Attorney Docket No.: 072174-05701 ULTRAFAST FLASH JOULE HEATING SYNTHESIS METHODS AND SYSTEMS FOR PERFORMING SAME CROSS-REFERENCED TO RELATED PATENT APPLICATIONS [0001] The application claims priority to U.S. Patent Appl. Serial No. 63/585,465, to James Mitchell Tour, et al., entitled “Ultrafast Flash Joule Heating Synthesis Methods and Systems For Performing Same,” filed September 26, 2023, which patent application is commonly owned by the owner of the present invention and is incorporated herein in its entirety. [0002] The application is related to PCT Application No. PCT/US21/52030, entitled “Ultrafast Flash Joule Heating Synthesis Methods And Systems For Performing Same,” filed September 24, 2021, to James M. Tour, et al. (“Tour ’030 PCT Application”), which patent application is commonly owned by the owner of the present invention and is incorporated herein in its entirety. [0003] The application is related to PCT International Patent Appl. No. PCT/US23/67000, entitled “Flash Joule Heating For Production of 1D Carbon And/Or Boron Nitride Materials,” to J. M. Tour, et al., filed May 15, 2023, which patent application is commonly owned by the owner of the present invention and is incorporated herein in its entirety. TECHNICAL FIELD [0004] The present invention relates to ultrafast Joule heating synthesis methods and systems, and, more particularly, ultrafast flash Joule heating upcycling from fiber-reinforced plastics (such as waste fiber-reinforced plastic, glass fiber-reinforced plastic, carbon fiber-reinforced plastic, and/or quartz fiber-reinforced plastic or mixtures of plastic and glass more generally) and materials that include fiber-reinforced plastics (such as reinforced metal laminates including glass reinforced aluminum laminates and other glass reinforced metal laminates) to phase-controllable silicon carbide (SiC). Further embodiments relate to ultrafast Joule heating synthesis methods and systems to synthesize include SiC fibers/fibrils (such as SiC nanowires), SiC nanowires and SiC in polymer composites, and B
4C nanowires.
Attorney Docket No.: 072174-05701 GOVERNMENT INTEREST [0005] This invention was made with government support under Grant No. FA9550-22-1- 0526, awarded by the United States Air Force Office of Scientific Research, and Grant No. ERDC W912HZ-21-2-0050 and W912HZ-24-2-0027, awarded by the United States Engineer Research and Development Center for the United States Army Corp of Engineers. The United States government has certain rights in the invention. BACKGROUND [0006] Fiber-reinforced plastic (FRP), with the structure of reinforce fibers embedded into a polymer matrix, is a robust composite material. [Goncalves 2022; Cunliffe 2003]. Glass fiber- reinforced plastic (GFRP) accounts for 95% of all FRP with merits of light weight, chemical stability, and excellent mechanical properties [Cui 2020; Cheng 2022; Sena-Cruz 2020; Sathishkumar 2014], and has been widely used in various platforms ranging from the automotive and aerospace industries to wind turbine blades and sports equipment. It has been estimated that global annual demand for GFRP will exceed 6 million tonnes by 2030, with an annual growth rate of ~10%. [Xue 2021]. However, the life span of the GFRP is only 10-40 years [Karuppannan Gopalraj 2020; Jensen 2018], leading to the disposal of millions of tonnes of GFRP. [0007] Currently, more than half of the waste GFRP is directly landfilled, since it is regarded as the cheapest and simplest disposal route. [Krauklis 2021; Thomason 2016]. GFRP typically includes a thermosetting plastic composite containing glass fibers, and the plastic matrix is difficult to degrade through natural decomposition or microbiological treatment. [Zheng 2005; Bahl 2021]. Incineration [Jacob 2011; Naqvi 2018] and solvolysis methods [Liu 2006; Ahrens 2023] enable the reuse of the glass fiber by combusting the polymer matrix or dissolving it using chemical reagents, such as highly concentrated acids or alkalis, and then the glass fiber is remolded.
Attorney Docket No.: 072174-05701 [0008] However, the polymer removal process often leads to additional greenhouse gas (GHG) emissions or solvent consumption, resulting in secondary waste streams. Upcycling of GFRP into functional materials, like silicon carbide (SiC), represents a promising route. SiC is a high- performance reinforcement and semiconducting material with high mechanical strength, high- temperature stability, high thermal conductivity and a wide bandgap. [Wang 2023]. Conventionally, SiC synthesis methods mainly include chemical vapor deposition (CVD) [Booker 2016; Clavaguera-Mora 1997], physical vapor transport (PVT) [Yan 2014; Herro 2003], and Acheson carbothermic reduction (ACR) [Shin 2005; Guo 2013]. The CVD and PVT methods often require a specific temperature gradient and a large supply of carrier gas, and expensive gaseous silicon and carbon precursors, such as silane or methane. [Booker 2016; Yan 2014]. The precursors are more versatile for the SiC synthesis by the ACR process, including charcoal, biomass or silica gel [Shin 2005; Guo 2013]. However, it requires annealing for hours or even days at high temperature (>1500 °C) to complete the reaction [Shin 2005; Guo 2013], leading to high energy consumption. The waste GFRP contains both Si and C, which have the potential to be both Si and C sources for SiC synthesis. [0009] Recently, direct electrical heating has emerged as a scalable and efficient method for materials synthesis [Jiang 2021; Cheng 2022; Liu 2020; Zhu 2023] and waste management [Wyss 2023; Yu 2023] without additional usage of solvent and catalyst. With the electric pulse input, the sample can reach an ultrahigh temperature of > 3000 K with a rapid heating (~10
4 °C s
-1) and cooling rates (~10
3 °C s
-1), which are inaccessible by traditional furnace heating. At such a high temperature, carbon-containing waste can be effectively converted to crystalline graphene [Jia 2022; Luong 2020] and heavy metals can be removed [Deng I 2023; Deng II 2023]. [0010] Accordingly, the need remains to develop methods for recycling fiber-reinforced plastic particularly once these reach their end-of-life. The need also remains to reduce/eliminate
Attorney Docket No.: 072174-05701 undesirable waste of resources and environmental contamination resulting currently by landfilling and incineration, which are the major disposal methods of fiber-reinforced plastic. SUMMARY OF THE INVENTION [0011] The present invention relates to ultrafast Joule heating synthesis methods and systems, and, more particularly, ultrafast flash Joule heating upcycling from fiber-reinforced plastics (such as waste fiber-reinforced plastic, glass fiber-reinforced plastic, carbon fiber-reinforced plastic, and/or quartz fiber-reinforced plastic, or more generally mixtures of plastics with glass) and materials that include fiber-reinforced plastics (such as reinforced metal laminates including glass reinforced aluminum laminates and other glass reinforced metal laminates) to phase-controllable silicon carbide (SiC). Further embodiments relate to ultrafast Joule heating synthesis methods and systems to synthesize include SiC fibers/fibrils (such as SiC nanowires), SiC nanowires and SiC in polymer composites, and B
4C nanowires. [0012] Direct electrical heating has emerged as a time- and energy-efficient method for materials synthesis [Yao 2018; Wang 2020; Cheng 2021; Chen 2016; Zhu 2023] and waste management [Wyss I 2023; Liu 2022; Dong 2023; Luo 2023; Jia 2022]. Applicant has previously applied flash Joule heating methods to the conversion of waste plastic into turbostratic graphene [Wyss II 2023; Luong 2020] and the valorization of solid wastes [Deng 2021; Deng II 2022; Deng 2023; Chen 2023]. It has been discovered that direct electric heating provides a rapid and energy-efficient alternative to upcycle GFRP into SiC, which can potentially boost circular economy and clean production. When carbothermic reduction occurs during the flash Joule heating process, the process can be referred to as a flash carbothermic reduction process. [0013] In general, embodiments of the present invention include a solvent-free and energy- efficient flash upcycling method to convert the mixture of milled glass fiber-reinforced plastic and carbon fiber-reinforced plastic into SiC powders within seconds and in yields of >90%. By
Attorney Docket No.: 072174-05701 modulating input pulse voltages and flash times, SiC with two different phases, 3C-SiC and 6H-SiC, can be selectively synthesized, each with a phase purity of 90-99%. The SiC powders are further used as the anode material for lithium-ion batteries, which yields a phase-dependent performance. The 3C-SiC anode exhibits superior reversible capacity and rate performance over the 6H-SiC anode, while both show excellent cycling stability. Life cycle assessment reveals the flash upcycling process exhibits significant reductions in energy demand, greenhouse gas emission and water consumption, when compared with solvolysis and incineration processes. Therefore, the flash process enables the effective, economic and environmentally friendly repurpose of waste fiber-reinforced plastics into value-added SiC materials. [Deng I 2022; Tour ’030 PCT Application]. [0014] In general, in one embodiment, the invention features a method of synthesizing a material. The method includes forming a mixture including a source or sources of the elements and a catalyst. The method further includes performing a flash Joule heating process utilizing the mixture to form a structure selected from the group consisting of fibers, fibrils, whiskers, nanotubes, and 1-dimensional structures. The flash Joule heating process includes applying voltage across the mixture for one of one or more periods of flash times. The product includes a material selected from the group consisting of carbide, boride, nitride, boronitride, borocarbide, BNC, oxynitride, carbonitride, oxide, dioxide, sulfide, disulfide, selenide, diselenide, telluride, ditelluride, phosphide, oxycarbide, oxyboride, oxynitridecarbide, oxyboridenitride, oxycarbideboride, OBNC, arsenide, and antimonide materials. [0015] Implementations of the invention can include one or more of the following features: [0016] The structure can include an inorganic compound. The inorganic compound can include a first element or compound selected from the group consisting of boron, silicon, carbon, aluminum, germanium, tin, gallium, indium, lead, copper, zinc, cadmium, magnesium, titanium, cobalt, tungsten, vanadium, hafnium, niobium, molybdenum, zirconium, tantalum,
Attorney Docket No.: 072174-05701 and combinations thereof. The inorganic compound can include a second element or compound selected from the group consisting of C, B, O, N, S, P, As, Sb, Se, Te, Si, Ge, Sn, I, and combinations thereof [0017] The inorganic compound can be selected from the group consisting of transition metal dichalcogenides, mixed chalcogen transition metal dichalcogenides, transition metal dichalcogenides containing more than one type of transition metal, III-V compound, II-VI compound, I-VII compound, group IV compound, group IV element, IV-VI compound, and mixtures thereof. [0018] The catalyst can be an element, salt, polyoxometalate, or organometallic compound that comprises a main group metal, a transition metal, a lanthanide, or an actinide. [0019] The mixture can further include a growth promotor or modifier that includes an element selected from the group consisting of F, S, Se, Cl, Br, I, P, O, or N is added to the mixture to enhance the growth of one-dimensional structures. [0020] In general, in another embodiment, the invention features a method of synthesizing silicon carbide fibers or fibrils. The method includes forming a mixture including a silicon source, a carbon source, and a catalyst. The method further includes performing a flash Joule heating process utilizing the mixture to form silicon carbide fibers or fibrils. The flash Joule heating process includes applying voltage across the mixture for one of one or more periods of flash times. [0021] Implementations of the invention can include one or more of the following features: [0022] The silicon or carbon source can be selected from the group consisting of powders, fibers, silicone, sodium silicate, iron silicate, silicates, aluminosilicates, silicon oxides, silicon dioxide, fiber-reinforced plastic particles, silicon wafer, and waste solar panel. [0023] The silicon or carbon source can be fiber-reinforced plastic particles derived from the group consisting of fiber-reinforced plastic, reinforced metal laminate, and combinations
Attorney Docket No.: 072174-05701 thereof. [0024] The silicon or carbon source can be fiber selected from a group consisting of waste fiber, glass fiber, carbon fiber plastic, quartz fiber, basalt fiber, rockwool, polymer fiber, plant fiber, asbestos, rock fibers, mineral fibers, and combinations thereof. [0025] The catalyst can be a metal catalyst. [0026] The metal catalyst can include a metal selected from the group consisting of iron, nickel, cobalt, and manganese. [0027] The metal catalyst can be made from a metal selected from the group consisting of iron, nickel, cobalt, and manganese. [0028] The metal catalyst can be a metal acetylacetonate, metal salts, metal chlorides, metal nitrites, nickelocene, ferrocene, metal oxides, metal acetates, metal fluorides, organometallic compounds, polyoxometalates, and combinations thereof. [0029] The metal catalyst can be selected from the group consisting of Fe(acac)
3, Ni(acac)
2, Co(acac)
2, ferrocene, iron nitrite, iron nitrate, nickel nitrite, nickel nitrate, cobalt nitrite, cobalt nitrate, manganese nitrite, manganese nitrate, manganese acetylacetonate, manganese acetate, iron acetate, nickel acetate, cobalt acetate, iron fluoride, nickel fluoride, cobalt fluoride, manganese fluoride, and combinations thereof. [0030] In general, in another embodiment, the invention features a method of synthesizing B
4C nanowires. The method includes forming a mixture comprising a boron source, a carbon source, and a catalyst. The method further includes performing a flash Joule heating process utilizing the mixture to form the B
4C nanowires. The flash Joule heating process includes applying a voltage across the mixture for one of one or more periods of flash times. [0031] Implementations of the invention can include one or more of the following features: [0032] The boron source can be selected from the group consisting of boric acid, boric oxide, borax, metal borates, boranes, carboranes, and combinations thereof.
Attorney Docket No.: 072174-05701 [0033] The carbon source can be selected from the group consisting of carbon black, coke, silicone, carboranes, graphite, graphene, carbon fibers, carbon nanotubes, biochar, and combinations thereof. [0034] The catalyst can include a metal catalysts selected from the group consisting of metal salts, metal powders, polyoxometalates, organometallic compounds, and combinations thereof. [0035] The metal salt can include a metal element selected from the group consisting of Fe, Co, Ni, and Mn. [0036] The metal salt can include a metal element selected from the group consisting of Mo, Cr, V, Ru, Rh, and Nb. [0037] The metal salt can be selected from the group consisting of iron chloride (FeCl
3), ferrocene, iron nitrite, iron(III) acetylacetonate (Fe(acac)
3), nickel(II) acetylacetonate (Ni(acac)
2), cobalt(II) acetylacetonate (Co(acac)
2), iron nitrate, nickelocene, iron acetate, nickel acetate, cobalt acetate, manganese acetate, manganese acetylacetonate, manganese chloride, manganous chloride, iron fluoride, cobalt fluoride, nickel fluoride, manganese fluoride, and combinations thereof. [0038] The flash Joule heating process can be performing utilizing a flash power source selected from the group consisting of charged capacitors, commercial arc welders, direct current power supply, and combinations thereof. [0039] The output of the flash power source can be a current pulse or a continuous current. [0040] The B
4C nanowires can have diameters between 2 nm and 1 μm. The B
4C nanowires can have lengths between 0.1 μm and 5000 μm. [0041] In general, in another embodiment, the invention features a battery that includes an electrode including silicon carbide particles produced from fiber-reinforced plastic utilizing the method of any of the above-described methods. [0042] Implementations of the invention can include one or more of the following features:
Attorney Docket No.: 072174-05701 [0043] The battery can be a lithium-ion battery. [0044] The silicon carbide particles can be used in the anode material of an anode of the battery. [0045] In general, in another embodiment, the invention features a method. The method includes producing silicon carbide particles from fiber-reinforced plastic utilizing any of the above-described methods. The method further includes utilizing the silicon carbide particles for an application selected from the group consisting of composite reinforcement, semiconductors, photocatalysis, and electrocatalysis. [0046] In general, in another embodiment, the invention features a method of synthesizing silicon carbide fibers or fibrils. The method includes forming a mixture including fibers or fiber-reinforced plastic particles and a catalyst. The method further includes performing a flash Joule heating process utilizing the mixture to form silicon carbide fibers or fibrils. The flash Joule heating process includes applying voltage across the mixture for one of one or more periods of flash times. [0047] Implementations of the invention can include one or more of the following features: [0048] The fiber-reinforced plastic particles can be formed from a material selected from the group consisting of fiber-reinforced plastic, reinforced metal laminate, and combinations thereof. [0049] The fiber-reinforced plastic particles can be formed from fiber-reinforced plastic. [0050] The step of forming the fiber-reinforced plastic particles includes milling the fiber- reinforced plastic. [0051] The fiber-reinforced plastic can be selected from a group consisting of waste fiber- reinforced plastic, glass fiber-reinforced plastic, carbon fiber-reinforced plastic, quartz fiber- reinforced plastic, mixtures of plastic and glass, and combinations thereof. [0052] The fiber-reinforced plastic particles can be formed from reinforced metal laminate. [0053] The catalyst can be a metal catalyst.
Attorney Docket No.: 072174-05701 [0054] The metal catalyst can include a metal selected from the group consisting of iron, nickel, cobalt, and manganese. [0055] The metal catalyst can be made from a metal selected from the group consisting of iron, nickel, cobalt, and manganese. [0056] The metal catalyst can be selected from the group consisting of metal acetylacetonate, metal salts, metal chlorides, metal nitrites, nickelocene, ferrocene, metal oxides, metal acetates, metal fluorides, organometallic compounds, polyoxometalates, and combinations thereof. [0057] The metal catalyst can be selected from the group consisting of Fe(acac)
3, Ni(acac)
2, Co(acac)
2, ferrocene, iron nitrite, iron nitrate, nickel nitrite, nickel nitrate, cobalt nitrite, cobalt nitrate, manganese nitrite, manganese nitrate, manganese acetylacetonate, manganese acetate, iron acetate, nickel acetate, cobalt acetate, iron fluoride, nickel fluoride, cobalt fluoride, manganese fluoride, and combinations thereof. [0058] The silicon carbide fibers or fibrils can be silicon carbide nanowires. [0059] In general, in another embodiment, the invention features an apparatus. The apparatus includes a vessel operable for receiving a mixture including fiber-reinforced plastic particles and a metal catalyst. The apparatus further includes electrodes that are operable for applying a voltage pulse across the mixture for one of one or more periods of flash times to subject the mixture to a flash Joule heating process. The flash Joule heating process upon the mixture results in the conversion of the mixture to silicon carbide fibers or fibrils. [0060] Implementations of the invention can include one or more of the following features: [0061] The apparatus can be further operable to perform any of the above-described methods. [0062] In general, in another embodiment, the invention features a method of fabricating a polymer composite. The method includes forming a mixture of fiber-reinforced plastic particles. The method further includes performing a flash Joule heating process utilizing the mixture to form a silicon carbide material. The flash Joule heating process includes applying a
Attorney Docket No.: 072174-05701 voltage across the mixture for one of one or more periods of flash times. The silicon carbide material is selected from the group consisting of silicon carbide particles, silicon carbide fibers, and silicon carbide fibrils. The method further includes loading between 0.5 wt% and 5 wt% of the silicon carbide material into a liquid polymer matrix. The method further includes curing the liquid polymer matrix to form the polymer composite. [0063] Implementations of the invention can include one or more of the following features: [0064] The silicon carbide material can be SiC. The polymer composite can be a SiC-polymer composite. [0065] The silicon carbide material can be silicon carbide fibers or fibrils. The polymer composite can be a SiC fiber or fibril-polymer composite. [0066] The silicon carbide material can be silicon carbon nanowires. The polymer composite can be a SiC nanowire-polymer composite. [0067] The mixture including the fiber-reinforced plastic particles can further include a first catalyst. [0068] The step of curing can include mixing a catalyst/hardener to the liquid polymer matrix loaded with the silicon carbide material. [0069] The liquid polymer matrix can be selected from the group consisting of a vinyl ester, epoxy, polyurethane, polyaspartic, bismaleimide, pthalonitrile, cyanate ester, polyester, bismaleimide-triazine, acrylic, PCTG, PETG, PLA, copolyesters, PCTA, PEKK, PAEK, polycarbonate, polyester, polybenzoxazole, polyimide, aramid, polysulfone, PTFE, PVDF, HFP, PVDF/HFP, benzoxazine, polyoxazole, PEEK, PEK, PAI, PPSU, PPS, PSU, PES, PA, PC, silicone, silicon carbide, phenolic, graphite, carbon fiber, boron nitride, boron nitride fiber, boron carbide, or carbon/carbon composite matrix. [0070] The step of curing can include mixing a curing agent or a crosslinking agent to the liquid polymer matrix loaded with the silicon carbide material.The curing agent or the
Attorney Docket No.: 072174-05701 crosslinking agent can be methyl ethyl ketone peroxide. [0071] The step of curing can include heating the liquid polymer matrix loaded with the silicon carbide material. [0072] In general, in another embodiment, the invention features a method of synthesizing silicon carbide particles. The method includes forming a mixture including fiber-reinforced plastic particles. The method further includes performing a flash joule heating process utilizing the mixture to form silicon carbide particles. The flash joule heating process includes applying voltage across the mixture for one of one or more periods of flash times. [0073] Implementations of the invention can include one or more of the following features: [0074] The step of forming the mixture can include forming the fiber-reinforced plastic particles from a material selected from the group consisting of fiber-reinforced plastic, reinforced metal laminate, and combinations thereof. [0075] The step of forming the mixture can include forming the fiber-reinforced plastic particles from fiber-reinforced plastic. [0076] The step of forming the mixture can include milling the fiber-reinforced plastic to form the fiber-reinforced plastic particles. [0077] The fiber-reinforced plastic can be selected from a group consisting of waste fiber- reinforced plastic, glass fiber-reinforced plastic, carbon fiber-reinforced plastic, quartz fiber- reinforced plastic, plastic mixed with glass, carbon mixed with glass, plastic mixed with silicon dioxide, carbon mixed with silicon dioxide, and combinations thereof. [0078] The step of forming the mixture can include forming the fiber-reinforced plastic particles from reinforced metal laminate. [0079] The step of forming the mixture can include milling the reinforced metal laminate to form the fiber-reinforced plastic particles. [0080] The step of performing the flash Joule heating process can form the silicon carbide
Attorney Docket No.: 072174-05701 particles and metal carbide particles. [0081] The reinforced metal laminate can be glass reinforced metal laminate. [0082] The glass reinforced metal laminate can be glass reinforced aluminum laminate. [0083] The step of performing the flash Joule heating process can form the silicon carbide particles and aluminum carbide particles. [0084] The flash Joule heating process can be performed within 10 seconds and can have a yield of at least 90 wt%. [0085] The applying of the voltages across the mixture can be controlled by controlling modulating input pulse voltage and by controlling time of the one or more periods of flash times. [0086] Controlling the applying of the voltages across the mixture can control the purity of the phase of the silicon carbide particles produced by flash Joule heating process. [0087] The method can produce silicon carbide particles comprising phases of 3C-SiC and 6H- SiC. [0088] The method can produce silicon carbide particles having a phase purity of 3C-SiC of at least 90 wt%. [0089] The method can produce silicon carbide particles having a phase purity of 3C-SiC of between 90 wt% and 99 wt%. [0090] The method can produce silicon carbide particles having a phase purity of 6H-SiC of at least 90 wt%. [0091] The method can produce silicon carbide particles having a phase purity of 6H-SiC of between 90 wt% and 99 wt%. [0092] The mixture can be stirred in a reactor with electrodes while performing the flash Joule heating process. [0093] In general, in another embodiment, the invention features an apparatus. The apparatus
Attorney Docket No.: 072174-05701 includes a vessel operable for receiving a mixture including fiber-reinforced plastic particles. The apparatus further includes electrodes that are operable for applying a voltage pulse across the across the mixture for one of one or more periods of flash times to subject the mixture to a flash Joule heating process. The flash Joule heating process upon the mixture results in the conversion of the fiber-reinforced plastic particles to silicon carbide particles. [0094] Implementations of the invention can include one or more of the following features: [0095] The apparatus can be further operable to perform any of the above-described methods. [0096] In general, in another embodiment, the invention features a method. The method includes producing silicon carbide particles from fiber-reinforced plastic utilizing any of the above-described methods. The method further includes utilizing the silicon carbide particles as the anode material of a battery. [0097] Implementations of the invention can include one or more of the following features: [0098] The battery can be a lithium-ion battery. [0099] The use of the silicon carbide particles in the battery can yield a phase-dependent performance. [0100] In general, in another embodiment, the invention features a battery made by the process of any of the above-described methods. BRIEF DESCRIPTION OF THE DRAWINGS [0101] FIGS.1A-1D show upcycling FRP to silicon carbide by flash carbothermic reduction. FIG.1A is a schematic of the FCR process for FRP upcycling. Insets in step 1 of FIG.1A are pictures of waste GFRP disassembled from a Dewar bottle and chopped carbon fiber-reinforced plastic (CFRP). Insets in step 2 of FIG.1A are pictures of the sample in the quartz tube before (i) and during (ii) the FCR reaction. FIG.1B is current curve with an input voltage of 150 V and duration of 1 s during the FCR process. FIG.1C is real-time temperature curve with the input voltage of 100 V and 150 V recorded by an infrared thermometer. The temperature
Attorney Docket No.: 072174-05701 detection range of the thermometer is 1000 to 3000 °C. FIG. 1D shows the relationship between the Gibbs free energy change (ΔG) and temperature with different ratios between SiO
2 and carbon. The horizontal dashed line denotes the ΔG at zero. [0102] FIGS. 2A-2K show phase controllable synthesis of SiC. FIG. 2A shows crystal structures of 3C-SiC (left) and 6H-SiC (right). FIG.2B shows Si 2p core-level XPS spectra of 3C-SiC (top) and 6H-SiC (bottom). The small peak of Si-O (~103 eV) may be ascribed to the slight oxidation when exposed to air. FIG. 2C shows XRD patterns of purified 3C-SiC synthesized at a voltage of 100 V and single flash (top) and purified 6H-SiC synthesized at a voltage of 150 V and 10 flashes (bottom). The PDF reference cards for each are 3C-SiC, 01- 073-1708; 6H-SiC, 01-075-8314. FIG.2D shows representative Raman spectra of purified 3C- SiC (top) and 6H-SiC (bottom). TO is the transverse optical mode. LO is the longitudinal optical mode. TA is the transverse acoustic mode. LA is the longitudinal acoustic mode. FIG. 2E shows Tauc plots of 3C-SiC (top) and 6H-SiC (bottom). FIG.2F is an HRTEM image of 3C-SiC. FIG.2G is a zoom-in HRTEM image of 3C-SiC. FIG.2H is an SAED pattern of 3C- SiC. FIG.2I is an HRTEM image 6H-SiC. FIG.2J is a zoom-in HRTEM image of 6H-SiC. FIG.2K is an SAED pattern of 6H-SiC. [0103] FIGS.3A-3F show mechanism of SiC phase transformation. FIG.3A shows SiC phase mass ratios versus the input voltage under the one flash pulse. FIG.3B shows SiC phase mass ratios versus the flash pulses under the input voltage of 150 V. The error bars in FIGS.3A-3B are standard deviation (SD) of SiC phase ratio in 3 parallel experiments (n=3). Data are presented as means ± SD. FIG.3C shows EPR spectra of 3C-SiC and 6H-SiC. FIG.3D shows temperature-vapor pressure relationships for silicon and carbon. FIG. 3E shows formation energy of 3C-SiC and 6H-SiC with different content of silicon vacancy. FIG. 3F shows calculated crystal structures of 3C-SiC (top) and 6H-SiC (bottom) with different atomic content of Si vacancy. The dashed circles denote the silicon vacancies.
Attorney Docket No.: 072174-05701 [0104] FIGS. 4A-4I show phase dependent lithium-ion battery (LIB) performance of SiC anode. FIG.4A shows charge-discharge profiles of 3C-SiC anode at different cycles. FIG.4B shows charge-discharge profiles of 6H-SiC anode at different cycles. FIG.4C shows cycling stability of 3C-SiC anode and 6H-SiC anode at 0.2 C. FIG.4D shows rate capacity of 3C-SiC anode and 6H-SiC anode. FIG.4E shows CV curves of 3C-SiC anode at different scan rates. FIG. 4F shows CV curves of 6H-SiC anode at different scan rates. FIG. 4G shows Nyquist plots of 3C-SiC anode and 6H-SiC anode before cycling. FIG. 4H shows the Li
+ diffusion coefficient of 3C-SiC anode and 6H-SiC anode during the charging process. FIG. 4I shows cycling stability of the full-cell LIB with 3C-SiC anode and NMC622 cathode at 0.2 C. [0105] FIG.5 shows a schematic of a system for continuous flash upcycling FRPs. [0106] FIGS.6A-6E show LCA for the FRP recycling. FIG.6A shows materials flow analysis of solvolysis, incineration, and FCR processes. FIG.6B shows comprehensive comparisons of the solvolysis, incineration and FCR process. FIG.6C shows comparison of cumulative energy demand. FIG.6D shows comparison of cumulative GHG emission. FIG.6E shows Techno- economic comparison. The materials mass flow is normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) to produce 1 tonne of SiC during FCR process. [0107] FIGS.7A-7B show protocols for SiC synthesis from, respectively, (FIG.7A) non-Fe- containing Si sources and (FIG.7B) Fe-containing Si sources. [0108] FIGS.8A-8E show SiC NW yield with different flash times. FIGS.8A-8D show flash times, respectively, of (FIG.8A) once; (FIG.8B) 3 times; (FIG.8C) 5 times; and (FIG.8D) 10 times. FIG. 8E shows statistical results of NW yield and diameters. The error bar in e represents the standard deviations, where N = 10. [0109] FIGS. 9A-9E show SEM images of SiC NW synthesized using different catalysts, respectively: (FIG. 9A) FeCl
3; (FIG. 9B) ferrocene; (FIG. 9C) Fe(acac)
3; (FIG. 9D) Ni(acac)2; and (FIG.9E) Co(acac)2.
Attorney Docket No.: 072174-05701 [0110] FIG. 9F shows SiC NW yield with the different catalysts used for the SiC NW synthesized in FIGS. 9A-9E, with the catalyst loading contents of 1 wt%. The error bar represents the standard deviations, where N = 10. [0111] FIGS.10A-10E show SiC NW diameter and nanowire yields using different contents of catalysts. FIGS.10A-10D show contents of, respectively: (FIG.10A) 0.1 wt%; (FIG.10B) 0.5 wt%; (FIG.10C) 1 wt%; and (FIG.10D) 2 wt%. FIG.10E shows statistical results of NW yield and diameters. The error bar in e represents the standard deviations, where N = 10. [0112] FIGS.11A-11C show SEM images of the SiC NW synthesized from GFRP, desert sand, and diatomite, respectively. [0113] FIG. 12A-12E show SiC NW synthesized from fire glass with different additives. FIGS.12A-12D show: (FIG.12A) No additive; (FIG.12B) 1 wt% PTFE; (FIG.12C) 1 wt% NaF; and (FIG.12D) 1 wt% PVC. FIG.12E shows NW yield using different additives. The error bar in e represents the standard deviations, where N = 10. [0114] FIG 12F shows SiC NW yield from fire glass with different amounts of PTFE additives. The error bar represents the standard deviations, where N = 10. [0115] FIG. 13A-13B show SEM images of SiC NW synthesized from CFA, respectively (FIG.13A) without PTFE and (FIG.13B) with 1 wt% of PTFE. [0116] FIG. 14A-14B show SEM images of scale-up synthesis of, respectively (FIG. 14A) fire glass and (FIG.14B) sand/ferrocene [0117] FIG. 15 shows characterization of microscale mechanical properties of Young’s modulus and hardness. [0118] FIG.16 shows characterization of microscale mechanical properties of Tensile testing of SiCNW in VER composites. [0119] FIG.17 shows stress vs strain curves comparing the neat VER to 1 wt%. [0120] FIG.18 shows stress vs strain curves for SiC particles in VER.
Attorney Docket No.: 072174-05701 [0121] FIG. 19 shows a schematic of the thermal conductivity testing set up showing the temperature of heat flow vs. the distance along the z-axis of each thermocouple from the sample. [0122] FIG.20 shows thermal conductivity testing of SiC and SiCNW in VER composites. [0123] FIG.21 shows nanowire yield versus heating time. [0124] FIG.22 shows B
4C nanowire yield using different catalysts. [0125] FIGS.23A-23D show SEM images of B
4C nanowires with different ferrocene contents of (a) 0.1 wt%, (b) 0.5 wt%, (c) 1.0 wt%, and (d) 2.5 wt%, respectively. [0126] FIGS. 24A-24D show statistics of B
4C nanowire diameters with different ferrocene contents of (a) 0.1 wt%, (b) 0.5 wt%, (c) 1.0 wt%, and (d) 2.5 wt%, respectively. [0127] FIG.25 shows nanowire yield versus catalyst loading content. [0128] FIG.26A-26C show characterizations of B
4C nanowires. FIG.26A is XRD patterns. Gr denotes graphene. PDF card number: B
4C, 00-006-0555. Gr, 00-056-0160. FIG. 26B is Raman spectra. FIG.26C is B 1s XPS spectra. [0129] FIG. 27A-27C show B
4C nanowires synthesis using B powder as the boron sources. FIG. 27A is XRD patterns. Gr denotes graphene. PDF card number: B
4C, 00-006-0555. Gr, 00-056-0160. FIG.27B is XPS spectra. FIG.27C is an SEM image. DETAILED DESCRIPTION [0130] The present invention relates to ultrafast Joule heating synthesis methods and systems, and, more particularly, ultrafast flash Joule heating upcycling from fiber-reinforced plastics (such as waste fiber-reinforced plastic, glass fiber-reinforced plastic, carbon fiber-reinforced plastic, and/or quartz fiber-reinforced plastic, or plastic plus glass more generally) and materials that include fiber-reinforced plastics (such as reinforced metal laminates including glass reinforced aluminum laminates and other glass reinforced metal laminates) to phase- controllable silicon carbide (SiC). Further embodiments relate to ultrafast Joule heating
Attorney Docket No.: 072174-05701 synthesis methods and systems to synthesize include SiC fibers/fibrils (such as SiC nanowires), SiC nanowires and SiC in polymer composites, and B
4C nanowires. [0131] A flash carbothermic reduction (FCR) upcycling method has been discovered that achieves rapid and energy-efficient upcycling of waste FPR into value-added SiC materials in 1 to 10 s. By modulating flash parameters, greater than 90% phase-purity 3C-SiC and 6H-SiC can be selectively synthesized. When using SiC as the lithium-ion battery (LIB) anode material, its phase-dependent performance was discovered, where the 3C-SiC anode exhibits superior capacity and rate performance compared with that of the 6H-SiC anode. With positive attributes of low energy consumption, low GHG emission, solvent- and water-free reaction, and scalability, the FCR method is extended to upcycle multiple silicon-containing wastes, including glass. In addition, the phase-controllable and easily scaled SiC synthesis offer opportunities in wider-range applications beyond batteries, such as composite reinforcement, semiconductors, photocatalysis and electrocatalysis. [0132] Embodiments include a flash carbothermic reduction (FCR) method to upcycle GFRP into SiC. (Aluminum carbide formation is possible if the feedstock includes aluminum, such as feedstock that includes glass reinforced aluminum laminate). During FCR process, an electric pulse brings the pre-milled FRPs to a high temperature of 1600 – 2900 °C. Silicon dioxide in GFRP is carbothermically reduced to SiC within seconds. By modulating operating parameters, SiC can be selectively synthesized with two different phases, as either the 3C or 6H phase. The as-fabricated SiC was further used as the anode material for lithium-ion batteries (LIBs) and its phase-dependent performance was explored. Benefitting from the rapid reaction process, ultrafast heating, and cooling rates, the FCR process exhibits a significant reduction of energy consumption, GHG emission and solvent consumption, comparing to traditional GFRP recycling methods. Thus, it provides a viable and sustainable strategy to upcycle end- of-life FRPs into value-added materials with low cost and environmental impact.
Attorney Docket No.: 072174-05701 Ultrafast Upcycling Waste FRP By Flash Carbothermic Reduction [0133] Before the FCR process, the waste GFRP and CFRP were ground and milled into micrometer-sized powders. FIG. 1A, Step 1 (milling and mixing 101). The milled GFRP powder consisted of 63 wt% amorphous SiO
2 and 37 wt% polymer coating. The milled CFRP powder, mainly composed of low crystalline and defective carbon, maintained a comparable conductivity with the initial CFRP and was thus suitable to serve as conductive additive for the FCR process. [0134] In the FCR process, the mixture of the GFRP and CFRP was slightly compressed inside a quartz tube with two graphite electrodes on each side, which were connected to the external capacitor bank. FIG.1A, Step 2 (flash carbothermic reduction 102). The CFRP served as both the conductive additive and the carbothermic reduction agent. During the flash process, the current pulse passed through the sample with a high-voltage input, bringing the sample to a high temperature within milliseconds. Typically, with the GFRP and CFRP mass ratio of 2:1, the sample resistance was ~1.5 Ω. See TABLE I. TABLE I

Note: The input mass is the total mass of GFRP and CFRP powders. [0135] With the input voltage of 150 V, the maximum current passing through the sample
Attorney Docket No.: 072174-05701 reached ~350 A within the discharging time of 1 s. FIG.1B. The sample temperature profile was measured using an infrared thermometer, where the peak temperature was recorded to be ~2900 °C with an ultrafast heating (~10
4 °C s
-1) and cooling rate (~10
3 °C s
-1) under the input voltage of 150 V. FIG.1C (with plots 121-122 for 150 V and 100 V, respectively). At such a high temperature, SiO
2 in GFRP can be carbothermically reduced into SiC and the excess carbon would be converted into flash graphene. [Feldman 1968]. [0136] To optimize the reaction conditions, thermodynamic analysis of carbothermic reduction of SiO
2 was conducted. According to the plot of Gibbs free energy change (ΔG) vs. temperature, the increase of carbon/SiO
2 ratio can effectively decrease the reaction temperature from ~2450 °C to ~1600 °C. FIG.1D (plots 131-132 for SiO
2 + 2C and SiO
2 + 3C, respectively). Consequently, the carbon was excessively supplied during FCR process to ensure the complete conversion from SiO
2 to SiC. By modulating the flash input voltage from 80 to 150 V, the flash peak temperature can be tailored in the range of 1600 – 2900 °C, which meets the temperature requirement for SiC synthesis. [0137] During the FCR process, CO was identified as the main gaseous product with a small quantity of CO
2 and trace amounts of organic compounds, such as acetone, hexane, benzene and toluene, according to the gas chromatography-mass spectra. With the increase of the input GFRP/CFRP mass ratio, the CO/CO
2 mole ratio in the FCR-evolved gas decreased, which was consistent with FIG. 1D. The input GFRP/CFRP mass ratio was also related to sample conductivities, where a certain amount of CFRP was required to ensure suitable conductivity of the sample for flash reaction. Specifically, the input GFRP/CFRP mass ratio can be modulated from 0.25 to 3, and the obtained SiC contents in the flash products can be tailored from 7.6 wt% to 85 wt%, correspondingly. Phase-Controlled Synthesis Of SiC [0138] The structure of SiC varies depending on the arrangement of silicon and carbon atoms,
Attorney Docket No.: 072174-05701 which significantly affects its properties and performance in applications. [Shen 2020]. For example, 3C-SiC has a smaller bandgap, lower thermal conductivity, higher electron mobility, and higher hardness than 6H-SiC. [Persson 1999; Kong 2020]. Therefore, it is helpful to control the crystal phases of SiC for optimizing its properties and enabling its wide-range applications. However, the phase control of SiC is challenging, because the SiC phase can be influenced by multiple parameters including reaction precursors, pressure, and temperature. [Shimojo 2000; Yoo 1991]. [0139] The 3C-SiC has a cubic lattice structure with one silicon atom at the center and eight carbon atoms at the corners of each unit cell. FIG.2A, 3C-SiC structure 201. In contrast, the 6H-SiC has a hexagonal structure with carbon atoms located at the hexagonal lattice sites and silicon atoms occupying the interstitial sites between the carbon atoms. FIG. 2A, 6H-SiC structure 202. [Persson 1999; Kong 2020]. [0140] During the FCR process, it was discovered that by modulating flash voltages and flash times, phase-controllable 3C-SiC and 6H-SiC can be selectively synthesized. Specifically, phase-pure 3C-SiC was synthesized with an input voltage of 100 V by single flash, according to the X-ray diffraction (XRD) patterns. Further increasing voltage to 150 V and flashing for 10 times facilitated its phase transformation to 6H-SiC. Note that the diffraction peak at ~26° was ascribed to the graphene that formed inside the as-synthesized SiC powders. [Luong 2020]. [0141] In Raman spectra, in addition to the characteristic D (~1350 cm
-1), G (~1580 cm
-1) and 2D (~2680 cm
-1) bands of flash graphene, the representative TO (~790 cm
-1) and LO (~970 cm
-1) peaks were observed for both 3C-SiC and 6H-SiC. The additional TA (~505 cm
-1) and LA (~240 cm
-1) peaks of 6H-SiC are ascribed to its higher symmetric modes than 3C-SiC. [Feldman 1968]. [0142] To characterize the electronic structure of as-synthesized SiC, X-ray photoelectron spectroscopy (XPS) measurements were conducted. FIG.2B. Different from the existence of
Attorney Docket No.: 072174-05701 Si-O (~103 eV) and C-O (~288 eV) peaks for the GFRP precursors, both SiC phases show the distinct Si-C (~100 eV) and C-Si (~282 eV) peaks in the C 1s and Si 2p core-level spectra. FIG.2B. [Yu 2021]. [0143] To better compare the intrinsic properties of the two phases of SiC, the SiC samples were calcined at 700 °C in air to remove graphene. After calcination, SiC shows negligible weight loss (<0.5 wt%) in air when heating to 1000 °C, according to the TGA analysis. The XRD patterns of the purified SiC showed that phase purity of 3C-SiC and 6H-SiC can reach 99% and 90%, respectively. FIG.2C. The distinct TO and LO bands in Raman spectra (FIG. 2D), as well as Si-C bond vibration peak (~800 cm
-1) in the infrared spectra, confirmed the high purity of SiC without any graphene or SiO
2 signals [Yu 2021], proving that the air calcination is a simple and effective way to purify SiC. [0144] Furthermore, diffuse reflectance ultraviolet visible (UV-Vis) spectra demonstrate the different optical properties of these SiC powders, where 3C-SiC had a smaller bandgap (2.45 eV) compared with 6H-SiC (2.86 eV). FIG.2E. [0145] Morphology characterization by scanning electron microscopy (SEM) showed that 3C- SiC and 6H-SiC powders have similar lateral sizes of 2-3 μm. The energy dispersive spectroscopy (EDS) mapping images exhibited uniform distribution of Si and C signals with negligible O signal. The high-resolution transmission electron microscopy (HRTEM) images further revealed the different atomic arrangement and lattice fringes of the two phases. FIGS. 2F-2K. The 0.25 nm interplanar spacing (d) corresponds to the (111) plane of 3C-SiC (FIG. 2G, which is a zoom-in HRTEM image of 3C-SiC in box 251 of FIG.2F), while the d at 0.26 nm corresponds to the (010) plane of 6H-SiC (FIG.2J, which is a zoom-in HRTEM image of 6H-SiC in box 281 of FIG.2I). The distinct selected-area electron diffraction (SAED) patterns further confirm the structural difference of 3C-SiC and 6H-SiC (FIGS. 2H and 2K, respectively). The silicon-based yield was tested by inductively coupled plasma mass
Attorney Docket No.: 072174-05701 spectrometry (ICP-MS), which maintained a high value of 94% and 91% for 3C-SiC and 6H- SiC, respectively, indicating that the FCR process leads to negligible silicon loss. Mechanism Of The Phase Transformation Process [0146] To investigate the SiC phase transformation process, the phase ratios were calculated of SiC samples synthesized under different input voltage and flash times from the XRD patterns. FIGS.3A-3B (plots 301-302 in FIG.3A are 3C-SiC and 6H-SiC, respectively; plots 311-312 in FIG. 3B are 3C-SiC and 6H-SiC, respectively). It was observed that the increase of input voltage and flash times leads to the conversion from 3C-SiC to 6H-SiC, indicating that higher reaction temperature and longer reaction time facilitate the phase transformation. [0147] To explain the phase transformation mechanism, the detailed structural features of these two phases were first characterized. By using electron paramagnetic resonance (EPR) spectroscopy, Si vacancy was detected in both 3C-SiC and 6H-SiC. The different EPR line shapes of 3C-SiC and 6H-SiC suggest the different environments of Si vacancy. FIG.3C (plots 321-322 are 3C-SiC and 6H-SiC, respectively). [Son 2007]. The high temperature (~2900 °C, 150 V) during multiple FCR processes can lead to continuous evaporation of silicon atoms, contributing to higher content of silicon vacancy in 6H-SiC. FIG.3D (plots 331-332 are 3C- SiC and 6H-SiC, respectively). [0148] Furthermore, density functional theory (DFT) calculations were employed to depict the energy landscape of the Si-C system. FIGS.3E-3F (plots 341-342 in FIG.3E are 3C-SiC and 6H-SiC, respectively; crystal structures 351-352 are 3C-SiC and with atomic content of Si vacancy of 1 at% and 10 at%, respectively; crystal structures 353-354 are 6H-SiC and with atomic content of Si vacancy of 10 at% and 15 at%, respectively). It is shown that silicon vacancy dominated the formation energy of the Si-C phases and served as a key factor for the SiC phase transformation. FIGS.3E-3F. With a low content of silicon vacancy (<10 at%), 3C- SiC exhibited a lower formation energy than 6H-SiC, while 6H-SiC was more
Attorney Docket No.: 072174-05701 thermodynamically stable with a higher content of silicon vacancy (>10 at%, FIGS.3E-3F). When further considering the possible double-silicon-vacancy in SiC, the trend of the phase- dependent formation energy is similar, where 3C-SiC was more stable with a lower content of silicon vacancy and 6H-SiC was more stable with a higher content of silicon vacancy. [0149] It is noteworthy that conventional carbothermal reduction processes, involving hours to days of reaction time [Shin 2005; Guo 2013], are unfavorable for SiC phase control. In contrast, in the present FCR process, the phase controllability benefits from the ultrafast heating and cooling rates, and precise energy input, where the 3C-SiC and 6H-SiC can be selectively synthesized. LIB Performance Of SiC-Based Anode Material [0150] SiC with Si–C bilayer stacking structure provides an ideal space for lithium-ion intercalation and is regarded as a potential anode material for LIBs. [Sun 2020; Li 2016; Yu 2022]. The electrochemical properties of SiC, including carrier density, electron conductivity and ion diffusion performance are highly dependent on its phase. [Shen 2020; Kong 2020]. Therefore, phase control is important for the performance of SiC anodes in LIBs. [0151] First, the FCR-synthesized SiC was applied with graphene residue and the bare SiC after calcination as the anodes in coin cells with lithium chips serving as the counter electrodes. It was observed that the inclusion of graphene in the anode improves its performance, with an optimal SiC ratio of ~60 wt%. This improvement of the anode performance could be attributed to the enhanced carrier density and better electrical conductivity of SiC in the presence of graphene, as demonstrated in the simulated density of states (DOS) band and electrochemical impedance spectra. [0152] The battery performances of 3C-SiC and 6H-SiC anodes were further compared. The long-term galvanostatic discharge-charge cycling results reveal that both 3C-SiC and 6H-SiC anodes can maintain a stable capacity over 200 cycles with a capacity loss of ~5%. FIGS.4A-
Attorney Docket No.: 072174-05701 4C (with plots 401-404 in FIG.4A for 1
st, 10
th, 100
th, and 200
th cycles, respectively; with plots 411-414 in FIG. 4B for 1
st, 10
th, 100
th, and 200
th cycles, respectively; plots 421-422 in FIG. 4C for specific capacity for 3C-Sic anode and 6H-SiC anode, respectively; and plots 423-424 in FIG. 4C for coulombic efficiency for 3C-Sic anode and 6H-SiC anode, respectively). However, the 3C-SiC anode exhibited an excellent capacity of 741 mAh·g
-1 after 200 cycles, which was ~16% higher than that of 6H-SiC (626 mAh·g
-1). The average specific capacity of 3C-SiC anode is 781, 765, 679, 550 and 309 mAh·g
-1 at the rate of 0.1 C, 0.2 C, 0.4 C, 0.8 C and 1.6 C, respectively, all of which exhibit enhanced performances compared with those of the 6H-SiC anode. FIG.4D, TABLE II. (In FIG.4D, spots 431a-431f show the rate capacity of 3C-SiC anode at different scan rates and spots 432a-432f show the rate capacity of 6H-SiC anode at different scan rates). When using the cycling rate of 0.4 C, the 3C-SiC anode exhibits 82% capacity retention after 200 cycles, which is higher than that of the 6H-SiC anode (71%). TABLE II Specific capacity of SiC-based anode under different cycling rate

Note: The retention ratio of the anode capacity was calculated by the ratio between the average capacity at a certain cycling rate and the average capacity at 0.1 C. [0153] After cycling, the solid electrolyte interphase (SEI) layer covered the surface of SiC anode continuously and uniformly. The phase, structure and crystallinity of SiC were maintained, as confirmed by XRD patterns and XPS spectra, proving the excellent stability of SiC as the LIB anode material. [0154] The mechanism of the phase-dependent LIB performance of SiC was further investigated. First, the two phases of SiC powders have comparable specific surface areas, as shown by the Brunauer–Emmett–Teller (BET) characterizations. This eliminated the
Attorney Docket No.: 072174-05701 interference of specific area and pore-size distributions on their LIB performance. Further ICP- MS results show the contents of trace metal impurities, specifically Fe, Ni, Co, Mn and Li, in both 3C-SiC and 6H-SiC are well below 50 ppm, thereby avoiding their negative influence on anode performance. [Li 2023; Chen 2023]. [0155] Second, cyclic voltammetry (CV) was performed to assess the Li
+ diffusion kinetics. For both 3C-SiC and 6H-SiC anodes, the irreversible lithiation peak at ~0.8 V in the first scan relates to the SEI formation, corresponding to the discharging platform in FIGS.4A-4B. After the first-cycle scan, with further increasing potential scan rate, all CV curves exhibited similar shapes during the lithiation/delithiation processes, suggesting the reversible Li
+ insertion and extraction, and small polarization. FIGS.4E-4F (plots 441-446 in FIG.4E are for 0.1 mV/s, 0.5 mV/s, 1.0 mV/s, 2.0 mV/s, 5.0 mV/s, and 10.0 mV/s, respectively; and plots 451-456 in FIG. 4F are for 0.1 mV/s, 0.5 mV/s, 1.0 mV/s, 2.0 mV/s, 5.0 mV/s, and 10.0 mV/s, respectively). [0156] Generally, Li
+ storage mainly includes two parts: the diffusion-controlled Faradaic reaction process and the surface-induced capacitive process. The contribution of these two processes can be calculated according to the equation of i = av
b, where i is the current, v is the scan rate, a and b are adjustable constants. [Qian 2018]. Here, b can be used to describe various reaction kinetics during the ion-storage process, which was calculated from the slope of log(i) versus log(ν) with the value of ~0.5 for both 3C-SiC and 6H-SiC anodes. It indicated that the Li
+ diffusion process was the dominant process for the SiC anode. [Chen 2015]. [0157] Third, EIS spectra revealed that the 3C-SiC anode had a lower charge-transfer resistances (R
ct = 139 Ω, corresponding to the semicircle in the high-to-medium frequencies) compared with that of the 6H-SiC anode (R
ct = 181 Ω) (FIG.4G, with plots 461-462 for 3C- SiC anode and 6H-SiC anode, respectively), indicating the higher charge-transfer rate of 3C- SiC anode. [Kim 2018]. The slope in the low-frequency region is related to the Li
+ diffusion
Attorney Docket No.: 072174-05701 process. The higher slope of 3C-SiC anode suggests its higher Li
+ diffusion efficiency. FIG. 4G. After 100 and 200 cycles, the EIS curves exhibit lower charge-transfer resistances and lower slope in the low-frequency region, which indicates the improvement of charge-transfer behavior but a decay in Li
+ diffusion efficiency after cycling. Therefore, the EIS results confirmed that Li
+ diffusion is the dominant process for the SiC anode, which is consistent with the CV results. [0158] Last, the diffusion coefficients of SiC anodes were quantitatively measured by the galvanostatic intermittent titration technique (GITT). [Chen 2023; Yang 2018]. The Li
+ diffusion coefficients of 3C-SiC and 6H-SiC anode materials (D
Li +) were measured by the galvanostatic intermittent titration technique (GITT), according to Fick’s second law. During the tests, the representative GITT curve tested under the cycling conditions of 0.1 C, where the duration time of each current pulse (τ) is set as 1800 s with a relaxation time of 7200 s after each pulse. The voltage is recorded every 1 s. [0159] During the discharging process, the potential first rapidly decreases, which can be attributed to the electrical internal resistance of the electrodes. Afterwards, the decrease in potential rate slows, due to the electrochemical Li
+ deintercalation upon galvanostatic discharge. After each current pulse, the potential then instantaneously increases due to the electrical internal resistance. Finally, it gradually reaches the quasi-equilibrium open circuit potential. [Chen 2023; Sun 2020]. [0160] Then the D
Li + could be calculated as Eq. (1):
where, DLi
+ (cm
2 s
−1) is chemical diffusion coefficient of Li
+; τ is the duration of the current pulse (s). n
B is the moles (mol) of active material, V
B (cm
3 mol
−1) is molar volume; S (cm
2) is the apparent area of electrode area; τ (s) is the pulse time; ΔE
τ (V) is the potential change in a single-step of the current pulse; ΔE
s (V) is the steady-state potential change between steps.
Attorney Docket No.: 072174-05701 [0161] The 3C-SiC anode showed a higher Li
+ diffusion coefficient than the 6H-SiC anode under different voltages, with an average increase of 31% and 26% in charge and discharge processes, respectively. FIG. 4H (plots 471-472 for 3C-SiC anode and 6H-SiC anode, respectively). These findings support the notion that the enhanced performance of 3C-SiC anode results from the improved Li
+ diffusion. [0162] Based on the excellent half-cell performance, the 3C-SiC anode was further applied as the anode in the full-cell battery with the commercial NMC622 (LiNi
0.6Mn
0.2Co
0.2O
2) as the cathode. After 200 cycles, the capacity of the full cell can maintain a high value of 2.39 mAh with a capacity retention of 82% (FIG. 4I, with plots 481-482 for capacity and coulombic efficiency, respectively), where the areal capacity was calculated as 1.55 mAh cm
-2. This indicated that the flash-upcycled SiC anode material holds promise as an anode material for high-performance rechargeable batteries. Scalability Demonstration [0163] The FCR method demonstrates good scalability. The upcycling of FRPs and the phase control of SiC mainly depend on the flash peak temperature and the flash duration. Therefore, temperature control is expected to be a factor for the scale-up process. [0164] Initial analysis revealed that the increase of flash voltage and capacitance of the FCR system can enhance the productivity per batch. The FCR process can be scaled to higher production of the product, as demonstrated in Deng 2021. The theoretical possibility for scaling up was first analyzed and then the scalability of the process was demonstrated by successfully producing gram-scale samples in a batch process. Scaling Rule Of FCR Process By Theoretical Analysis [0165] For the FRP upcycling process, the conversion from silicon dioxide to silicon carbide and its phase transformation relies on the maximum flash temperature and the flash time. FIG. 1D; FIGS.3A-3F. Hence, the flash temperature across the sample has import when scaling up.
Attorney Docket No.: 072174-05701 For the Joule heating process, the heat (Q) is calculated by Eq. (2), ^^^^ = ^^^^
2 ^^^^ ^^^^ (2) where I is the current passing through the sample, R is the sample resistance, and t is the discharging time. The heat amount per volume (Q
v) is calculated by Eq. (3), ^^^^
v = ^^^^
2 ^^^^
e ^^^^ (3) where j is the current density, and ρ
e is the electrical resistivity. For a specific sample, the electrical resistivity (ρ
e) is constant. [0166] The temperature difference (ΔT) is proportional to the heat amount by Eq. (4), ^^^^ = ^^^^
p ^^^^∆ ^^^^ (4) where C
p is heat capacity and m is the mass of the sample. The Eq. (4) could be reformulated per volume to Eq. (5), ^^^^
v = ^^^^
p ^^^^
m∆ ^^^^ (5) where ρ
m is the density of the sample. For a specific sample, the C
p and ρ
m were constant; hence, maintaining a constant Q
v is proportional to ΔT. [0167] The charge amount (q) in the capacitor bank could be calculated by Eq. (6), ^^^^ = ^^^^ ^^^^ (6) where C is the capacitance of the capacitor bank, and V is the voltage of the capacitor bank. Assuming that all the charges in the capacitor bank are discharged within the time of t, the current density (j) could be calculated by Eq. (7), ^^^^ =
^^^^ ^^^^ ^ ^^^^ =
^^^ ^^^^ ^^^^ (7) where S is cross-sectional area of the sample. Since we usually use the cylinder-shaped sample, the mass (m) could be calculated by Eq. (8), ^^^^ = ^^^^
m ^^^^ ^^^^ (8) where ρ
m is the density of the sample, S is the cross-sectional area of the sample, and L is the length of the sample. For a specific sample type, the density (ρ
m) is kept the same.
Attorney Docket No.: 072174-05701 [0168] To summarize, the below Eq. (9) is obtained determining the current density,
[0169] Hence, ΔT can be calculated following the Eq. (10) below.
[0170] Based on the calculations above, an increase the mass (m) of the sample, combined with maintaining a constant temperature difference (ΔT) is required to scale up the FCR process There are two routes that can be adopted: (1) increasing the input flash voltage (V), and/or (2) increasing the capacitance (C) of the FCR system. Scaling Up To Gram Scale Per Batch [0171] In a first-generation flash setup, a capacitor bank was used that composed of 10 aluminum electrolytic capacitors (450 V, 6 mF, Mouser #80-PEH200YX460BQU2) with the total capacitance of C
0 = 60 mF. In a small-scale experiment, the input flash voltage (V
0) of 100 V and capacitance (C
0) of 60 mF were used for the sample mass of m
0 = 0.30 g. [0172] Subsequently, a second-generation FCR system was developed with a larger capacitance (C = 0.624 F). The scaling up of the FCR process was demonstrated to an input mass of m
1 = 10 g based on the second-generation flash setup. Thus, the formula of Eq. (11) was obtained,
[0173] For a mass of m
1 = 10 g and C
1 = 0.624 F, a flash voltage of V
1 = 300 V was used, which agrees with Eq. (11). The peak temperature during this flash process is ~2000 °C, similar to the small-batch flash temperature (FIG.1C), proving the efficiency of the scale-up. [0174] With an input voltage of 300 V, the sample temperature can ramp to 2000 °C, and 10 g of SiC per batch can be synthesized within 5 s. The FCR process can be potentially integrated to a continuous feed system, enabling continuous upcycling of FRPs, such as shown by the
Attorney Docket No.: 072174-05701 system 500 shown in FIG.5. In system 500, a sheet metal belt 501 is used for converting the milled FCR precursors (such as FCR precursors prepared by using grinder 503 to grind waste GFRP 502a and/or waste CFRP 502). Doctor blade 504 can be used to control the thickness and the compactness of the precursors. During FCR, the sheet metal belt 501 and another conductive column are connected to external electrical power source 506 as two electrodes 505. The entire system can be set in a vacuum or inert gas-filled chamber (in the FCR zone 507) to avoid the oxidation of as-synthesized SiC 508. [0175] Moreover, the flash process is undergoing scale-up for graphene synthesis, en route to a productivity of tonnes per day by 2024. [Luong 2020]. This capability can be readily harnessed for FRP upcycling purposes. Life Cycle Assessment And Techno-Economic Analysis [0176] A comparative cradle-to-gate life cycle assessment (LCA) was conducted to compare the environmental impact and energy demand of the FCR upcycling process with other FRP disposal routes. [0177] The study followed to the ISO 14044 requirements (Life cycle assessment-requirements and guidelines (ISO 14044:2006)) with the aim of comparing the potential environmental impact of the current recycling processes of FRP, such as solvolysis [Liu 2006] and incineration [Dong 2019; Xue 2021], with the FCR upcycling GFRP into SiC. A goal of the assessment was to determine whether the FCR strategy results in reduced GHG emissions and energy consumption. Scenario Description And System Boundaries [0178] Three scenarios were considered in the study. FIG.6A; TABLE III. In each scenario, 1 tonne of silicon carbide for service life is used as the baseline, and all other materials flows are normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne of SiC during FCR process.
Attorney Docket No.: 072174-05701 TABLE III Materials flow for various scenarios

Note:
aThe materials mass flow is normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne of SiC during FCR process.
bGFRP, glass fiber reinforced plastic; CFRP, carbon fiber reinforced plastic; FCR, flash carbothermal reduction. [0179] Scenario 1 Solvolysis: In this prior-art solvolysis scenario 601, the GFRP (1.5 tonnes) and CFRP (0.75 tonne) were immersed into 112.5 tonnes of 6 M nitric acid (33 wt% concentrated nitric acid-67 wt% water) to dissolve the polymer matrix in a 60 °C water bath for 5 h. [Liu 2006]. Then, the recovered FRP (1.5 tonnes) was washed by 1.5 tonnes of acetone in an agitator (200 rpm) for three times. This process consumes 37.5 tonnes of concentrated nitric acid, 75 tonnes of water, and 1.5 tonnes of acetone. The solvents can be recovered, with an assumed recovery yield of 98% of nitric acid and 95% acetone (while the recovering process was not accessed herein). [0180] Scenario 2 Incineration: For the prior-art incineration scenario 602, the GFRP (1.5 tonnes) and CFRP (0.5 tonne) were incinerated. Afterwards, the remaining ash (1 tonne, mainly silicon dioxide) was purified and remolded. [0181] Scenario 3 FCR upcycling process: During the herein-disclosed FCR process 603, 3C-SiC was taken as an example of the output upcycling product. Waste GFRP (1.5 tonnes) and CFRP (0.75 tonne) were mixed and then milled into powder. 3C-SiC (1 tonne) was synthesized by the FCR process.
Attorney Docket No.: 072174-05701 Life cycle inventory [0182] The environmental impacts, including energy consumption demand and GHG emission, for the materials production, processing, solvolysis, incineration and FCR processes are summarized in TABLE IV. The values are explained below. Note that 1 MJ electricity produces 0.13 kg GHG from Argonne GREET model. TABLE IV Life Cycle Inventory

Note:
aThe environmental impacts or energy demands are normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne of SiC during FCR process.
bGFRP, glass fiber reinforced plastic; CFRP, carbon fiber reinforced plastic; FCR, flash carbothermal reduction; GHG, greenhouse gas. [0183] Materials production: The GHG emission, energy consumption and water consumption for nitric acid (1961.8 kg tonne
-1, 10366 MJ tonne
-1, 4586.9 kg tonne
-1) and acetone (2548 kg tonne
-1, 65000 MJ tonne
-1, 0) were from the Argonne GREET model. [0184] Processing - Mixing: Energy input as needed for the mixing process, including the mixing of milled GFRP and CFRP for FCR, and the mixing of the silicon dioxide and carbon powder for thermal reduction. It was assumed that the mixing is conducted using an electrically driven Powder Mixer
9 with an energy consumption of 9.43 MJ tonne
-1. Correspondingly, 1.23 kg tonne
-1 GHG emitted during the mixing process. [0185] Processing - Milling: The GFRP and CFRP were required to be milled into powder
Attorney Docket No.: 072174-05701 before FCR. The energy input was assumed to be 270 MJ tonne
-1 according to the data from the literature [Den 2018], while 35.1 kg tonne
-1 GHG emission was assumed in the mixing process. The total mixing and milling energy demand and GHG emission for CFRP and GFRP were calculated to be 279.4 MJ tonne
-1 and 36.3 kg tonne
-1, as listed in TABLE IV. [0186] Processing - FCR: The energy consumption for FJH was estimated to be 1000 MJ tonne
-1 for the FCR synthesis of 3C-SiC powders. The energy consumption of the flash upcycling process is calculated using Eq. (12),
[0187] Where E is the consumed energy per gram (kJ g
-1), V
1 and V
2 are the voltage before and after flash, respectively, C is the capacitance (C = 60 mF), n is the times of flash, and M is the mass per batch. [0188] For the experiment to synthesize 3C-SiC with V
1 = 100 V, V
2 = 0 V, M = 0.3 g, and n = 1, the energy consumption is calculated to be: E = 1.0 kJ g
-1 = 0.28 kWh kg
-1. [0189] For the experiment to synthesize 6H-SiC with V
1 = 150 V, V
2 = 0 V, M = 0.3 g, and n = 10, the energy consumption is calculated to be: E = 22.5 kJ g
-1 = 6.25 kWh kg
-1 [0190] Given that the current industrial price of electrical energy in Texas, USA is $0.0587 kWh, the cost for upcycling 1 kg of waste FRP into SiC can be estimated to be: P = $0.016 to 0.37 kg
-1. [0191] The GHG was calculated based on the chemical equation in FIG. 1D and the GHG emission was calculated as 337.56 kg tonne
-1. [0192] Processing – Acid dissolution: 1 tonne of waste FRP immersed in 50 tonnes of 6 M nitric acid needed to be heated in a water bath at 60 °C for 5 h. An industrial wash bath equipment was used with the power of 1.2 kW (ref
10). The energy consumption was 21.6 MJ tonne
-1. Correspondingly, 2.81 kg tonne
-1 GHG emitted during the process. [0193] Processing – Acetone wash: It was assumed the acetone washing is conducted using
Attorney Docket No.: 072174-05701 an industrial agitator with the power of 0.4 kW with the tank of ~0.5 m
3, and operating time of 1 h. The energy consumption was calculated to be 0.8 kWh tonne
-1, or 2.88 MJ tonne
-1. [0194] Processing – Incineration: During the incineration process, the GHG emissions for CFRP and GFRP were 3390 and 1120 MJ tonne
-1, respectively, according to the data from the literature. [Dong 2018; Xue 2021]. Meanwhile, considering that incineration is an exothermic process, the energy consumption during the process approached zero. [0195] Processing – Purification and remolding: The GHG emission, energy consumption and water consumption during the purification and remolding process were 4654.4 kg tonne
-1, 85000 MJ tonne
-1 and 12.19 kg tonne
-1, respectively, from the Argonne GREET model. Life Cycle Impact Assessment [0196] Herein, the environmental impacts were classified into three midpoint indicators, including energy demand (TABLE V), GHG emission (TABLE VI) and water consumption (TABLE VII). TABLE V Cumulative energy demand for various scenarios
Note:
aThe materials mass flow is normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne SiC during FCR process.
bGFRP, glass fiber reinforced plastic; CFRP, carbon fiber reinforced plastic; FCR, flash carbothermal reduction.
Attorney Docket No.: 072174-05701 TABLE VI Cumulative GHG emissions for various scenarios
Note:
aThe materials mass flow is normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne SiC during FCR process.
bGFRP, glass fiber reinforced plastic; CFRP, carbon fiber reinforced plastic; FCR, flash carbothermal reduction; GHG, greenhouse gas. Supplementary Table VII Cumulative water use (CWU) for various scenarios
Note:
aThe materials mass flow is normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne SiC during FCR process.
Attorney Docket No.: 072174-05701 Cost Evaluation [0197] Herein, the costs for raw materials are from the current prices of commercial products, including concentrated nitric acid ($30000 tonne
-1), water ($0.5 tonne
-1), acetone ($1000 tonne
-1). The current costs for energy consumption were calculated according to the industrial electricity rate in Texas, US ($0.0587 kWh
-1, US Energy Information Administration). The values are listed in TABLE VIII. The materials cost and energy cost in electricity are calculated, as shown in TABLE IX. The operating cost is calculated as the sum of the materials cost and energy cost without including labor cost in the operating expense. TABLE VIII Materials and energy cost inventory
Note:
aThe materials mass flow is normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne SiC during FCR process.
bThe consumed energy is assumed to be from electricity, and the industrial price of electrical energy in Texas, USA is $0.0587 kWh. TABLE IX Cost evaluation of various scenarios
Attorney Docket No.: 072174-05701
Note:
aThe materials mass flow is normalized to the consumption amounts of GFRP (1.5 tonnes) and CFRP (0.75 tonne) for the production of 1 tonne SiC during FCR process. Sensitivity And Uncertainty [0198] There are some uncertainties associated with the energy demand, GHG emission, and water consumption values of the materials used herein due to the availability of data from different sources. [0199] Three scenarios were considered (FIG. 6A), namely, solvolysis 601 (the polymer matrix of GFRP and CFRP were dissolved by solvent), incineration 602 (GFRP and CFRP were incinerated and the ash was remolded into fiber) and FCR process 603 (GFRP and CFRP were upcycled into SiC powders by FCR process, and 3C-SiC was taken as the example of output products). [0200] Three environmental impacts, energy demand, GHG emission, and water consumption were analyzed. Benefitting from ultrashort reaction time and high energy efficiency, the FCR process exhibited a significant decrease of energy consumption, GHG emissions, and water consumption. FIG. 6B (area 611-613 for solvolysis, incineration, and FCR process, respectively). Specifically, the FCR process exhibited a low cumulative energy demand of 2879 MJ tonne
-1, which were ~77% and ~96% lower than that of the solvolysis and incineration recycling processes, respectively. FIG.6C; TABLE V. (In FIG.6C, bar 622 shows cumulative energy demand for the solvolysis materials, and bars 621a-621b show, respectively, cumulative energy demand for the incineration and FCR processes). [0201] The FCR process also demonstrates a cumulative GHG emission of 1709 kg tonne
-1, which is comparable with solvolysis process (1669 kg tonne
-1), and ~81% lower than the incineration process. FIG. 6D; TABLE VI. (In FIG. 6D, bar 632 shows cumulative GHG
Attorney Docket No.: 072174-05701 emission for the solvolysis materials, and bars 631a-631b show, respectively, cumulative GHG emission for the incineration and FCR processes). Both the FCR process and incineration processes showed minimal cumulative water use, whereas solvolysis process required substantial amounts of water. TABLE VII. When synthesizing 1 kilogram of SiC, the cost for FCR was as low as $0.047 kg
-1, which is ~0.2% and ~3.4% of the solvolysis and incineration processes, respectively, to recycle the corresponding amount of waste FRP. FIG.6E; TABLE VIII-IX. (In FIG. 6E, bar 642 shows operational cost for the solvolysis materials, and bars 641a-641b show, respectively, operational cost for the incineration and FCR processes). [0202] Then, the FCR process was compared with the conventional SiC synthesis processes, such as CVD and ACR. Generally, CVD processes require expensive gaseous precursors, and the deposition rate of SiC is ~10 μm h
-1 with low silicon utilization yield (<0.1%, TABLE X). [Booker 2016; Clavaguera-Mora 1997]. TABLE X Comparisons between different SiC synthesis methods

[0203] More versatile kinds of precursors can be used for SiC synthesis using carbothermic reduction methods. However, the traditional ACR process always lasts for hours, leading to significant energy consumption. [Shin 2005; Guo 2013] In contrast, the FCR process only lasted for seconds under a higher temperature (2000 – 3000 °C). The FCR reaction time was three to four orders of magnitude lower than other SiC synthesizing processes. TABLE X.
Attorney Docket No.: 072174-05701 These demonstrated the enormous potential of FCR as an economic and eco-friendly process for FRP upcycling and SiC synthesis. SiC Fibers/Fibrils [0204] Embodiments of the present invention further include adding a metal catalyst to the method to obtain SiC fibers and/or fibrils. For SiC nanowire (SiC NW) growth by flash Joule heating, there are mainly two technical routes using non-Fe-containing Si sources (FIG. 7A) and Fe-containing Si sources (FIG.7B). It should be noted that the final calcination step is not required if graphene does not influence further applications. Non-Fe Containing Si Sources [0205] TABLE XI shows parameters for examples of flash synthesis of SiC nanowires using non-Fe-containing Si sources. TABLE XI Parameters for flash synthesis of SiC nanowires using non-Fe-containing Si sources

Note: Each flash was conducted for a duration of 1 s. The mass ratio between the Si source and the C source is 2:1. [0206] For example, the non-Fe-containing Si source utilized included silica powders, silica
Attorney Docket No.: 072174-05701 gel, sand, diatomite, and glass fiber-reinforced plastics (GFRP), where the carbon sources can be carbon black, metallurgical coke (metcoke), biochar, chopped carbon fiber. In order to enhance the complete reaction between Si and carbon sources, these precursors can be ground into several micrometer sizes (or even smaller sizes), which, for example, was achieved by the planetary ball miller (MSE Supplies, PMV1-0.4L). The catalysts can be metal salts and, in the examples, mainly included at least one of the following metal elements: Fe, Co, and Ni. Other metals, such as Mo, Cr, V, Ru, Rh, Nb, may also be able to catalyze the nanowire growth. Iron chloride (FeCl
3), ferrocene, iron(III) acetylacetonate (Fe(acac)
3), nickel(II) acetylacetonate (Ni(acac)
2), cobalt(II) acetylacetonate (Co(acac)
2), were used as the catalyst for SiC NW synthesis, respectively. [0207] For the catalyst loading, the solvent was usually used to uniformly load the catalytic metal ion on the precursor surface. Experimentally, 5-50 mg of metal salts, were dissolved in 10 mL of ethanol with a concentration of 0.01-0.05 g mL
-1. Afterwards, 1 g of a mixture of Si and C sources was added into the ethanol solution and immersed into an ultrasonic bath (Cole- Parmer Ultrasonic Cleaner) for 15 min. The mixture was then dried in a vacuum desiccator overnight to ensure the uniform loading of the metal catalyst. Therefore, the catalyst loading content could be calculated to be 0.5-5 wt%. For a large-scale catalyst loading, the 0.25-2.5 g of catalysts was mixed with 50 g of Si and C sources using a planetary ball miller (MSE Supplies, PMV1-0.4L) with a rotating rate of 400 rpm for 3 h. [0208] During the nanowires synthesis process, 300 mg of the dried precursors with loaded catalysts were loaded into a quartz tube with an inner diameter (ID) of 8 mm and an outer diameter (OD) of 12 mm with two graphite electrodes on each side. The tube was loaded on a jig and connected to the external flash power system. The sample was enclosed in a vacuum desiccator at ~10 mmHg to facilitate outgassing of volatiles. The capacitor bank (60 mF) was charged by an AC supply and output a DC pulse. The maximal voltage of the capacitor bank
Attorney Docket No.: 072174-05701 coul reach 400 V. The relay with programmable delay time with millisecond controllability was applied to control the discharging time. The input voltage was modulated from 0 to 150 V and the discharging time was regularly set as 1 s. To ensure enough growth time for the nanowires, several electric pulse inputs (>3 times) were usually needed. [0209] In some experiments, silica powder (SiO
2, Millipore-Sigma, ~50 nm particle size) and carbon black (Cabot, Black Pearls 2000, average diameter ~10 nm) were taken as the representative Si and carbon sources. The SiC nanowire yield was investigated under different flash times, with ferrocene catalyst content of 1 wt%. With the increase of flash times from 1 to 5, the nanowire yield gradually increases to 63%. FIGS. 8A-8E (plots 841-842 in FIG. 8E for diameter and nanowire yield, respectively). Further increased flash times did not show a distinct influence on the yield. [0210] Different catalysts, including several FeCl
3, ferrocene, Fe(acac)
3, Ni(acac)
2, and Co(acac)
2 were compared It was found that Fe contributes a better catalytic performance than Ni and Co, and ferrocene and Fe(acac)
3 can benefit a better NW yield than FeCl
3. FIGS.9A- 9F. [0211] Using ferrocene as the catalyst, the catalyst concentration was modulated. It was found that more catalyst loading benefits the increase of NW yield in the flash products and leads to the increase of the NW diameter. FIGS. 10A-10E (plots 1041-1042 in FIG.10E for diameter and nanowire yield, respectively). As shown in FIGS. 8E and 10E, the diameters grew with five flashes around 100 nm in magnitude. Moreover, the length to width ratio of the NW were could be at least 3:1. It was also found that, with the increase in catalyst content, the nanowire yield and its diameter increased simultaneously. More catalyst concentration can increase the NW diameters, and longer heating times generally increases the aspect ratios (longer length). Accordingly, the aspect ratio can be modified/controlled by the duration of growth, by the concentration of catalyst, by the power input (temperature vs time profile), and combinations thereof. This provides that the NW can be grown to larger diameters and longer lengths. [0212] A series of characterizations were conducted to confirm the as-synthesized NW is SiC. Distinct SiC and graphene signals were observed in both XRD patterns and Raman spectrum. In TEM images,
Attorney Docket No.: 072174-05701 some Fe particles could be observed on the end of the nanowires, indicating its catalytic effect for the SiC NW growth. [0213] An optional calcination method was used to remove the flash graphene inside the SiC NW products. According to thermogravimetry (TGA) results, the flash-synthesized samples were calcined at 700 °C in the air for 1 h. (TGA was conducted in the 100 mL min-1 air flow with a heating rate of 10 °C min-
1). The NW maintained its original structures, and no carbon peaks were observed in Raman spectra and XRD patterns. [0214] GFRP, ground desert sand, and diatomite were also used as the Si sources. See FIGS.11A-11C shows the SEM images of the SiC NW synthesized from GFRP, desert sand, and diatomite. Fe Containing Si Sources [0215] TABLE XII shows parameters for examples of flash synthesis of SiC nanowires using Fe-containing Si sources. TABLE XII Parameters for flash synthesis of SiC nanowires using Fe-containing Si sources

Note: Fire glass (FG); coal fly ash (CFA). Each flash was conducted for a duration of 1 s. [0216] For example, for the Fe-containing Si sources, fire glass and coal fly ash (CFA) were used. X-ray fluorescence spectroscopy (XRF) was used to confirm the Fe contents were 5.3 at% and 6.6 wt%, respectively, for the fire glass and CFA. [0217] After grinding, when directly mixing it with carbon black and flash, the nanowire yield
Attorney Docket No.: 072174-05701 was often very low (<30 %), which was due to the low catalytic activity of Fe
2O
3 in fire glass. The NW growth is usually based on a vapor-liquid-solid (VLS) mechanism, where the volatilization of Fe compounds and the size of the Fe catalyst would influence its catalytic performance. Therefore, some halogen-contained additives, including polytetrafluoroethylene (PTFE), sodium fluoride (NaF), and polyvinyl chloride (PVC), were added to activate the inherent Fe in the fire glass with the content of 1 wt%. [0218] It was found that all of these halogen-contained additives can facilitate the NW synthesis, while PTFE realize the optimal NW yield of more than 60%. FIGS 12A-12E. The PTFE additive amount for NW growth was also investigated. It was found that ~1 wt% of PTFE can realize an optimal SiC NW yield of 60 wt% (FIG.12F), comparable to that of using the ferrocene as the catalyst. [0219] This strategy was extended to upcycle coal fly ash (CFA) into SiC NW. FIGS.13A- 13B. Similar to fire glass, the 1 wt% of PTFE can also significantly enhance the NW yield from CFA. Upscale [0220] For examples of enlarged NW synthesis, a mixture of Si sources (~5.0 g) and metcoke (~5.0 g) was loaded into a quartz tube with an ID of 1.6 cm and OD of 2.0 cm. TABLE XIII shows parameters for examples of scale-up flash synthesis of SiC nanowires. A large arc welder (TDK Lambda GENESYS 125-80), with a rated power of 10 kW, was used as the power source. [Tour ’535 Application; Eddy 2024]. After 60 s electrothermal heating, ~6 g SiC NW can be obtained from and fire glass and sand/ferrocene. FIGS.14A-14B.
Attorney Docket No.: 072174-05701 TABLE XIII Parameters for the scale up flash synthesis of SiC nanowires

Note: The mass ratio between the Si source and C is 1:1. SiCNW and SiC in Polymer Composites [0221] Embodiments of the present invention further include fabricating polymer composites that include SiC nanowires (SiCNW) and SiC. For example, composites can be prepared as follows. ~3 g of SiCNW was produced to test loadings of 0.5, 1, 3 and 5 wt% into a vinyl ester (VE) matrix. 5 g of VE (Fiberglass Supply Depot, as received) was added to a 20 mL scintillation vial and the amount of SiCNW added to the VE matrix depended on the desired wt % loading. The mixture of SiCNW and VE was then stirred at room temperature with a magnetic stir bar for 30 min at 300 rpm. [0222] After stirring, the mixture was then shear mixed with a homogenizer for 3 min at ~10 000 rpm.15 wt% (~0.15 g) of the catalyst/hardener, methyl ethyl ketone peroxide (MEKP) (Fiberglass Supply Depot), was added to the vial while stirring with a magnetic stir bar at 300 rpm for 5 min. [0223] The composites for nanoindentation, compression testing, and thermal conductivity testing were left in the scintillation vial overnight and the cured composite was released from the vial. The composite was then sanded using side of an abrasive wheel and then using 800, 1000, 1200, and 2500, 3000 grit sandpaper until it was the appropriate dimensions for microscale mechanical testing. The composites prepared for tensile testing were poured into a
Attorney Docket No.: 072174-05701 PTFE mold coated with silicone release agent and allowed to cure overnight. [0224] For mechanical properties, SiCNW-reinforced vinyl ester resin (VER) nanocomposites assessed using nanoindentation demonstrated an increase in compressive modulus at even 0.5 wt%, resulting in a 26% increase. FIG. 15. The Young’s modulus (bars 1501) and hardness (bars 1502) of SiCNW additive in VER composite was determined using triboindentation. At 3 wt% of SiCNW filler loading the hardness increased by 84.53% and the Young’s modulus increased 48.6% compared to the neat VER (n = 5). [0225] Macro-scale mechanical testing showed improvements under tensile testing at 1 wt% with the 1 wt% SiCNW composite showing 27% and 10% increases in Young’s Modulus and ultimate tensile strength (UTS). FIG.16 (with plots 1601-1604 for filler loading of 0 wt%, 0.5 wt% 1 wt%, and 3 wt%, respectively); FIG.17 (with plots 1701-1702 for filler loading of 0 wt%, and 1 wt%, respectively). Nanocomposites do not exhibit a linear increase in mechanical properties as more reinforcing agent is added, here 0.5-3 wt% of SiCNW show some improvement in the mechanical properties. Specifically, at 3 wt% of SiCNW filler loading the hardness increased by 84.53% and the Young’s modulus increased 48.6% compared to the neat VER. [0226] For compression of SiC particles in VER, it was found that there was a 59.22% and 40.70% increase in the Young’s Modulus in the 1 wt% and 5 wt% sample, respectively. FIG. 18 (with plots 1801-1804 for filler loading of 0 wt%, 0.5 wt% 1 wt%, and 5 wt%, respectively). [0227] For thermal properties, the temperature of heat flow vs. the distance along the z-axis of each thermocouple from the sample is shown in FIG.19. The points are fitted with a line that minimizes the least squared error, from which the heat flow is calculated. The uncertainty in heat flow and the uncertainty in temperature difference across the sample was calculated from the fitting. The area of the sample was calculated by measuring the volume of the sample and dividing it by thickness, with appropriate uncertainty. All uncertainties are propagated to final
Attorney Docket No.: 072174-05701 thermal conductivity value. [0228] FIG 20 shows thermal conductivity testing of SiC and SiCNW in VER composites. (Circles 2001a-2001d show the thermal conductive at a SiC loading of 0 wt%, 1 wt%, 3 wt%, and 5 wt%, respectively; Circles 2002a-2002d show the thermal conductive at a SiCNW loading of 0 wt%, 1 wt%, 3 wt%, and 5 wt%, respectively). FIG.17 shows that, a 5 wt% loading of filler the thermal conductivity of SiCNW is superior to that of SiC particles. The nanowires provide a connective pathway that allows for better conduction in the composite. [0229] With respect to mechanical strength, SiCNWs possess high tensile strength and Young’s modulus, which can reinforce polymer matrices, resulting in stronger, more durable composites. Moreover, the nanowires can improve the toughness of the polymer composites by preventing crack propagation, enhancing resistance to mechanical failure. [0230] With respect to thermal stability, due to SiCNWs and SiC excellent thermal conductivity, they can increase the thermal conductivity of polymer composites, which is useful for heat dissipation applications. Furthermore, by incorporating SiCNWs, the thermal conductivity of the polymer can be increased, which is beneficial in applications requiring heat dissipation. Additionally, in metal matrix composites, SiCNWs can reduce the thermal expansion mismatch between the metal matrix and other components, improving thermal stability. These composites also be used in high temperature applications. [0231] With respect to weight, the composites are lightweight. SiCNWs have a low density compared to traditional reinforcing materials like metals. The addition to polymers can improve the strength-to-weight ratio, which is essential in aerospace, automotive, and other lightweight applications. [0232] With respect to corrosion resistance, SiCNW-reinforced composites (polymer and metal matrix composites) can offer better corrosion resistance, especially in harsh environments, which can extend the lifespan of the composite and improve its durability.
Attorney Docket No.: 072174-05701 [0233] With respect to wear resistance, SiCNWs can improve the wear and abrasion resistance of polymer composites and metal matrix composites, which is critical in applications involving friction, , abrasion, ablation, or erosion such as gears, moving parts, wind turbine blades, aircraft, rockets, helicopter blades, turbine blades, missiles, or spacecraft. Likewise, the friction, abrasion, erosion, or ablation resistance of SiCNWs can make them useful for protective coatings for wind turbine blades, aircraft, rockets, helicopter blades, turbine blades, missiles, or spacecraft. Si Nanowires [0234] In some of the flashes performed, the flash times were modulated during the nanowire synthesis. XRD patterns revealed the co-existence of Si and SiC after flash. It was found that increasing the flash times from once to 5 times could lead to an increase of Si content from ~0.2 to ~37 wt%, accompanied with the signal of iron. However, both of SiC and Si signals were observed in Raman and XPS spectra, even for the products after 5 times flash. [0235] The possible reaction pathways were analyzed with the Gibbs free energy change calculated of at each step. These indicated Fe cannot directly reduce SiO
2 precursors into Si, but it will react with carbothermically reduced SiC and catalyze the formation of Si nanowires. Moreover, the other metals can be utilized in place of iron favor the formation of Si nanowires. [0236] As the iron residue (or other residue depending on the process utilized) can be removed, such as by washing, the Si NW can be used in applications, such as Si NW suitable for use in batteries. B4C Nanowires [0237] Embodiments of the present invention further include synthesizing B
4C nanowires ((B
4C NWs) by flash Joule heating. For example, B
4C NW can be grown by flash Joule heating as follow. The B source included boron powders (Millipore-Sigma, 95%), boric acid (Millipore-Sigma, 99.5%), where the carbon sources were carbon black, metallurgical coke
Attorney Docket No.: 072174-05701 (metcoke). The catalysts were metal salts and mainly included at least one of the following metal elements: Fe, Co, and Ni. Other metals, such as Mo, Cr, V, Ru, Rh, Nb, could also be able to catalyze the nanowire growth. Iron chloride (FeCl
3), ferrocene, iron(III) acetylacetonate (Fe(acac)
3), nickel(II) acetylacetonate (Ni(acac)
2), cobalt(II) acetylacetonate (Co(acac)
2), were used as the catalyst for B4C NW synthesis. [0238] For the catalyst loading, the solvent was usually used to uniformly load the catalytic metal ion on the precursor surface. Experimentally, 5-50 mg of metal salts were dissolved in 10 mL of ethanol with a concentration of 0.01-0.05 g mL
-1. Afterwards, 1 g of a mixture of B and C sources was added into the ethanol solution and immersed into an ultrasonic bath (Cole- Parmer Ultrasonic Cleaner) for 15 min. The mixture was then dried in a vacuum desiccator overnight to ensure the uniform loading of the metal catalyst. Therefore, the catalyst loading content can be calculated to be 0.5-5 wt%. For a large-scale catalyst loading, the 0.25-2.5 g of catalysts was also mixed with 50 g of B and C sources using a planetary ball miller (MSE Supplies, PMV1-0.4L) with a rotating rate of 400 rpm for 3 h. [0239] During the nanowires synthesis process, 300 mg of the dried precursors with loaded catalysts were loaded into a quartz tube with an inner diameter (ID) of 8 mm and an outer diameter (OD) of 12 mm with two graphite electrodes on each side. The tube was loaded on a jig and connected to the external flash power system. A commercial arc welder was used as the power source with a set input voltage of 120 V. For a larger scale, 3 g of precursors into a quartz tube with an inner diameter (ID) of 12 mm and an outer diameter (OD) of 16 mm. TABLE XIV shows parameters for the flash synthesis of B
4C nanowires.
Attorney Docket No.: 072174-05701 TABLE XIV Parameters for flash synthesis of B
4C nanowires
Note: BA denotes boric acid. B denotes boron powders. CB denotes carbon black. For the 300 mg sample per batch, 8 mm inner diameter (ID) tube was used as the reactor. For the 3 g sample per batch, 16 mm inner diameter (ID) tube was used as the reactor. [0240] The relationship between electrothermal heating time and B
4C NW yield was investigated. Usually, a longer duration time facilitates the higher yield of B
4C NW. FIG.21. Considering that there is no distinct increase of NW after 60 s, 60 s heating time was chosen for the examples. [0241] In the examples, different catalysts, including ferrocene, FeCl
3, Fe(NO
3)
3, Fe(acac)
3, Co(acac)
2, and Ni(acac)
2 were used. These catalysts are useful for B
4C NW synthesis. However, the Fe-based catalysts often benefit a better NW yield. FIG. 22. (In FIG. 22, all catalysts loading content was set at 1.0 wt% and the heating duration was 60 s). [0242] The catalyst loading content was modulated from 0.1 wt% to 2.5 wt%. FIGS. 23A- 23D. It was found that the increase in catalyst content would increase the nanowire yield and
Attorney Docket No.: 072174-05701 its diameters. However, the yield did not show a distinct increase when the catalyst content increased to higher than 1.0 wt%. FIGS.24A-24D; FIG.25. [0243] The as-synthesized NW was characterized. XRD patterns and Raman spectra show the as-synthesized NWs were B
4C. FIGS.26A-26B. The slight oxidation peak in B 1s XPS spectra came from the oxidation on its surface. FIG.26C. [0244] Boron powder was also used as the boron source (FIGS. 27A-27C), which is also a promising precursor for B
4C NW synthesis. [0245] Accordingly, the processes of embodiments of the present invention are faster, more energy efficient, and less expensive than other methods in producing gram-scale transition metal dichalcogenides. The crystallinity of the products is comparable to that produced via chemical vapor deposition, which requires minutes to hours to perform. [0246] These processes are also kinetically, rather than thermodynamically driven, allowing the formation of products that are unable to be synthesized through many other methods. Compared to conventional flash Joule heating, this method allows for the formation of products that cannot normally be formed. [0247] While embodiments of the invention have been shown and described, modifications thereof can be made by one skilled in the art without departing from the spirit and teachings of the invention. The embodiments described and the examples provided herein are exemplary only, and are not intended to be limiting. Many variations and modifications of the invention disclosed herein are possible and are within the scope of the invention. The scope of protection is not limited by the description set out above, but is only limited by the claims which follow, that scope including all equivalents of the subject matter of the claims. [0248] The disclosures of all patents, patent applications, and publications cited herein are hereby incorporated herein by reference in their entirety, to the extent that they provide exemplary, procedural, or other details supplementary to those set forth herein.
Attorney Docket No.: 072174-05701 [0249] Amounts and other numerical data may be presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a numerical range of approximately 1 to approximately 4.5 should be interpreted to include not only the explicitly recited limits of 1 to approximately 4.5, but also to include individual numerals such as 2, 3, 4, and sub-ranges such as 1 to 3, 2 to 4, etc. The same principle applies to ranges reciting only one numerical value, such as “less than approximately 4.5,” which should be interpreted to include all of the above-recited values and ranges. Further, such an interpretation should apply regardless of the breadth of the range or the characteristic being described. [0250] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood to one of ordinary skill in the art to which the presently disclosed subject matter belongs. Although any methods, devices, and materials similar or equivalent to those described herein can be used in the practice or testing of the presently disclosed subject matter, representative methods, devices, and materials are now described. [0251] Following long-standing patent law convention, the terms “a” and “an” mean “one or more” when used in this application, including the claims. [0252] Unless otherwise indicated, all numbers expressing quantities of ingredients, reaction conditions, and so forth used in the specification and claims are to be understood as being modified in all instances by the term “about.” Accordingly, unless indicated to the contrary, the numerical parameters set forth in this specification and attached claims are approximations that can vary depending upon the desired properties sought to be obtained by the presently disclosed subject matter.
Attorney Docket No.: 072174-05701 [0253] As used herein, the term “about” and “substantially” when referring to a value or to an amount of mass, weight, time, volume, concentration or percentage is meant to encompass variations of in some embodiments ±20%, in some embodiments ±10%, in some embodiments ±5%, in some embodiments ±1%, in some embodiments ±0.5%, and in some embodiments ±0.1% from the specified amount, as such variations are appropriate to perform the disclosed method. [0254] As used herein, the term “substantially perpendicular” and “substantially parallel” is meant to encompass variations of in some embodiments within ±10° of the perpendicular and parallel directions, respectively, in some embodiments within ±5° of the perpendicular and parallel directions, respectively, in some embodiments within ±1° of the perpendicular and parallel directions, respectively, and in some embodiments within ±0.5° of the perpendicular and parallel directions, respectively. [0255] As used herein, the term “and/or” when used in the context of a listing of entities, refers to the entities being present singly or in combination. Thus, for example, the phrase “A, B, C, and/or D” includes A, B, C, and D individually, but also includes any and all combinations and subcombinations of A, B, C, and D. REFERENCES [0256] PCT Application No. PCT/US2019/047967, filed on August 23, 2019, entitled “Flash Joule Heating Synthesis Method And Compositions Thereof,” to J.M. Tour, et al. (“Tour ’967 PCT Application”). [0257] U.S. Patent Application Serial No. 63/645,535, filed May 10, 2024, entitled “Scaled Flash Joule Heating Systems And Methods of Using Same,” to J.M. Tour, et al. (“Tour ’535 Application”). [0258] Ahrens, A., et al., “Catalytic disconnection of C–O bonds in epoxy resins and composites,” Nature, 2023, 617, 730-737 (“Ahrens 2023”).
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