditelluride (WTc ). Potassium heptafluorotantalate (FGTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBi), Niobium disulfide (NbSz), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), at least one of a hyroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), chalcogenides, Vanadium (V), Tungsten (W), and combinations thereof. In another exemplary embodiment, nanostructure additives may also include one of metals such as Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B). Oxides/ hyroxides of Silver (Ag), Copper (Cu), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), Niobium (Nb), Vanadium (V), Tungsten (W), Zinc (Zn), Titanium (Ti), Silicon (Si), and Boron (B), a metal oxide or a metal hydroxide such as Titanium dioxide (TiOi). Zinc oxide (ZnO), Copper oxide (CuO), Silicon dioxide (SiOi), Iron oxide (FeiOs), Iron oxide (FCSO ), Magnesium oxide (MgO), and Magnesium hydroxide (MgOH), Salts of Titanium (Ti), Calcium (Ca), Sodium (Na), Tellurium (Te), Copper (Cu), Selenium (Se), Iron (Fe), Carbon (C), Zinc (Zn), Silicon (Si), Titanium (Ti), Germanium (Ge), Gallium (Ga), Cobalt (Co), Cerium (Ce), Iridium (Ir), Vanadium (V), Strontium (Sr), Tantalum (Ta), Cadmium (Cd), Manganese (Mn), Magnesium (Mg), Tin (Sn), Niobium (Nb), Antimony (Sb), Lead (Pb), Platinum (Pt), Gold (Au), Silver (Ag), Aluminum (AL), Tungsten (W), Molybdenum (Mo), Potassium (K), transition metal cholcogenides, etc., with one another and/or with Chlorine (Cl), Fluorine (F), Sulfur (S), Iodine (I), Boron (B), Nitrogen (N), Phosphorus (P), Sulfate (SO4), Nitrate (NO3), Carbonate (CO3), Bicarbonate (HCO3), Periodate (IO4), Phosphate (PO4), etc, and combinations thereof, Multi and bimetals with one of Ti, Ca, Te, Cu, Se, Fe, C, Zn, Si, Ge, Ga, Co, Ce, Ir, Sr, Ta, V, Cd, Mn, Mg, Sn, Nb, Sb, Pb, Pt, Au, Ag, W, Te, Na, K and combinations thereof, carbon structures (e.g. CNT, carbon nanofibres (CNFs), fullerene, graphene, graphene oxide, reduced graphene oxide (rGO), MOFs, hBN, borophene, Bismuth strontium calcium copper oxide (BSCCO), kagome lattices (e.g. kagome (BETS)2GaC14), BETS metal compounds (e.g. (BETS)2GaC14), hydroxyapatite, phosphosilicates, Composites of SiO2, TiO2, MgO, MgOH, CuO, ZnO, Fe2O3, Fe3O4, Ag, Ce, Cu, Pt, Au, V, Ca, Mg, Mn, Mg, Sn, Ga, Fe, Pb, Al, Cd, Si, Co, Te, B, SrSno3 < MgB2, WTe2, WS2, Ag/ ZnO, Ag/SiO2, Ag/TiO2, NbS2, FePS3, clays, CaCO3, SiC, LDH, Na3N, MXenes, magnetites, hBN, borophene, CNFs, CNT, fullerene, carbon structures, MOFs, Ir, Mo, Ni, SiC, Sn, Pd, Nb, , W, Sr, Si, Potassium heptafluorotantalate (K2TaF?), Bismuth strontium calcium copper oxide (BSCCO), kagome lattices, hydroxyapatite, bioglass, biomaterials, their oxygen compounds, etc., such as Ag/TiO2, Au/SiO2, Ag/ZnO, Ag/SiO2, Ag/TiO2, including core-shells, etc., Ion loaded nanostructures by Cl, F, S, Fe, I, B, N, P, Te, Cu, Se, C, Zn, Si, Ti, Ge, Ga, Co, Ce, Ir, Sr, Ta, Cd, Mn, Se, Mg, Sn, Nb, Sb, Pb, Pt, Au, Ag, W, Mo, Te, Na, K, their anionic species for example with O (e.g. Sulfate (SO4), Nitrate (NO3), Carbonate (CO3), Bicarbonate (HCO3), Periodate (IO4), Phosphate (PO4)), etc. Nanostructures treated, activated, and/or etched via one of methods of treating, activating, coating, etching, patterning, and/or decorating using chemical methods (oxidants, acids, alkalis, organic solvents, etc.), irradiation based methods e.g. laser, plasma, gamma, rays ultraviolet (UV) electronic waves, magnetron, microwave, lithography, ion etching pretreatments, atomic force microscopy, PVD, CVD, sputtering, electrospray, etc., and combinations thereof, organic/inorganic nanostructures in which the organic component may be one of anhydrides (e.g. Maleic anhydride), acrylic acid, n-methylols, carbamides, acrylic resins, silicones, poly siloxanes, polyurethanes, aldehydes, PVA, PA, polyols, polyoxides, polyesters, proteins, polycarbonates, polystyrenes, polysaccharides, carbohydrates, poly electrolytes, hydrogels, poly(sodium acrylate), polyimides, PAMAMs, polyaniline, polyvinyls, PVdF, their monomers, ammonias, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, electrolytes, MOFs, drugs, dyes, softeners, antistatic, flame-retardants, etc. their derivatives, their mixtures, their co- or tri-polymers, and combinations thereof. [0093] In an exemplary embodiment, forming an exemplary carbon-rich nanostructures may include intermediate processes such as washing, purification, in-situ synthesis, irradiation, coating, loading additives in the form of combined and sequential processes, etc. In an exemplary embodiment, exemplary washing and purification processes may be performed due to removing some components, creating porosity, improving the thermal, mechanical, rheological properties, etc. In an exemplary embodiment, an exemplary carbon-rich nanostructure may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof. In an exemplary embodiment, an exemplary plurality of carbon- containing fibers may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof. In an exemplary embodiment, an exemplary nanostructured network may be washed with at least one of an organic solvent, an aqueous solution, and combinations thereof. In an exemplary embodiment, an exemplary washing process may be performed via one, two, or frequent immersing, dipping, centrifuging, in one of an organic solvent, an acid solution, an alkaline solution, an oxidant solution, an enzyme solution, a surfactant solution, reducing agent solution, an ionic solvent, aqueous solutions, water, and combinations thereof. In an exemplary embodiment, an exemplary washing process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc. and combinations thereof.
[0094] In an exemplary embodiment, at least one of an exemplary carbon-rich nanostructure, an exemplary plurality of carbon-containing fibers, an exemplary nanostructured network, and combinations thereof may be purified using at least one of an acid solution, a basic solution, an oxidant solution, an organic solution, and combinations thereof. In an exemplary embodiment, an exemplary purifying process may include applying heat, for example, in a furnace. In an exemplary embodiment, an exemplary purifying process may be used for eliminating/reducing dust and impurity from air and environment, for activation, increasing specific surface area, refining morphology of an exemplary carbon rich nanostructure, mending defects, covering defects, functionalization, etc. In an exemplary embodiment, an exemplary purifying process may be performed along with one of irradiation, electrochemical process, freeze-drying, etching, photocatalysis, etc., and combinations thereof
[0095] In an exemplary embodiment, an exemplary nano structured additive may be in-situ synthesized using at least one of a hydrothermal process, a solvothermal process, a chemical reduction/oxidation, irradiation, a thermal process, and combinations thereof. In an exemplary embodiment, a component may be eliminated before or after forming an exemplary nanostructured network using at least one of an organic solvent, an acid solution, a basic solution, an oxidant solution, water, and combinations thereof. In an exemplary embodiment, an exemplary component may depend on an exemplary carbon containing precursor, an exemplary thermoplastic material, additives, etc. In an exemplary embodiment, additives may be added for reinforcement of an exemplary carbon-rich nanostructure, forming a porous structure, or for synergistic effects, covering defects, improving properties of an exemplary carbon rich nanostructure, improving performance of an exemplary carbon rich nanostructure, surface modifications of an exemplary carbon rich nanostructure, adding a roughness, nano roughness, modifying the thermal, rheological, mechanical, tensile properties during or after an exemplary process, forming a composite, nanostructure, superstructure, a metamaterial, a heterostructure, surface modification, conducting fiber morphology, conducting IFN or FRIC steps, adding a feature on an exemplary substrate, achieving a smart, a multi-functional, a multi targeted feature, and combinations thereof, adding a nano, meso, quantum size feature, jagged morphology, increasing exemplary leaving gas flow rate, porosity, etc. and combinations thereof. In an exemplary embodiment, conducting IFN or FRIC steps may include designing smart self-activated topology control mechanisms. In an exemplary embodiment, achieving a smart, a multi-functional, a multi targeted feature may include a smart multi-purpose drug delivery, multi targeted drug delivery and cell attachment, bone cement/injectable gel reinforcement, etc.
[0096] In an exemplary embodiment, an exemplary eliminated component may include one of exemplary additives, for example, a salt, a softener, an electrolyte, a thermoplastic component, a hydrogel, a resin, a nanostructure, a metal, etc., a byproduct (for instance achieved from an in situ synthesis), precursor or intermediates of an in-situ synthesis, an impurity, an attached substrate which may be designed to be detached before, component which may not be proper or designed to remain during a thermal process, creating porosity, hollow fibers, hollow structures, etc. In an exemplary embodiment, an exemplary special approaches may include an additive and/or a thermoplastic and/or a meltable content material may be set to achieve an especial morphology through fiber production or processing, but it may be partially or completely removed according to approaches set through an exemplary thermal process.
[0097] Example 1; Producing intertwined woven-like nanocomposites with control on topology in sharp folded edges [0098] For production of intertwined woven-like nanocomposites, a method similar to method 100 or method 110 may be used. For preparing exemplary intertwined woven-like nanocomposites, a polymer solution of PEG/PAN and a nanocomposite solution of PEG/TiCb were electrospun alternatively. Firstly, two polymer solutions were prepared. For preparing the first polymer solution, a nanocomposite polymer solution was prepared. For preparing the nanocomposite polymer solution, titanium dioxide (TiCh) and PEG were dissolved in distilled water at room temperature. FIG. 2A illustrates a field emission scanning electron microscopy (FESEM) image of exemplary intertwined woven-like nanocomposite nanostructures, consistent with one or more exemplary embodiments of the present disclosure. FIG. 2B illustrates a magnified FESEM image of intertwined woven-like nanocomposite nanostructures shown in FIG. 2A, consistent with one or more exemplary embodiments of the present disclosure. The nanocomposite polymer solution contained 100-150 wt. %, here for the exemplary structure shown in FIG. 2A and 2B, 120 wt. % PEG and 1-5 wt%, here for the exemplary structure shown in FIG. 2A and 2B, 1 wt. % TiCE. The nanocomposite polymer solution was homogenized for 0.2-24 hour here for the exemplary structure shown in FIG. 2A and 2B, 1 hour using a magnetic stirrer. Then, the nanocomposite polymer solution may be sonicated for 0-5 minute (here for the exemplary structure shown in FIG. 2A and 2B, it was sonicated for 1 minute) using an ultrasound probe at ambient temperature before the electrospinning process. The nanocomposite polymer solution was injected using a dual-nozzle pump syringe. A voltage of 15-22 kV was be applied, here for the structure shown in FIG. 2A and 2B, a voltage of 18 kV was applied to the nozzle tips. Pump syringe may set with a flow rate of 0.08-0.4 mL/h, here for the exemplary structure shown in FIG. 2A and 2B, 0.1-0.3 mL/h for 0.5-20 minutes (here for the exemplary structure shown in FIG. 2A and 2B 1-10 minutes) in each turn. The polymer solution, may be injected using a single, dual-nozzle or multi-nozzle. A distance between a collector and a tip of the dual-nozzle pump syringe may be set at 14-25 cm (here for the exemplary structure shown in FIG. 2A and 2B, 20 cm).
[0099] To prepare the second polymer solution, polyethylene glycol (PEG) and polyacrylonitrile (PAN) were mixed with dimethylformamide (DMF). The polymer solution may contain 4-9 wt. %, (here for the exemplary structure shown in FIG. 2A and 2B, 5 wt. %) PAN and 10-17 wt. % PEG (here for the exemplary structure shown in FIG. 2A and 2B, 15% PEG) in DMF solvent. The polymer solution may be homogenized using a homogenizer at room temperature for 30 minutes to 24 hours (here for the exemplary structure shown in FIG. 2A and 2B, 1 hour). The polymer solution, may be injected using a single, dual-nozzle or multinozzle pump syringe with flow rate of 0.1 -0.4 mL/h (here for the exemplary structure shown in FIG. 2A and 2B, 0.1-0.3 mL/h) (accuracy of 0.01 mL/h). The applied voltage to the dualnozzle pump syringe may be set 16-22 kV (here for the exemplary structure shown in FIG. 2A and 2B, applied voltage was 18 kV) and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe may be considered 10-27 cm (here for the exemplary structure shown in FIG. 2A and 2B, applied voltage was 20 cm) for 10-540 min (here for the exemplary structure shown in FIG. 2A and 2B, 60-180 min in each trun).
[00100] For preparing the intertwined woven-like nanocomposites, the polymer solution of PEG/PAN and the nanocomposite solution of PEG/TiO were electrospun alternatively. Here for the exemplary structure shown in FIG. 2A and 2B in the first step, the nanocomposite solution of PEG/TiCh was electrospun for 10 minutes on a collector covered with an aluminum foil. Then, the polymer solution of PEG/PAN was electrospun for (60-180 minutes). After that, the nanocomposite solution of PEG/TiCh was electrospun for (1-10) minutes, the polymer solution of PEG/PAN was electrospun for (60-180 minutes) minutes, the intermediate subsequent turns may be repeated keeping the alternate (for another turn PEG/TiCh, then, PEG/PAN), and for the last step the nanocomposite solution of PEG/TiCh was electrospun for 10 minutes. The collector may be covered with a lace fabric e.g. a PET lace fabric. The collector may be made of a metallic or conductive lace, a magnetic or conductive pattern, etc. A rotary collector may be used. A traverse (partial movement) can be applied between the nozzle tip and the collector. For the structure shown in FIG 2A and 2B a simple collector covered with an aluminum sheet was used.
[00101] After electrospinning the polymer solution on the collector, the electrospun nanofibers was collected from the collector and transferred on a titanium sheet. A thermal process to form integrated fused network (IFN) and a process of fixing and refining the topology via increasing the carbon content (FRIC) were applied on the electrospun nanofibers. The electrospun nanofibers were heated at 220-300 °C, here for the exemplary structure shown in FIG. 2A and 2B, 230°C for 0.5-2 hour, here for the exemplary structure shown in FIG. 2A and 2B, 1 hour under ambient atmosphere. Then, the electrospun nanofibers were heated at 1000 °C under nitrogen atmosphere for 0.5-2 hour (for the exemplary structure shown in FIG. 2A and 2B, 1 hour). The integrated fused network (IFN) was fixed and refined via increasing carbon content and the topology fixed in the form of carbon-rich nanostructure nanocomposite. The heating rate may be 3-15 °C/min, here for an exemplary structure shown in FIG. 2A and 2B, it was 10 °C/min.
[00102] These microscopic images of carbon/graphite samples with woven-like structure even after applying gold coating show nanoscale curves and waves and nanoscale and even quantum size pores and spaces between the fibers. Carbon/graphite samples include nanocurved, nano-wavy and twisted, intertwined structures. As it is clear in the FESEM microscopic image of this sample, the texture is beautifully preserved in the 90 degree bend and similarly expanded in the other direction, which proves the achievement of the desired structure with the texture and bending with the designed angles. FIG. 2B with higher magnification, in addition to showing the excellent dispersion and distribution of nanoparticles on exemplary surface of the innovative interwoven fibrous structures in the nanocomposite sample, also shows more structural details of the interlacings, curves, waves and twists of this unique structure. The abundance and closeness of the fibers and the amount of the thermoplastic component in this example should be chosen in such a way that the fibers be connected to each other and the possibility of forming connections at closer distances enhances. Meanwhile, the thermoplastic component with a high ratio in this example may also have the role of a plasticizer and it may help to bring closer the distances of connections and thermal shrinkage to some extent. The thermoplastic component in this example melts in the initial stages of the thermal process and guides the control of the structure. The thermoplastic component may leave the final structure almost completely or partially, or a small percentage of it may remain. The residue may join the carbon-rich nanostructure.
[00103] Example 2; Creating dome-shaped intertwined woven-like nanostructures on sharp micro-size curvatures
[00104] For producing woven-like nanostructures, a method similar to method 100 or method 110 may be used. To this end, a polymer solution was produced. For preparing the polymer solution, polyethylene glycol (PEG) and polyacrylonitrile (PAN) were dissolved in dimethylformamide (DMF). In this example, the type and composition and the percentage of materials along with the production conditions are selected in such a way that the mixture after leaving the nozzle have a tendency to form a two-phase system comprising elements of thermoplastic or fusible components when the mixture is subjected to solvent evaporation, exposure to the electrospinning process forces with the controlled and selected conditions and/or spinning environment conditions (such as humidity, etc.). The thermoplastic or meltable component, during the subsequent thermal process are able to create connections at the fiber contact/crossing sites and create an integrated fused interconnected network of thermoplastic joints with desired frequency, distances, and control the abundance of the fibers to connect to each other and to create the necessary connections. It is possible to add thermoplastic component to other methods along with or instead of this mode. FIG. 3A illustrates a FESEM image of exemplary dome-shaped intertwined woven-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure. FIG. 3B illustrates a magnified FESEM image of exemplary dome-shaped intertwined woven-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure. The polymer solution, for an exemplary sample shown in FIG 3 A and 3B, contained 5 wt. % PAN and 15 wt. % PEG in DMF solvent. The polymer solution was homogenized using a homogenizer at room temperature for 1 hour. The polymer solution, was injected using a dual-nozzle pump syringe with flow rate of 0.1 mL/h (accuracy of 0.01-0.3 mL/h). The applied voltage to the dual-nozzle pump syringe was 18 kV and a distance between a collector (substrate) and a tip of the dualnozzle pump syringe was 20 cm for an exemplary sample.
[00105] After electrospinning the polymer solution on the collector, the electrospun nanofibers were collected from the collector and transferred on a titanium sheet. Then, a thermal process (IFN) and a process of increasing carbon content (FRIC) were applied on the electrospun nanofibers. The electrospun nanofibers were heated at 220 °C -300 °C, for an exemplary sample shown in FIG. 3A and 3B, 230°C for 30 minutes to 2 hours, here for the exemplary structure shown in FIG. 3A and 3B, 1 hour under ambient atmosphere. Then, the electrospun nanofibers may be heated at 1000 °C under nitrogen atmosphere for 30 minutes to 2 hours (here, for the exemplary structure shown in FIG. 3A and 3B, was 1 hour). The process of increasing the carbon content may include forming the integrated fused network (IFN) and fixing and refining the structure via increasing carbon content (FRIC) of the electrospun nanofibers. The process of increasing the carbon content may include increasing carbon content, fixing, and forming the topology of the integrated fused network.
[00106] The heating rate may be set 5-10 °C/min, here for the exemplary structure shown in FIG. 3A and 3B, it was 10 °C/min. In order to produce a dome-shaped structure, inorganic or polymeric microspheres may be added on the surface of the collector. Inorganic microspheres such as titanium dioxide, silicon dioxide, zinc oxide or salts such as zinc sulfide, zinc nitrate, etc., carbon structures, metallic and organic/ inorganic structures such as MOFs, etc., can be loaded, coated, sputtered, and/or sprayed on the surface through one of the surface modification methods. They can be sprayed or coated, or they can be sprayed or added at the same time as spinning of fibers. Polymeric microspheres can also be added by the same usual methods or be formed simultaneously with the process of producing nanofibers, for example, by an electrospray process. This process can also include spraying capsules, etc. The polymer may be include for example one of materials mentioned for carbon precursor and/or thermoplastic components, etc. such as polyacrylonitrile and its derivatives, chitosan, PVA, PEG, etc. and combinations thereof. The spheres can leave the structure during the process, for example, during the thermal process, to increase porosity of structure or remain and join the carbon structure or a combination of these options may be used. In this example, the simultaneous production of polymer micro sphere and their spraying during the electrospinning of carbon-containing nanofibers was used while designing an electrospray process through a separate nozzle. For example, for the simultaneous production of polymer spheres and spraying them between the nanofibers during, before or between the process (e.g. via a paused process with designed time- intervals from a separate nozzle), etc., a PAN polymer/mixture electro spraying may be used as one of the cheapest options. For example, PAN polymer may be homogenized with a concentration of 2.5-3.5% in DMF for 30 minutes-24 hours, and electrospray with a feed rate 0.5-1 ml/hour, a distance of 10-13 cm, a voltage of 6.5-8.5kV (for instance an AC voltage) may be used. The nozzle may traverse to cover the entire sample.
[00107] For the exemplary structure shown in FIG. 3A and 3B, the electrospun nanofibers were heated at 230°C for 1 hour under ambient atmosphere. Then, the electrospun nanofibers were heated at 1000°C under nitrogen atmosphere. The heating rate was 10°C/minute for the exemplary structure (shown in FIG. 3A and 3B.
[00108] Example 3; Producing bone tissue-like nanocomposites nanostructures
[00109] For production bone tissue-like nanocomposites, a method similar to method 100 or method 110 may be used. For producing bone tissue-like nanocomposites, the polymer solution of PEG/PAN and the nanocomposite solution of PEG/TiO? were electrospun alternatively. To this end, two polymer solutions were prepared. For preparing the first polymer solution, a nanocomposite polymer solution was prepared. For preparing the nanocomposite polymer solution, titanium dioxide (TiCh) and PEG were dissolved in distilled water at room temperature. FIG. 4 illustrates a scanning electron microscopy (SEM) image of exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure. The nanocomposite polymer solution may contain 100- 150 wt. %, here for the exemplary structure shown in FIG. 4, 120 wt. % PEG and 1-5 wt. % here for the exemplary structure shown in FIG. 4, 1 wt. % TiCF. The nanocomposite polymer solution was homogenized for 0.2-24 hour here for the exemplary structure shown in FIG. 4, 1 hour using a magnetic stirrer. Then, the nanocomposite polymer solution may be sonicated or not. The nanocomposite polymer solution may be sonicated for 0.1-5 minute (here for the exemplary structure shown in FIG. 4, it was sonicated for 1 minute) using an ultrasound probe at ambient temperature before the electrospinning process. The nanocomposite polymer solution was injected using a dual-nozzle pump syringe. A voltage of 15-22 kV, here for the structure shown in FIG. 4, 18 kV was applied to the nozzle tips, the pump syringe may run with a flow rate of 0.02-0.5 mL/h, here for the exemplary structure shown in FIG. 4, 0.1 mL/h for 0.5-20 minutes (here for the exemplary structure shown in FIG. 4, 10 minutes) in each turn. A distance between a collector and a tip of the dual-nozzle pump syringe may be set 15-25 cm (here for the exemplary structure shown in FIG. 4, it was 20cm).
[00110] To prepare the second polymer solution, polyethylene glycol (PEG) and polyacrylonitrile (PAN) were mixed with dimethylformamide (DMF). The polymer solution may contain (7-16 wt. %) (here, for the exemplary structure shown in FIG. 4, 11 wt. %) PAN and 0.1-4.5 wt. % PEG, here, for the exemplary structure shown in FIG. 4, 1 wt. % PEG in DMF solvent. The polymer solution was homogenized using a homogenizer at room temperature for (0.5-24 h) (here for the exemplary structure shown in FIG. 4, 1 hour). The polymer solution, was injected using a dual-nozzle pump syringe with flow rate of 0.15-0.6 mL/h, here for the exemplary structure shown in FIG. 4, 0.5 mL/h) (accuracy of 0.01 mL/h). The applied voltage to the nozzles tips pump syringe may be 10-16 kV (here for the exemplary structure shown in FIG. 4, it was 12 kV) and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe may be set 10-17 cm (here for the exemplary structure shown in FIG. 4, it was set 12 cm) for 3-60 min (here for the exemplary structure shown in FIG. 4, 60 min). The collector may be covered with a lace fabric e.g. a PET lace fabric. The collector may be made of a metallic or conductive lace, a magnetic or conductive patterns, etc. for especial approaches. A rotary collector may be used. A traverse (partial movement) can be considered between the nozzle tip and the collector. For the exemplary structure shown in FIG 4, a simple collector covered with an aluminum sheet was used. The system may include at least one nozzle. [00111] For preparing the bone tissue-like nanocomposites, the polymer solution of PEG/PAN and the nanocomposite solution of PEG/TiCh may be electrospun alternatively. Here, for the exemplary structure shown in FIG. 4, in the first step, the nanocomposite solution of PEG/TiCh was electrospun for 10 minutes on a collector covered with an aluminum foil. Then, the polymer solution of PEG/PAN was electrospun for 60 minutes. After that, the nanocomposite solution of PEG/TiO was electrospun for 10 minutes, the polymer solution of PEG/PAN was electrospun for 60 minutes and for the last step the nanocomposite solution of PEG/TiOi was electrospun for 10 minutes.
[00112] After electrospinning the polymer solution on the collector, the electrospun nanofibers were collected from the collector and transferred on a titanium sheet. Then, a thermal process (IFN) and a process for increasing carbon content of the integrated fused network were applied on the electrospun nanofibers. The process of increasing the carbon content may include forming the integrated fused network (FIN) and fixing and refining the structure via increasing carbon content (FRIC) of the electrospun nanofibers. The process of increasing the carbon content may include increasing carbon content, fixing, and conducting formation the topology of the integrated fused network. The electrospun nanofibers may be heated at (220-300 °C, here for the exemplary sample in FIG. 4, 230°C for 30 minutes to 2 hours, here for the exemplary sample in FIG 4, 1 hour under ambient atmosphere. Then, the electrospun nanofibers were heated at 1000 °C under nitrogen atmosphere for 0.5-2 hour (here for the exemplary sample in FIG 4, 1 hour). The heating rate may be set at 10-20 °C/min, here for the exemplary sample in FIG 4, it was 10 °C/min. In this way, by creating a two- or multiphase system, including one phase of at least one thermoplastic or melting component and one phase comprising of carbon fiber precursor, in such a way that the melting component or components are able to create connections at the crossing sites of the fibers, an integrated fused nanostructured network can create via the thermal process. In the integrated fused network structure, the fibers between the connections are subjected to tension during the expansion of the system due to the outflow of gases when exposure to the flow of exhaust gases. Since the fibers are connected with different directions and angles, as a result of the tension, due to the outgoing flow of gases, curves, twists, waves, pores and an amazing architecture, for example, resemble the architecture of bone tissue can be formed. In addition, the thermoplastic material may help to boost flexibility, extension, elasticity and/or elongation of the fiber between the connections just when they are subjected to the tension by the outgoing gases flow, align the polymer chains more effectively and arrange them more by plasticizing the structure.
[00113] It is obvious that inventing such a topology can bring many advantages of natural bone tissue at the same time, only one of which is providing the possibility of cell penetration into the scaffold as one of the biggest challenges of other conventional nanofibrous scaffolds. In addition, the problem of shrinkage and swelling in biological fluids, which causes the pores to close and become inaccessible in the case of most scaffolds, will not exist in the case of scaffolds based on these structures.
[00114] Energy Dispersive X-ray analysis (EDX) was also performed to study weight percent of different elements in an exemplary bone tissue-like nanocomposite. Results showed that there are 74% carbon, 18.9% gold, 6.6% oxygen, and 0.5% titanium in an exemplary bone tissue-like nanocomposite coated with gold for the analyze. It should be notified that EDX is almost a qualitative test. The data resulted from the EDX should not be considered as exact quantitative data. However, the EDX results proved the existence of Ti as a chemical element in TiCh nanostructures in one of bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure FIG. 5 illustrates an Energy-dispersive X-ray spectroscopy (EDX) diagram for exemplary bone tissue-like nanocomposites nanostructures, consistent with one or more exemplary embodiments of the present disclosure.
[00115] Example 4; Producing bone tissue-like nanostructure
[00116] For production bone tissue-like nanostructure, a method similar to method 100 or method 110 may be used. For producing bone tissue-like nanostructure in this example, polyethylene glycol (PEG) and polyacrylonitrile (PAN) were dissolved in dimethylformamide (DMF). FIG. 6 illustrates a SEM image of exemplary bone tissue-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure. The polymer solution may contain (7-16 wt. %) (here for the exemplary sample shown in FIG. 6, it was 13.25 wt. %) PAN and 0.1-4.5 wt. % PEG, here for this exemplary sample, (0.1-1 wt. %) PEG in DMF solvent. The polymer solution was homogenized using a homogenizer at room temperature for 30 minutes to 24 hours (here for this exemplary sample shown in FIG. 6, 2 hour). The polymer solution, was injected using a dual, single or multi-nozzle pump syringe with flow rate of 0.1-0.6 mL/h, here for the exemplary sample in FIG. 6, a single-nozzle syringe with flow rate of 0.22 mL/h (accuracy of 0.01 mL/h) was applied. The applied voltage to the nozzles tips pump syringe may be set 10-16 kV (here for the exemplary sample in FIG. 6, 12 kV) and a distance between a collector and a tip of the dual-nozzle pump syringe may set 10-17 cm (here for the exemplary sample in FIG. 6, 10 cm) for 3-60 min (here 20-45 min).
[00117] The collector may cover with a metal sheet, a fabric, lace fabric, e.g. a PET lace fabric. A rotary collector may be used. A traverse can be considered between the nozzle tip and the collector. For the structure shown in FIG. 6, a simple collector was applied.
[00118] After electrospinning the polymer solution on the collector, the electrospun nanofibers were collected from the collector and transferred on a titanium sheet. Then, a thermal process to form the integrated fused nano structured network and a process of conducting, refining and fixing the topology via increasing carbon content were applied on the electrospun nanofibers. The process of increasing the carbon content may include forming the integrated fused network (IFN) and fixing and refining the structure via increasing carbon content (FRIC) of the electrospun nanofibers. The process of increasing the carbon content may include increasing carbon content, conducting and refining the topology and fixing, of the integrated fused network in form of a topology-controlled carbon-rich nanostructure. The electrospun nanofibers were heated at 220 °C -300 °C, (here for the exemplary sample in FIG. 6, at 230 °C) for 30 minutes to 2 hours, (here for the exemplary sample in FIG. 5, 1 hour) under ambient atmosphere. Then, the electrospun nanofibers were heated at 1000 °C under nitrogen atmosphere for 30 minutes to 2 hours (here for the exemplary sample in FIG. 6, 1 hour). The heating rate may be set at 10 °C/min -20 °C/min, here for the exemplary sample in FIG. 6, 10°C/min, The bone tissue-like nanostructures were hollow sphere-like with spongy cancellous bone-like nano structured shell. It is highly similar to human shin bone tissue structure. It is obvious that the invention of such a topology can simultaneously bring many advantages of natural bone tissue, only two of which include a special architecture, to withstand pressure and to provide the possibility of producing a scaffold with proper porosity and open pores with appropriate size with the advantage of providing (creating) the possibility of cell penetration and compatibility. Cell penetration into the scaffold is one of the biggest challenges of nanofibrous scaffolds, while the problem of shrinkage and swelling in biological fluids intense this challenge, which in most scaffolds causes the pores to close and become inaccessible. This invention response to these challenges by engineering such biomimetic steady topologies resistant also to deformation. It seems that the bone topology may play a remarkable role to provide bones with an amazing resistance to pressure. Thus, achieving such a cancellous bone-like topology especially with graphite or graphite/carbon morphology may simultaneously response to the associated challenges in tissue engineering for restoration of the load-bearing bone tissues which is required not only for cure the diseases but also for damages may unfortunately happen during accidents, natural disasters, etc.
[00119] Analytical characterization of the fixed topologies in form of carbon nanostructures
[00120] FIG. 7A illustrates Fourier transform infrared (FTIR)-attenuated total reflection (ATR) (FTIR-ATR) spectrums of exemplary nanostructures (spectrum 702) and nanocomposites nanostructures (spectrum 704) after an exemplary fixing and refining process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure. Diagram 701 shows magnified view of curve 704 shown in diagram 700. FIG. 7B illustrates FTIR-ATR spectrums of exemplary electrospun bone tissue-like nanostructures before an exemplary heating process for forming integrated fused network (IFN) (spectrum 708) and after an exemplary fixing process in form of carbon nanostructures (spectrum 706), consistent with one or more exemplary embodiments of the present disclosure. A similar trend and almost the same results have been observed for all topologies with the same compositions and same thermal treatments (differences in each point was less than 1% basis of the reported one). As illustrated in FIG. 7A curve 702 shows PEG/PAN nanofiber after an exemplary fixing and refining process in form of carbon nanostructures. The results of the infrared spectroscopic analysis show that after the heating process, all functional groups have been removed from the polymer structure, so that no peak can be seen in the FTIR-ATR spectrum of the carbon-rich nanostructures, FIG 7B, and therefore the results of this conversion analysis confirm and show the complete conversion of polymer nanostructures to carbon nanostructures. The final architectures have a completely "carbon" structure. While FTIR results were identical for different polymers (FIG. 7B, Curve 708) before the heating procedures. Curve 704 shows TiC /PEG/PAN nanocomposite nanofiber after an exemplary fixing and refining process in form of carbon nanostructures. FTIR results were identical for nanocomposite samples containing nanoparticles. Exemplary peaks at 400 cm-1-700 cm'1 and at 1626 cm-1 were characteristic peaks of TiO A similar trend and almost the same result has been observed for all topologies with the same compositions and same thermal treatments (differences in each point was less than 2% basis of the reported one). Curve 704a shows magnified curve 704 of TiCF/PEG/PAN nanofiber after an exemplary fixing and refining process in form of carbon nanostructures. FIG. 8 illustrates a thermogravimetric analysis (TGA) spectrum after an exemplary fixing process in form of exemplary carbon nanostructures for an exemplary bone tissue-like composite, consistent with one or more exemplary embodiments of the present disclosure.
[00121] The weight loss in the sample was recorded up to a temperature of about 700 °C and after that the weight loss was stopped. The weight loss up to 200 °C is usually related to the removal of moisture regains and water molecules may be trapped in the structure, which in this case includes about one percent of the weight loss, after that it is about 3.5 percent. The percentage of weight loss is related to the removal of non-carbon impurities of functional groups connected to structural defects. This analysis also confirms the previous analysis and the results of FTIR-ATR spectroscopy, showing the formation of an almost complete carbon structure in this process. After leaving the furnace, the samples have been analyzed without any further process, even washing, to check the morphology in the minimum conditions and in the most pristine state after production, and therefore this small amount of about 3.5% of carbon impurity can be mainly related to the deposition of gases and vapors inside the furnace on the sample, and the natural structure of the edges. Therefore, achieving a more ideal structure can easily be achieved by various methods of washing or treating with other materials and/or subsequent thermal procedures.
[00122] A similar trend and almost the same result has been observed for all topologies with the same compositions and same thermal treatments (differences in each point was less than 1 % basis of the reported one). FIG. 9 illustrates a Raman spectroscopy spectrum for an exemplary bone tissue-like nanostructure after an exemplary fixing process in form of carbon nanostructures, consistent with one or more exemplary embodiments of the present disclosure. The peak related to the ordered graphite structures is very dominant in the Raman spectrum and it has recorded a significant difference with the peak related to the disordered structures, which shows that the dominant structure even in the sample after leaving the furnace (without any post-treatments is the ordered graphite structure. Therefore, it is easy to achieve a structure with more structural order via various methods of washing or treating with other materials and/or subsequent thermal procedures.
[00123] The structural order of graphite can perform better in terms of characteristics and strength. These results show that especially tension applied to the structure under the gases outflow exposure in wavy and curved areas have increased the ordered graphite structure. Especially considering the rate of temperature increase. Change the angle of the graphene layers in the wavy and curvature graphite structure is formed in the curves. In this way nanocurvature graphitic nanostructures/ nanocomposites with a twisted layered structure and nanowaved graphitic nanostructures/nanocomposites with twisted graphene layers may be formed. The results for the topology of woven-like structures also showed the graphitic structure, but this structure was more dominant in the bone-like structures.
[00124] In addition, the carbon precursor selected for the examples is the cheapest, most available and most abundant precursor on a commercial scale. This selection is due to prove the performance of strategy of this invention to engineer architecture, topology, geometry and morphology based on fibrous or nano-fibrous structures awarding also the unique feature of axial arrangement of the polymeric chains of the precursor in form of fibrous structure and all the advantages resulting from it with the cheap and plenty precursors providing the patients with affordable products.
[00125] The present method is not limited to expensive materials or biomaterials (with the limitation of rare and expensive sources/processing procedures or biomaterials (with further limitations such as high price, limited storage time, storage conditions, unpleasant odor, risk of transmission or absorption and spread of biological pollution, costly and time-consuming multi-step procedures for their extraction, processing and/or use, low chemical, thermal, biological and mechanical resistance (at least for the precursor), etc.) but the method can be used for producing such structures with abundant and cheap materials. The examples show that the control of the morphology, topology and architecture of these structures with cost-effective scalable techniques (with the ability of mass production), which does not require a special mold and is not limited to the morphology of the mold and does not require expensive processes of extraction, purification or subsequent removal of the mold, in a simple way, easily- scalable, without depending on a template or expensive materials. On the other hand, for templatedependent carbon structures, it is not possible to be subjected to tension or basically form fibrous structures, extension is not done because it is in the form of a coating on the mold and the outgoing gas flow does not put much stress on it, so accomplishment such a biomimetic structures and graphitic morphology may not be predicted via the template dependent methods. In addition cheap and abundant available materials are very important for on a commercial scale. [00126] Different solvents for this polymer (PAN) are Dimethylformamide (DMF), dimethylacetamide (DMAc), 6-butyrolactone, dimethylsulfoxide (DMSO), dimethyl sulfone (DMSO2), dimethyl sulfonate (DMSO), DMF/urea, DMSO/urea, m-nitrophenol, carbonates (ethylene carbonate), N -methyl-2-pyrrolidone (NMP), NaScN(aq), LiBr(aq) and ZnC12(aq) concentrate water solutions, ionic liquids (e.g. pyridinium benzylchloride), aqueous acid solutions (e.g. nitric acid and sulfuric acid), other polar organic solvents, hydroxy acetonitrile and mixtures (e.g. hydroxy acetonitrile/ethyl alcohol), etc. and combinations thereof.
[00127] Furthermore, common solvents used in this example arel,l,3,3,3-Hexa-fluoro- 2-propanol (HFIP) can dissolve PET, nylon-6, and polyacrylonitrile (PAN), etc. and combinations thereof. Although the use of other solvents facilitates the design of many structures, the most economical solvent, which is also the most used on a commercial scale, was used for these examples to demonstrate the effectiveness of this invention in controlling the topology even with the cheapest materials.
[00128] Example 5; Creating a smart self-activated microdynamic topology-control mechanism using functionalized substrates and/or post treatments
[00129] To create a smart self-activated microdynamic control mechanism via nanorough friction and/or resin attachment via functionalizing a substrate, a method similar to method 110 was used by adding one of a layer of a resin, a layer of the thermoplastic material, a plurality of nanostructures, patterns of magnetic materials, conductive materials, etching the surface, and combinations thereof on the substrate. As an exemplary sample a bone tissue-like topology were produced by spinning a solution of 7-16 wt. % PAN (for the exemplary sample here about 13%) in DMF (without PEG) to form the plurality of carbon-containing fibers. The plurality of carbon-containing fibers were collected on the functionalized substrate and passed through the thermal treatments (Forming IFN and FRIC) with the functionalized heat resistant substrate. Through the heating process, the thermoplastic and/or meltable materials which their melting points meet the temperatures of the heating process will melt and the fibers may fuse to the substrate and/or each other at the connection sites. The carbon nanostructures further may treat with the nanostructures to produce a nanocomposite. In other exemplary samples patterned carbon nanostructured were devised via applying a resin post treatment after collecting the plurality of carbon-containing fibers on a functionalized heat resistance substrate. Several other exemplary topology-controlled nanostructures have been introduced in FIGs 16- 19 via using a functionalized substrates for collecting nano fibers according to a method similar to method 110.
[00130] In an exemplary embodiment, an exemplary nanoroughness resulting from the coating created with inorganic nanostructures may be considered to create nano roughness and use the resulting friction or nano friction to control movement, shrinkage, and also keep an exemplary plurality of carbon-containing nanofibers at certain places and prevent them from sticking and uncontrolled clumping. Therefore, an exemplary nano roughness may help to create curves, special spaces between curves, applying tension by dealing with thermal shrinkage microdynamically during an exemplary heating process to increase an exemplary arrangement of polymer chains, etc., and an exemplary microdynamic management on topology and morphology of an exemplary plurality of nano fibers. In an exemplary embodiment, the use of resins and applying changes in thermal processes (such as temperature and duration of applying the heat) may also help to control topology of an exemplary plurality of carbon-containing nanofibers. In addition, melting components or thermoplastic materials can also be included in this functionalization. The present disclosure may also establish the dynamic microdynamic, intelligent/microdynamic, intelligent/thermomicrodynamic, methods, etc. and combination thereof to control the thermal shrinkage through the thermal processes in the nano and atomic scale. The existence of resins that may activate an exemplary microdynamic mechanism at different stages of an exemplary thermal process by intelligently fusing the fibers to the surface of an exemplary substrate at the same time as the tendency to thermal shrinkage increases (with increasing temperature). In an exemplary embodiment, the combination of these three fusing mechanisms (in a scale of nano or larger), nano friction of roughness as well as nano fiber entanglement in nanometer spaces between nano structures may be considered together.
[00131] The substrate for electrospinning the spinning solution was treated before the electrospinning process. The functionalized substrate designed to go through the fixing and refining the topology via increasing carbon content (FRIC) with the integrated fused nanostructured network of two/multi-phase system and/or designed to go through the forming integrated fused network (IFN) of the two/multi-phase system may be a heat and or shrinkage resistant substrate e.g. a carbon fabric substrate, glass fabric, and so on. The substrate may be a carbon-forming material, a graphite- forming material, a carbon/ graphite-forming material. Carbon forming substrate e.g. a layer of cellulose fabric, PAN fabrics (including its copolymers (modacrylic) as the most common accessible fabrics in this category. The selection of fabric structures for the substrate according to the existing gaps between the filaments and/or yarns in the fabric construction and between the nanostructures may provide special channels for the gas outflow during the thermal process, while the connections created also keep the nanofibers on the fabric yarns and prevent from their possible penetration into the space between the yams with the flow of gases. Thus, in the exemplary functionalizations micro-carbon fabric and mercerized cotton fabric (cellulosic fabrics) were among the selections for functionalizations and application. The micro carbon fabrics treated with 1 wt. % to 10 wt. % aqueous colloidal solution of at least one of TiCh nanoparticles, clay nano layers, zinc oxide (ZnO) nanoparticles, silicon dioxide (SiCh) nanoparticles, graphene oxide (GO), silver/silicon dioxide (Ag/SiO ) nanostructures, FC3O4 nanoparticles, silver (Ag) nanoparticles and combinations thereof. The micro carbon fabrics were immersed inside the aqueous colloidal solutions for 10 seconds to 60 seconds. Then, the carbon fabrics were padded with 50% to 100% wet-pick up. The padded fabrics were then dried at a temperature of 10°C to 100°C. Some fabrics were also treated with a resin. Some resin e.g. PVA, PEG, etc. were used also in combination with the nanostructures by applying an aqueous mixture of resin and the nanostructures or by applying a layer of resin on the pre-nanofunctionalized fabrics with the nanostructures. In an approach for in- situ polymerization in- situ synthesis of a resin (a hydrogel), the nanofunctionalized micro carbon fabrics with the nanostructures or the untreated micro carbon fabrics were immersed inside a potassium persulfate aqueous solution (K2S2O8, 0.4 wt. %) for 10 seconds. Then, the functionalized carbon fabrics were padded and dried. After that, the padded functionalized micro carbon fabrics were immersed inside an aqueous solution of disodium hydrogen phosphate (8 wt. %) and acrylic acid monomer (8 wt. %) at pH of 7 for 15 seconds. The pH was adjusted using sodium carbonate. The functionalized carbon fabric was padded and left for 30 minutes at ambient temperature (28°C). The treated carbon fabrics were dried at a temperature of 110°C for 2 minutes to 10 minutes. Then, the functionalized carbon fabrics were cured at a temperature of 135°C to 200°C. The temperature of curing depends on the thermal resistance of the substrate. The same procedure was also applied on cellulosic fabrics.
[00132] The fabrics may be also functionalized using at least a polymer, a resin, and combinations thereof. The polymer and the resin may be in-situ polymerized on a substrate or may be added on the substrate using spray coating, impregnation, brushing, exhaustion, coating, dipping, impregnation, roll coating, padding, electro spraying, sputtering, etc. One of resin used for functionalizing the fabric was self-cross-linkable amino-functionalized polysiloxane resin with a weight ratio of 0.06 wt. % to 10 wt. %. The applied weight percent for the exemplary reported samples was 1.7 wt. % of the resin. The fabrics (the nanofunctionalized or untreated ones) was impregnated with the resin for 3 seconds to 10 seconds. The impregnated fabric was padded with 50% to 100% wet-pick- up. The padded fabric was dried at a temperature of 10°C to 200°C. Some of micro carbon fabrics were inserted into polysiloxane resin treatment after the pre nanofunctionalization with nanostructures and the in-situ polymerization. The same procedures were also applied on cellulosic fabrics with 1.5-3.5 wt. % polysiloxane resin.
[00133] Before analyzing the functionalized fabrics treated with the cross-linked resins, the functionalized fabrics were washed to remove unreacted materials. The functionalized fabrics were subjected to a fastness evaluation process to investigate the efficiency of the crosslinking and/or in-situ formed linkages through the in-situ polymerization to prevent leaching of nanostructures out. The washing process was performed in 40 cycles with 5g/L detergent in water at a temperature of 60 °C. Each cycle of the washing process was elongated for 30 minutes of treating the functionalized fabric with the detergent solution, the 40 cycles washing, then, followed by 200 hours immersing the fabric in the solution on the shaker + neutralization, rinsing with distilled water, 30 minutes immersing in the ultrasonic bath with detergent + 200 hours immersing in the solution on the shaker, rinsing and drying. The washing process was performed for evaluating the stability in different conditions. Nanostructures released from the functionalized fabric into the washing solution was a measure of resistance to leaching. To this end, effluents gained from the washing process were examined using inductively coupled plasma (ICP) spectroscopy. The stability of over 98% resulted from the use of silicone resins and the stability of about 97% for silicone treated synthesized polysodium acrylate and the stability of about 94% for polysodium acrylate without silicon was estimated. Microscopic images also show the presence of nanostructures on the fiber surface after passing this evaluation. The functionalized fabrics were also studied using microscopes after sputtering gold on the functionalize fabric. The microscopic techniques were used to study fastness and morphology of nanostructures on the functionalized fabrics. FIG. 10 illustrates a SEM image of a micro carbon fabric substrate modified by exemplary clay nano layers on, consistent with one or more exemplary embodiments of the present disclosure. Microscopic evidence of functionalization the substrate of micro carbon fabric modified with clay nanolayers, shows the successful transfer of nanostructures on the surface with method 110. The micro carbon fabric was selected as a shrinkage resistant and thermal resistant substrate for this functionalization and then collecting the nanofibers. FIG. 11 illustrates a SEM image of functionalized micro carbon fabric modified with exemplary inorganic nanoparticles and resins after the fastness evaluation procedures, consistent with one or more exemplary embodiments of the present disclosure. Microscopic evidence of functionalization the substrate of micro carbon fabric modified with inorganic nanoparticles and resin compounds (according to method 110) which shows the successful transfer of nanostructures on the surface and their stability after successive washing procedures and exposure to various acute conditions, which is used in this disclosure as a suitable method for the functionalization of the carbon fabric substrate. The micro carbon fabric was selected due to its shrinkage resistance and thermal resistance as the substrate to collect the nanofibers. The micro carbon fabric was functionalized with inorganic nanoparticles and resins. The SEM image shows nanofunctionalized micro carbon fabric subjected to the fastness evaluation procedures including the frequent washing process, etc. after functionalizing the micro carbon fabric.
[00134] FIG. 12 illustrates a SEM image of functionalized micro carbon fabric modified with exemplary clay nano layers and resins, consistent with one or more exemplary embodiments of the present disclosure. The SEM image shows nanofunctionalized micro carbon subjected to the fastness evaluation procedures including frequent washing process, etc. Microscopic evidence of functionalization the substrate of micro carbon fabric modified with clay nanolayers with a higher percentage than in FIG. 10 along with resin compounds (according to method 110) shows successful transfer of nanostructures on the surface of the carbon fabric and their stability after successive washings and exposure to various acute conditions. As a suitable method for the functionalization of the carbon substrate, which is also used in this disclosure.
[00135] A resin or a plurality of resins may be used to coat the plurality of collected fibers before the thermal procedures to form the integrated fused networks (IFN) and fixing and refining the topology via increasing carbon content (FRTC). The polymer and the resin may be added on the fibers using spray coating, impregnation, brushing, exhaustion, coating, dipping, impregnation, roll coating, padding, electrospraying, sputtering, etc. the resin including the thermoplastic components may be applied at least with a molecular thickness. Resins e.g. PVA (aq 1-10%), mixture of PVA (aq) and (0.1-2% HTCC(aq), mixture of PVA (aq) and/or PEG and (0.1-2% glucose), etc. and combination thereof were applied with brushing, spraying and/or electro spraying for the exemplary reported samples with a resin post- treatment in the examples (e.g. FIG 14, etc.). Self cross-linkable polysiloxane resin was used as one of the resin for producing functionalized fabrics. The in-situ synthesized resins and the cross-linkable resins especially self cross-linkable ones are especially efficient when an intermediate process e.g. washing, functionalization, hydro/solvo thermal synthesis are performed.
[00136] In these examples, the use of resins or acrylate hydrogel also provides the possibility of relative movement of fibers for nano-size displacement and trapping between nanometer roughness, and if the melting of thermoplastic resins takes place in the initial stages and also at higher temperatures (when more than one meltable/ thermoplastic component is included), it is possible to enhance the efficiency. For example, silicone resins may melt at higher temperatures, and may strengthening the connection of the fiber with the substrate at their melting point, simultaneously they may have a plasticizing effect on the fiber, they improve the effect of tension (by the outflow gasses) on the fiber and may result in the polymer chain arrangement, while thermal expansion and exposing to the outflow of gases. In addition, the functionalizations presented in the examples of this disclosure has been done in an aqueous environment and neutral pH as a green process.
[00137] The resins can be also coated on the carbon-rich nanostructures to fix the nanostructures on the fabric which is desirable for filtration applications, etc. and/or for their surface modification e.g. for controlled cell attachment approaches.
[00138] In this example, acrylate coatings, in addition to the mentioned cases, in terms of similarity to the carbon fiber precursor in this example, and its graft (chemical bonds and linkages) for reasons such as providing proper stability, on the other hand, because of providing more effective control of fibers on the substrate with considering the high capacity of keeping moisture (especially in the form of nanocomposite with inorganic nanostructures), it was designed as a nonsolvent for PAN and compatible surface feature with PEG.
[00139] FIG. 13 illustrates a SEM image of exemplary bone tissue-like nanostructures formed on an exemplary functionalized substrate, consistent with one or more exemplary embodiments of the present disclosure. The substrate was a carbon fabric functionalized by a resin including a thermoplastic resin component and the nanostructures. The bone-like structures have been produced via electrospinning pure PAN (13 wt. %) in DMF without PEG, thermoplastic component is only included in the resin treatment of the substrate for this exemplary sample. For this exemplary sample a bone tissue-like topology were produced by spinning a solution of 7-16 wt. % PAN (for the exemplary sample here 13%) in DMF (without PEG) to form the plurality of carbon-containing fibers. The plurality of carbon-containing fibers were collected on the functionalized substrate and passed through the heat treatments with the functionalized heat resistant substrate. Through the heating process the thermoplastic and/or meltable materials which their melting points meet the temperatures will melt and the fibers may fuse to the substrate and/or each other at the connection sites. The carbon nanostructures exemplary sample further was treated with nanoparticles to produce a nanocomposite. For producing this exemplary sample the polymer solution (13% PAN in DMF) was homogenized using a homogenizer at room temperature for (30 minutes -24 hours) (here 2 hours). The polymer solution, was injected using a dual, single or multi-nozzle pump syringe with flow rate of 0.2-0.6 mL/h, here a dual-nozzle syringe with flow rate of 0.2 mL/h (accuracy of 0.01 mL/h) was applied. The applied voltage to the nozzles tips pump syringe was 11-13 kV and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe was 10-14 cm the fibers were collected for 10-20 min. After electrospinning the polymer solution on the functionalized substrate on the collector, forming the integrated fused network and fixing and refining the topology via increasing carbon content were applied on the electrospun nanofibers on the functionalized substrate. The electrospun nanofibers were heated at (220-300 °C, here for the exemplary sample 230°C here for the exemplary sample 1 hour under ambient atmosphere. Then, the integrated connected network fixed via increasing carbon content and the topology formed and refined at 1000 °C under nitrogen atmosphere for 0.5-2 hour (here for the exemplary sample, 1 hour). The heating rate may be set at 10-20 °C/min, here for the exemplary sample, it was 10°C/min
[00140] FIG. 14 illustrates a SEM image of an exempalry quantum-size fibrous pattern formed on graphitic cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure. The quantum-size fibrous pattern formed on the graphitic cancellous bone-like structures are multilayered porous multiple-scaled of micro, nano, meso and quantum size structures. The patterned bone -like structures have been produced via the post resin treatment on the electrospun pure PAN (13.5 wt. %) in DMF. For producing the quantum-size fibrous pattern formed on the graphitic cancellous bone-like structures. In this exemplary sample, the substrate of the micro carbon fabric was functionalized by a resin including a thermoplastic resin component and the nanostructures. The bone-like structures have been produced via electrospinning pure PAN (13.5 wt. %) in DMF without PEG, thermoplastic component was included in the resin treatment of the substrate and post resin treatment on the electrospun fibers for this exemplary sample. For this exemplary sample a bone tissue-like topology were produced by spinning a solution of 7-16 wt. % PAN (for the exemplary sample here 13.5%) in DMF (without PEG) to form the plurality of carbon-containing fibers. The plurality of carbon-containing fibers were collected on the functionalized substrate and passed through the heat treatments with the functionalized heat resistant and shrinkage resistant substrate (micro carbon fabric). Through the heating process the thermoplastic and/or meltable materials which their melting points meet the temperatures will melt and the fibers may fuse to the substrate and/or each other at the connection sites. For electrospinning the nanofibers, the polymer solution was homogenized using a gentle homogenizer (here, a magnetic stirrer) at room temperature for (0.5-24 h) (here 2 hour). The polymer solution, was injected using a dual, single or multi-nozzle pump syringe with flow rate of 0.2-0.6 mL/h, here for the exemplary topology shown in FIG 14, a dual-nozzle syringe with flow rate of 0.26 mL/h (accuracy of 0.01 mL/h) was applied. The applied voltage to the nozzles tips pump syringe was 11-14 kV and a distance between a collector (substrate) and a tip of the dual-nozzle pump syringe was 10-14 cm. The process was performed for 20-40 min. After electrospinning the polymer solution on the functionalized carbon substrate on the collector, a resin post-treatment of one of PVA (aq 5-10%), mixture of the PVA (aq) and (0.1-2% HTCC (aq), mixture of PVA (aq) and/or PEG and (0.1-2% glucose), and combination thereof was applied, consistent with one or more exemplary embodiments of the present disclosure. Then, forming the integrated fused network and after that fixing and refining the topology via increasing carbon content were applied on the electrospun nanofibers on the functionalized substrate. The electrospun nanofibers were heated at (220-300 °C, here for the exemplary sample shown in FIG 14, 230°C here for the exemplary sample shown in FIG 14, 1 hour under ambient atmosphere. Then, the integrated fused network fixed via increasing carbon content and the topology formed at 1000 °C under nitrogen atmosphere for 0.5-2 hour (here for the exemplary sample shown in FIG 14, 1 hour). The heating rate may be set at 7-20 °C/min, here for the exemplary sample shown in FIG 14, it was 10°C/min. FIG. 15 illustrates a SEM image of exemplary fish-like patterns developed on a micro carbon fabric, consistent with one or more exemplary embodiments of the present disclosure. The micro carbon fabric was nanofunctionalized and the electrospun fibers were also post treated using a layer of resins. FIG. 16 illustrates a SEM image of exemplary multiaxial intertwined woven-like nanostructures formed on a circular/radial-patterned substrate, consistent with one or more exemplary embodiments of the present disclosure. The fibrous nanostructures were formed according to the general method of Example 3. FIG. 17 illustrates a SEM image of exemplary nanoflowers with a carbon shell, consistent with one or more exemplary embodiments of the present disclosure. The nanoflowers having sub-50 nm needle like petals with high aspect ratio were formed on the innovative graphitic cancellous bone-like carbon structures reported in FIG. 14. The nanoflowers were coated with one of an aqueous glucose solution, chitosan aqueous solution and HTCC aqueous solution and combination thereof and/or PAN (0.2-2%) and/or PEG (1-10 %) in DMF and combination thereof before the forming the integrated fused network and fixing and reforming the topology via increasing carbon content. FIG. 18 illustrates a SEM image of exemplary rose-shaped nanostructures, consistent with one or more exemplary embodiments of the present disclosure including an intermediate washing performed after electrospinning process on a patterned substrate. The intermediate washing was performed with hot water (65-75°C to partially remove PEG (the ratio of PEG to PAN was 4-5 before washing process) to create porous nanofibrous structure and refine the PEG content for this approach). The rose-shaped nanostructures were porous continuous nanofibrous roselike structures. FIG. 19 illustrates SEM images of exemplary cancellous bone-like nanostructures, consistent with one or more exemplary embodiments of the present disclosure. The cancellous bone-like nanostructures were produced by reducing electrospinning time. The innovative engineered strategies of this invention also include changing various factors such as the type of precursor, polymer mixtures or simple and single-component types, etc., their ratio, adding additives, substrate structures and types, pre-treatments and/or treatments on substrate, application of nanostructures, resins or nanocomposites pre-, after- and/or post-treatments, the production methods and conditions (for instance in the reported examples production methods are based on nanofiber production and production variants are including solution and processing parameters, humidity and ambient conditions, etc. e.g. solution characteristics, type and speed of collector, type and number and conditions of nozzle, other process parameters, etc.), after treatments, intermediate procedures, thermal processes, etc., to control the morphology of carbon structures produced on the basis of fibrous production in order to control the desired morphology, topology, geometry, architecture and structure which are within the scope of this disclosure. [00141] It is also possible to use the strategies of this disclosure when the nanofibers are collected in the form of yarn or in the coagulation bath, etc. The products of this method can be converted and used in the form of powder or colloidal solution, gel, paste, etc., which can be easily transferred to other surfaces and goods, and can also be used in the structure or precursor of other products, for example, in mixing with solutions or molten polymers or monomeric materials during in-situ synthesis, and in the same way precursors or intermediary materials for the process of metals, metal alloys, glass, ceramics, rubber, plastic, etc. or their precursors, in-situ synthesis of polymers, alloys, hybrids, different types of composites and modification of the surface or bulk of materials can also be integrated with various molding processes (melt, solution, etc.), such as the production of fibers, nanofibers, films and thin layers, coating, etc., different types of carbon-containing nanofibers including hybrid, multicomponent, hollow, porous, etc., alone or together with other nano, micro, meso, quantumsized, multi-scale structures, etc.
[00142] The development of any nanocomposite, hybrid, mixed material, the growth of any new structure, the creation of any pattern, additives, any polymer coating or modification, etc., with any method and technology, in addition to the production process on the surface of the product or on the product bulk, as well as the formation of structures such as patterns, roughness, etc., jagged structures, dentate -edge, multi-branched structures, pores, etc., in the meso, nano, quantum, micro and non-nano scale, etc., is possible using the products of this disclosure.
[00143] The production or process of the products of this invention can be combined or used with other methods such as lithography, surface etching, radiation, chemical, physical, atomic deposition, vapor state, etc. .
[00144] The present method disclosed herein may be used for the functionalization of any type of product or material such as hydrogels, resins, polymers, polymer mixtures, micro or non-nano carbon structures, porous, quantum-size, nanoscale or non-nano structures, carriers, carriers, capsules, resin, spinning oil, polymer synthesis precursor, paper, rubber, plastic, banknote, glass, ceramic, and various materials, paste, melt, solution, etc.
[00145] The present method disclosed herein may be used with other methods, for example, gel-spinning, dry-spinning, all kinds of melting processes, solution, etc., pad-dry, pad-dry-cure, exhaustion , spraying, printing nanostructures, synthesis, in situ synthesis, spin coating, sol-gel, various spinning process, ultrasound, irradiation, etc. [00146] The present method disclosed herein may be used, followed or integrated. In polymer, inorganic, glass, ceramic, metal, alloy and hybrid substrates, hybrid, composite, alloy, porous, patterned, functionalized and/or untreated, template, etc. and in a combination or any set of combinations and synergistic structures with any scale and feature.
[00147] All components of products based on this disclosure and their direct and indirect effects can be green, safe, renewable, sustainable, eco-friendly, bioinspired, and/or biomimetic. Any additive can be added to the carbon or graphite structures of this invention by developing or growth other materials, such as the production of carbon, graphite, carbon/graphite nanoflowers, etc.
[00148] Example 6: Analyzing cell viability and biocompatibility of produced nanostructures
[00149] Cell viability and biocompatibility test were investigated via an in vitro MTT (3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide) standard cell culture assay. The cell preparation and the in vitro evaluations all were conducted with respect to all the associated ethical principles by the experts at the associated valid and authoritative biological institutes. Each carbon structure was added in 50 ppm concentration to the standard cell culture media in a 96-well plate withlOOOO cell/well. The cell culture was followed for 6 days and performed in triplicates for each sample. To record the results after 6 days, the supernatant was eliminated from the wells and they were washed with PBS. Each well, then, was treated with serum-free medium and 5mg/ml of MTT detector and incubated for 4 hours. The purple sediments were, then, dissolved in dimethyl sulfoxide (DMSO) and the optical densities were recorded at 570 nm by an Elisa reader for each well. The results were averaged for each sample from the triplicate data.
[00150] ELISA readers or micro plate readers is an analytical instrument for spectrophotometry and evaluation the color difference values which is compatible with a 96- well plate. The evaluation is based on emitting a light beam at the specific wavelength, and recording the density of the absorbed beam by the sample in each well.
[00151] For microscopic study, another series of 7-day post-seeded scaffolds were considered. After the 7 days cell culture, the scaffolds of the carbon nanostructures were washed and then, were fixed using a glutaraldehyde solution (2.5%). After that, the scaffolds were dehydrated using the serial ethanol dilutions and dried, then, they were coated via gold sputtering. [00152] FIG. 20 illustrates a SEM image of cell attachment on exemplary produced nanostructures, consistent with one or more exemplary embodiments of the present disclosure. The results of MTT test has also indicated biocompatibility in comparison with tissue culture polystyrene (TCPs). The architectural effect (the effect of topology) of the porous scaffold is so dominant in this disclosure that even with the relative hydrophobicity of the surface and without any subsequent process, coating, or surface modification, it has led to excellent cell adhesion. It is obvious that the use of appropriate biopolymer coatings and other biomaterials, etc., can significantly improve these unique results and mark a new era in biomedical applications with a perspective to help the patients. At the same time, due to simulating bone tissue, the structures based on it can meet the amazing properties of bone, such as bearing load and pressure, and response the challenge of the weakness of biomaterials in tissue engineering, especially load-bearing hard tissue engineering.
[00153] Industrial Applicability
[00154] The present disclosure may be used for controlling topology of nanostructures. Nanostructures may be applicable for different applications such as medicine (such as drug delivery, bone tissue engineering, etc.), agriculture, water purification, etc. Designing the process of synthesizing nanostructures by changing the thermoplastic material, the temperature of curing, functionalizing the substrate, adding additives, engineering of solution and production parameters, etc. can change the topology of nanostructures.
[00155] While the foregoing has described what are considered to be the best mode and/or other examples, it is understood that various modifications may be made therein and that the subject matter disclosed herein may be implemented in various forms and examples, and that the teachings may be applied in numerous applications, only some of which have been described herein. It is intended by the following claims to claim any and all applications, modifications and variations that fall within the true scope of the present teachings.
[00156] Unless otherwise stated, all measurements, values, ratings, positions, magnitudes, sizes, and other specifications that are set forth in this specification, including in the claims that follow, are approximate, not exact. They are intended to have a reasonable range that is consistent with the functions to which they relate and with what is customary in the art to which they pertain.
[00157] The scope of protection is limited solely by the claims that now follow. That scope is intended and should be interpreted to be as broad as is consistent with the ordinary meaning of the language that is used in the claims when interpreted in light of this specification and the prosecution history that follows and to encompass all structural and functional equivalents. Notwithstanding, none of the claims are intended to embrace subject matter that fails to satisfy the requirement of Sections 101, 102, or 103 of the Patent Act, nor should they be interpreted in such a way. Any unintended embracement of such subject matter is hereby disclaimed.
[00158] Except as stated immediately above, nothing that has been stated or illustrated is intended or should be interpreted to cause a dedication of any component, step, feature, object, benefit, advantage, or equivalent to the public, regardless of whether it is or is not recited in the claims.
[00159] It will be understood that the terms and expressions used herein have the ordinary meaning as is accorded to such terms and expressions with respect to their corresponding respective areas of inquiry and study except where specific meanings have otherwise been set forth herein. Relational terms such as first and second and the like may be used solely to distinguish one entity or action from another without necessarily requiring or implying any actual such relationship or order between such entities or actions. The terms “comprises,” “comprising,” or any other variation thereof, are intended to cover a nonexclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. An element proceeded by “a” or “an” does not, without further constraints, preclude the existence of additional identical elements in the process, method, article, or apparatus that comprises the element.
[00160] The Abstract of the Disclosure is provided to allow the reader to quickly ascertain the nature of the technical disclosure. It is submitted with the understanding that it will not be used to interpret or limit the scope or meaning of the claims. In addition, in the foregoing Detailed Description, it can be seen that various features are grouped together in various implementations. This is for purposes of streamlining the disclosure, and is not to be interpreted as reflecting an intention that the claimed implementations require more features than are expressly recited in each claim. Rather, as the following claims reflect, inventive subject matter lies in less than all features of a single disclosed implementation. Thus, the following claims are hereby incorporated into the Detailed Description, with each claim standing on its own as a separately claimed subject matter. [00161] While various implementations have been described, the description is intended to be exemplary, rather than limiting and it will be apparent to those of ordinary skill in the art that many more implementations and implementations are possible that are within the scope of the implementations. Although many possible combinations of features are shown in the accompanying figures and discussed in this detailed description, many other combinations of the disclosed features are possible. Any feature of any implementation may be used in combination with or substituted for any other feature or element in any other implementation unless specifically restricted. Therefore, it will be understood that any of the features shown and/or discussed in the present disclosure may be implemented together in any suitable combination. Accordingly, the implementations are not to be restricted except in light of the attached claims and their equivalents. Also, various modifications and changes may be made within the scope of the attached claims.

Claims

79
What is claimed is:
1. A method for forming at least one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopatterned carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled- topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof, the method comprising: functionalizing a substrate by at least one of adding a layer of a resin on the substrate, adding a layer of at least one thermoplastic material on the substrate, adding a layer of a plurality of nanostructures on the substrate, forming a pattern of a magnetic material on the substrate, adding a layer of an electrically conductive material on the substrate, adding a patterned layer of an electrically conductive material on the substrate, etching surface of the substrate, and combinations thereof; forming a plurality of carbon-containing fibers on the substrate using a mixture containing a carbon fiber precursor; forming a two or multi-phase structure by adding at least one thermoplastic material to the plurality of carbon-containing fibers, the at least one thermoplastic material having a melting point below 450 °C; forming a nanostructured network by forming a plurality of thermoplastic connections among the plurality of carbon-containing fibers, forming the nano structured network comprising melting the at least one thermoplastic material among the plurality of carbon-containing fibers by heating the two or multi-phase system to a temperature up 80 to 450 °C, the nanostructured network comprising a plurality of carbon-containing fibers connected to each other via the plurality of thermoplastic connections; forming a carbon-rich nanostructure by increasing carbon content of the nanostructured network via removing at least one non-carbon containing element in form of gases from the nanostructured network, removing the at least one non-carbon containing element comprising heating the nanostructured network to a temperature of 800 °C or more under an inert atmosphere; and adding an additive to the carbon-rich nanostructure by coating a layer of the additive with a thickness up to 1 mm on the carbon-rich nanostructure, the additive comprising at least one of the thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compound, an electrolyte, and combinations thereof. A method for controlling topology of carbon-rich nanostructures, comprising: forming a plurality of carbon-containing fibers using a mixture containing a carbon fiber precursor; forming a two or multi-phase system by adding at least one thermoplastic material to the plurality of carbon-containing fibers, the thermoplastic material having a melting point below 450 °C ; forming a nanostructured network by forming a plurality of thermoplastic connections among the plurality of carbon-containing fibers, forming the nano structured network comprising melting the at least one thermoplastic material among the plurality 81 of carbon-containing fibers by heating the two or multi-phase system to a temperature up to 450 °C, the nanostructured network comprising a plurality of carbon-containing fibers connected to each other via the plurality of thermoplastic connections; and increasing carbon content of the nanostructured network by removing at least one non-carbon containing element in form of gases from the nanostructured network, removing the at least one non-carbon containing element comprising heating the nanostructured network to a temperature of 800 °C or more under an inert atmosphere.
3. The method of claim 2, wherein controlling the topology of the carbon-rich nanostructures comprises forming one of woven-like carbon-rich nanostructures, bone-like carbon-rich nanostructures, bone-tissue like carbon-rich nanostructures, multiaxial intertwined woven-like nanostructures, fish-like nanopatterned carbon-rich nanostructures, dome-shaped intertwined woven-like nanostructures, quantum size fibrous structures, sharp-fold controlled- topology, sharp-jagged nanocomposite, hollow sphere bone-tissue like shell, multiple scaled porous structures, nanocomposites of multiple scaled porous structures, and combinations thereof.
4. The method of claim 2, wherein the carbon fiber precursor comprises at least one of polyacrylonitriles, plysaccharides, cellulosic compositions, lignin, lignocellulose, carbohydrates, chitin, chitosan, polyarylenes, co-tri-polymers of polyarylenes, derivatives of polyacrylonitriles, derivatives of plysaccharides, derivatives of cellulosic compositions, derivatives of lignin, derivatives of lignocellulose, derivatives of carbohydrates, derivatives of chitin, derivatives of chitosan, derivatives of polyarylenes, and combinations thereof. 82
5. The method of claim 2, wherein forming the plurality of carbon-containing fibers comprises forming the plurality of carbon-containing fibers utilizing a process comprising at least one of electrospinning, electrospinning with bi or multi- parallel or opposite nozzles, coaxial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugal-blowing spinning, disk jet spinning/electrospinning, needleless electrospinning, magnetic fields -assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet-electrospinning, wet or gel electrospinning, and combinations thereof.
6. The method of claim 2, wherein the thermoplastic material comprises at least one of polyvinyl alcohol (PVA), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), a hydrogel, polyethylene oxide (PEO), an acrylic acid, an acrylic acid derivatives, an acrylate, a poly(sodium acrylate), a polyester, a polyamide (PA), a polyimide, a poly(amidoamine) (PAMAM), a silicone, a silicone compound, a poysiloxane, a polyol, a carbohydrate derivatives, an oligomer, a co-or tri-polymer, and combinations thereof.
7. The method of claim 2, wherein adding the at least one thermoplastic material to the plurality of carbon-containing fibers comprises at least one of adding the at least one thermoplastic material to the mixture containing the carbon fiber precursor, adding the at least one thermoplastic material to the plurality of carbon-containing fibers while forming the plurality of carbon-containing fibers, adding the at least one thermoplastic material to the plurality of carbon-containing fibers after forming the plurality of carbon-containing fibers, and combinations thereof. 83
8. The method of claim 7, wherein adding the at least one thermoplastic material to the plurality of carbon-containing fibers while forming the plurality of carbon-containing fibers or after forming the plurality of carbon-containing fibers comprises adding the at least one thermoplastic material to the plurality of carbon-containing fibers utilizing a process comprising at least one of spraying, exhaustion, coating, dipping, impregnation, roll coating, padding, electro spraying, sputtering, a fiber/nanofiber co(parallel) elctro/spinning, a parallel electrospinning with bi or multi- parallel or opposite nozzles with same, opposite, or alternating charge, co-axial or side or segmented-nozzle electrospinning, force (rotary jet) spinning, blowing (air-jet) spinning, electro-centrifugal spinning, electro-blowing spinning, centrifugalblowing spinning, disk jet spinning/ electrospinning, needleless electrospinning, magnetic fields-assisted electrospinning, irradiation-assisted electrospinning, dry-jet-wet- electrospinning, wet or gel-electro/spinning, sequential layer by layer fiber forming/electrospinning, a post- electrospinning, and combinations thereof.
9. The method of claim 2, wherein heating the two or multi-phase structure to a temperature up to 450°C comprises heating the two or multi-phase structure to the temperature up to 450°C under at least one of air atmosphere, an inert gas atmosphere, and combinations thereof, wherein the inert gas comprises at least one noble gas.
10. The method of claim 2, wherein forming the plurality of carbon-containing fibers comprises forming the plurality of carbon-containing fibers on a substrate, the substrate comprising at least one of a fabric, a layer, a film, a paper, a sheet, a lace, a web, and combination thereof of a heat resistant material, a carbon-forming material, a graphite -forming 84 material, a carbon/ graphite-forming material, a substrate configured to be separated from the nanostructured network before a heating process to a temperature above 200°C, and combinations thereof.
11. The method of claim 10, wherein the substrate comprises at least one of a carbon fabric, a micro-carbon fabric, a cellulosic fabric, an acrylic substrate, a layer of polysaccharides, a layer of polysaccharide derivatives, lignin, lignocellulose, a carbohydrates, a carbohydrate derivatives, polyacrylonitriles, a metal sheet, a layer of mercerized cellulose, polyester laces, and combinations thereof.
12. The method of claim 10, further comprising functionalizing the substrate by at least one of adding a layer of a resin on the substrate, adding a layer of the at least one thermoplastic material on the substrate, adding a layer of a plurality of nanostructures on the substrate, forming a pattern of a magnetic material on the substrate, adding a layer of an electrically conductive material on the substrate, adding a patterned layer of a conductive material on the substrate, etching surface of the substrate, and combinations thereof.
13. The method of claim 12, wherein the plurality of nanostructures comprises at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO) a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron 85 phosphorus trisulfide (FcPSr,). Strontium stannate (SrSnos), Tungsten ditelluride (WTe2),
Potassium heptafluorotantalate (KsTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgBi), Niobium disulfide (NbSz), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof.
14. The method of claim 12, wherein the plurality of nanostructures comprises at least one of ahyroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), chalcogenides, molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), and combinations thereof.
15. The method of claim 12, wherein the resin comprises at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, a carbohydrates, a polysaccharide, a carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), an acrylic resin, a silicone, a poly siloxane, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEG), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, hydrogels, acrylates, poly(sodium acrylate), a polyimide, poly(amidoamine) (PAMAMs), polyaniline, polysiloxane derivatives, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS metal compounds, MOFs, softeners, and combinations thereof. 16. The method of claim 2, further comprising adding an additive to at least one of the mixture containing a carbon fiber precursor, the thermoplastic material, the carbon-rich nanostructure, and combination thereof, wherein the additive comprises at least one of the thermoplastic material, a resin, a drug, a protein, an enzyme, a catalyst, a hydrogel, a vitamin, a softener agent, a metamaterial, a liposome, a dye, a nanostructured additive, a biomaterial, a macromolecule, a superstructure, BETS metal compound, an electrolyte, and combinations thereof.
17. The method of claim 16, wherein the additive comprises at least one of PEG, polyvinylpyrrolidone (PVP), chitosan, carbohydrates, polysaccharide, carbohydrate derivatives, polyacrylonitriles, polyacrylic acid (PAA), acrylic resins, silicones, poly siloxanes, polyurethanes, poly(vinyl alcohol) (PVA), polyamides (PA), polyethylene oxides (PEO), polyols, n-methylols, polyesters, polysaccharides, polyelectrolytes, a hydrogels, acrylates, poly(sodium acrylate), polyimides, a poly(amidoamine) (PAM AMs), a polyaniline, polysiloxane derivatives, proteins, their monomers, oligomers, co- or tri-polymers, dendrimers, cyclodextrin, amphiphilics, liposomes, macromolecules, superstructures, biomaterials, metamaterials, BETS, metal-organic frameworks (MOFs), softeners, a metal oxide, Silicon (Si), Boron (B), phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanotubes (CNTs), fullerene, graphene and graphene-based materials, graphene oxide (GO), a magnetic material, hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide
(SiC), Iron phosphorus trisulfide (FePSs), Strontium stannate (SrSnov). Tungsten ditelluride (WTe2), Potassium heptafluorotantalate (FLTaF?), Tungsten disulfide (WS2), Magnesium diboride (MgB2), Niobium disulfide (NbS2), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Lead (Pb), Iridium (Ir), Cobalt (Co), Nickel (Ni), Vanadium (V), tungsten (W), Tin (Sn), molybdenum (Mo), tellurium (Te), niobium (Nb), iron (Fe), palladium (Pd), strontium (Sr), an oxide of at least one of Cu, Zn, Fe, Mn, Ti, Mg, Mo, Si, chalcogenides, a salt comprising at least one of chalcogenides, Ag, Cu, Zn, Fe, V, Ni, Co, Ir, Pb, Mn, Au, Pt, Ti, W, Sn, Mo, Te, Nb, Pd, and Sr, and combinations thereof.
18. The method of claim 16, wherein the nanostructured additive comprises at least one of Silicon (Si), Boron (B), Phosphorus (P), clays, hydroxyapatite, layered double hydroxides (LDHs), phosphosilicates, MXenes, carbon nanostructures, nanotubes (CNTs), nanofibers (CNFs), fullerene, graphene and graphene -based materials, graphene oxide (GO), a magnetic material, metal-organic frameworks (MOFs), hexagonal boron nitride (hBN), chalcogenides, borophene, bismuth strontium calcium copper oxide (BSCCO), kagome lattices, bis(ethylenedithio)tetraselenafulvalene (BETS) metal compounds, Silicon carbide (SiC), Iron phosphorus trisulfide (FePSs), Strontium stannate (SrSnos), Tungsten ditelluride (WTei), Potassium heptafluorotantalate (BGTaE?), Tungsten disulfide (WS2), Magnesium diboride (MgB2), Niobium disulfide (NbS2), Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), Vanadium (V), Tungsten (W), at least one of a hyroxide, a salt, a composite, an oxide, a framework, and combinations thereof comprising at least one of Silver (Ag), Copper (Cu), Zinc (Zn), Titanium (Ti), Platinum (Pt), Gold (Au), Manganese (Mn), Tin (Sn), Iron (Fe), 88
Lead (Pb), Palladium (Pd), Strontium (Sr) Iridium (Ir), Cobalt (Co), Tellurium (Te), Nickel (Ni), molybdenum (Mo), Niobium (Nb), chalcogenides, Vanadium (V), Tungsten (W), and combinations thereof.
19. The method of claim 2, further comprising at least one of washing the carbon-rich nanostructure with at least one of an organic solvent, an aqueous solution, and combination thereof, washing the plurality of carbon-containing fibers with at least one of an organic solvent, an aqueous solution, and combination thereof, washing the nano structured network with at least one of an organic solvent, an aqueous solution, and combination thereof, purification at least one of the carbon-rich nanostructure, the plurality of carbon-containing fibers, the nanostructured network, and combinations thereof using at least one of an acid solution, a basic solution, an oxidant solution, an organic solution, and combination thereof, in-situ synthesis of a nano structured additive using at least one of a hydrothermal process, a solvothermal process, a chemical reduction/oxidation, irradiation, a thermal process, and combination thereof, eliminating a component before or after forming the nanostructured network using at least one of an organic solvent, an acid solution, a basic solution, an oxidant solution, water, and combination thereof, and combination thereof.
20. The method of claim 2, wherein the carbon-rich nanostructures comprises one of carbon, graphite, graphite/carbon, partially-carbon-rich materials, a carbon nanocomposite, a graphite nanocomposite, a graphite/carbon nanocomposite, a partially-carbon-rich nanocomposite, and combination thereof.
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