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WO2017209545A1 - Agent antimicrobien contenant des nanoparticules non oxydiques du groupe carbone et procédé de production associé - Google Patents

Agent antimicrobien contenant des nanoparticules non oxydiques du groupe carbone et procédé de production associé Download PDF

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WO2017209545A1
WO2017209545A1 PCT/KR2017/005748 KR2017005748W WO2017209545A1 WO 2017209545 A1 WO2017209545 A1 WO 2017209545A1 KR 2017005748 W KR2017005748 W KR 2017005748W WO 2017209545 A1 WO2017209545 A1 WO 2017209545A1
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nps
carbon
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조원일
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SHONANO Co Ltd
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SHONANO Co Ltd
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Priority claimed from KR1020170035634A external-priority patent/KR101804570B1/ko
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Priority to JP2019515756A priority Critical patent/JP6782836B2/ja
Priority to EP17807038.9A priority patent/EP3466263A1/fr
Priority to CN201780033856.0A priority patent/CN109310084A/zh
Priority to US16/306,339 priority patent/US20190159459A1/en
Publication of WO2017209545A1 publication Critical patent/WO2017209545A1/fr
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
    • A01N25/28—Microcapsules or nanocapsules
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/14—Boron; Compounds thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23B—PRESERVATION OF FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES; CHEMICAL RIPENING OF FRUIT OR VEGETABLES
    • A23B2/00—Preservation of foods or foodstuffs, in general
    • A23B2/70—Preservation of foods or foodstuffs, in general by treatment with chemicals
    • A23B2/725—Preservation of foods or foodstuffs, in general by treatment with chemicals in the form of liquids or solids
    • A23B2/788—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • A61K9/51—Nanocapsules; Nanoparticles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin

Definitions

  • the present invention relates to an antimicrobial agent comprising carbon group non-oxide nanoparticles and a method for producing the same.
  • Carbon group (Group 4A or Group 14) elemental nanoparticles are of high interest to many researchers as key elements in the development of nanodevices and applications as next-generation silicon-based optoelectronic devices.
  • Field application transistors (TFT), solar cells using PN junctions, diodes and indicators of living organisms have a wide range of applications.
  • silicon nanoparticles which is one of the carbon groups
  • silicon sources such as silicon tetrachloride and silicon triethyl orthosilicate, which is an excessive amount of silicon nanoparticles.
  • impurities such as carbon after capping, oxidation and sintering of silicon nanoparticles remain.
  • VLS vapor-liquid-solid
  • SLS solid-liquid-solid
  • carbon group nanoparticles such as silicon have been mainly applied to electronic products and the like, and there is no example of modifying the surface of the carbon group nanoparticles and using them as an antimicrobial agent.
  • Patent Document 0001 Korean Patent Publication No. 10-2012-0010901 (2012.02.06)
  • Patent Document 0002 Korean Patent Publication No. 10-2014-0072663 (2014.06.13)
  • the present invention is to solve the above-mentioned problems of the prior art, an object of the present invention is to exhibit an excellent antimicrobial effect even in a small amount, and the manufacturing process is simple, the antimicrobial agent containing carbon group non-oxide nanoparticles and low manufacturing cost and its It is to provide a manufacturing method.
  • One aspect of the present invention provides an antimicrobial agent comprising carbon group non-oxide nanoparticles having an average particle size of 5 to 400 nm.
  • the carbon-group non-oxide nanoparticles of the present invention have been found to exhibit a remarkably superior antimicrobial effect as compared to conventional organic antimicrobials.
  • carbon group non-oxide nanoparticle means a particle containing at least one carbon group (Group 14) element of C, Si, Ge, Sn, and further including B, if necessary. It is to be understood as a concept including a particle in which a different carbon group element is alloyed or boron (B) is alloyed in at least one carbon group element, a compound composed of a different carbon group element, and a compound composed of a carbon group element and boron. Can be.
  • the carbon group non-oxide nanoparticles are Si nanoparticles, Si / B alloy nanoparticles, SiB x nanoparticles, Si / C alloy nanoparticles, Si / Ge alloy nanoparticles, Si / Ge / B alloy nanoparticles , Si / Ge / C alloy nanoparticles, Ge nanoparticles, Ge / B alloy nanoparticles, GeB x nanoparticles, Ge / C alloy nanoparticles, C / B alloy nanoparticles, CB 4 nanoparticles, Sn nanoparticles have.
  • non-oxide nanoparticle means a particle substantially free of oxygen element (O), the oxide layer (oxide) generated on the surface of the non-oxide nanoparticles by a naturally occurring oxidation reaction (oxide) layer, a first oxide layer).
  • the thickness of the first oxide layer may be 1 nm. Since the carbon group non-oxide nanoparticles having the thickness of the first oxide layer having a thickness of 1 nm or less have high reactivity with alcohol, carboxylic acid, water, etc., surface efficiency is improved by alkoxy group, carboxyl group, and hydroxyl group. Dispersibility due to electrical repulsive force between particles is excellent.
  • the antimicrobial effect of the carbon group non-oxide nanoparticles can be implemented by the following mechanism.
  • antigens exist on the surface of bacteria.
  • carbon-based non-oxide nanoparticles such as silicon nanoparticles
  • the antigens act as agglutinants and combine to aggregate and digest aggregates that are antibodies against them. do.
  • Carbon group non-oxide nanoparticles adsorbed on the surface of the bacteria may penetrate into the bacteria by the phospholipid movement (contraction, expansion) of the bacteria and kill the bacteria.
  • the carbon group non-oxide nanoparticles may act as a nutrient necessary for the survival of bacteria.
  • Bacteria which are packed with bacteria to ingest inorganic nutrients, try to absorb carbon-based non-oxide nanoparticles by contracting and expanding, but due to the size of the nanoparticles, they are trapped between the phospholipids. Then, the gap between the phospholipids gradually increases, and the electrolytes inside the bacteria are discharged to the outside, thereby killing the bacteria.
  • the average particle size of the carbon group non-oxide nanoparticles may be 5 ⁇ 400nm. If the average particle size of the carbon-based non-oxide nanoparticles is less than 5nm may cause random particle aggregation during the production of nanoparticles, if more than 400nm can not implement a cell killing effect according to the mechanism.
  • 1 to 4 are SEM images of an antimicrobial agent consisting of silicon non-oxide nanoparticles according to an embodiment of the present invention, immediately after contact and after 24 hours of antibacterial treatment, before contact with 50 ppm Staphylococcus aureus.
  • the silicon non-oxide nanoparticles are contacted with and adsorbed to the bacteria.
  • the Staphylococcus aureus is killed after the antibacterial treatment.
  • Staphylococcus aureus has a sphere of 500nm, but after the antimicrobial treatment, silicon non-oxide nanoparticles contact and adsorption, the sphere is crushed and bacteria Killed.
  • the carbon group non-oxide nanoparticles may be nanoparticles having a carbon layer having a predetermined thickness, for example, 100 nm or less, preferably, 1 to 100 nm, more preferably, 1 to 10 nm on the surface of the particles. .
  • the carbon layer prevents peroxidation due to contact of carbon group non-oxide nanoparticles with air and consequently thickening of the first oxide layer, thereby stably implementing the antibacterial performance of the carbon group non-oxide nanoparticles.
  • the thickness of the carbon layer is less than 1nm, it is difficult to properly block the contact between the nanoparticles and the air, and if the thickness of the carbon layer exceeds 100nm, the nanoparticles are excessively enlarged, and cell death effects according to the mechanism cannot be realized.
  • it may further include one or more functional groups selected from the group consisting of a carboxyl group, a hydroxyl group and an alkoxy group bonded to the surface of the first oxide layer.
  • the carboxyl group, the hydroxyl group, and the alkoxy group are treated with the carbon group non-oxide nanoparticles with alcohol, carboxylic acid, boric acid solution, water, and the like, specifically, the surface of the carbon group non-oxide nanoparticle, specifically, the first oxide layer. Can be bonded to the surface.
  • the carbon group non-oxide nanoparticles in which the functional group is bonded to the surface not only shows an excellent antimicrobial effect, but also simplifies the manufacturing process and shows an excellent antimicrobial effect even with a small amount of use. It has excellent applicability to various products such as, so it is excellent in versatility and stability.
  • It may further include a second oxide layer made of boron oxide formed on the surface of the first oxide layer.
  • the second oxide layer prevents peroxidation due to contact of the carbon group non-oxide nanoparticles with air and thus thickening of the first oxide layer, thereby stably implementing the antibacterial performance of the carbon group non-oxide nanoparticles.
  • the antimicrobial agent may be provided in the form of a solution diluted to a certain concentration, for example, 1 to 1,000 ppm by water or the like, but the type of medium in which the antimicrobial agent may be diluted is not particularly limited. .
  • FIG. 5 another aspect of the invention, (a) preparing a carbon group non-oxide nanoparticles formed with a first oxide layer; (b1) preparing a mixed solution by mixing the carbon group non-oxide nanoparticles with one selected from the group consisting of alcohol, carboxylic acid, boric acid solution and water; And (c1) applying ultrasonic waves to the mixed solution.
  • FIG. 6 another aspect of the invention, (a) preparing a carbon group non-oxide nanoparticles formed with a first oxide layer; (b2) mixing the carbon group non-oxide nanoparticles with a first solution containing boric acid and an organic solvent to prepare a first mixed solution; (c2) applying ultrasonic waves to the first mixed solution to obtain carbon group non-oxide nanoparticles having a second oxide layer formed of boron oxide on the first oxide layer; (d) mixing the carbon group non-oxide nanoparticles with one selected from the group consisting of alcohol, carboxylic acid, boric acid aqueous solution and water to prepare a second mixed solution; And (e) applying ultrasonic waves to the second mixed solution.
  • the step (a) may be performed by irradiating a laser to a mixed gas containing at least one source gas containing a carbon group element and a sulfur hexafluoride catalyst gas.
  • Alcohols and carboxylic acids usable in step (b) are 1,10-decanediol, 1,2-propanediol, 1,2-hexanediol, 1,4-butanediol, 1,5-pentanediol, 1,8 -Octanediol, 1-decanol, 2,2,4-trimethylpentanediol, 2-butoxyethanol, 2-bromopentanoic acid, 2-bromohexadecanoic acid, 2-bromohexanoic acid, 2-ethylhexa Noric acid, 2-chlorobutanoic acid, 2-propanediol, 2-propenoic acid, 2-hydroxyethylmethacrylate, DHA, galtamine, galactose, galantamine, citric acid, glycine, gluconate, glucose, glutaric acid , Glutamine, glycerol, glycyrrhetinic acid
  • step (a) to irradiate a mixture of the carbon group non-oxide nanoparticles and carbon-based gas for example, acetylene gas or ethylene gas with a laser to form a carbon layer on the surface of the carbon group non-oxide nanoparticles It may further comprise the step of forming.
  • the organic solvent may be nonpolar.
  • a second oxide layer made of boron oxide may be formed on the first oxide layer in the step (c2) according to Scheme A below.
  • the boric acid solution dissolved in a polar solvent such as water in step (b2) does not produce an additional oxide layer made of boron oxide, the hydroxyl group derived from boric acid is the surface of the first oxide layer.
  • a functional group may be bonded to the surface of the carbon group non-oxide nanoparticle by applying ultrasonic waves for a predetermined time, for example, 4-6 minutes.
  • R is an alkyl or alkyl ketone group, aromatic or aromatic ketone group
  • the binding efficiency of the functional group to the surface of the carbon group non-oxide nanoparticles may be lowered, and if more than 6 minutes, more than necessary ultrasonic waves are applied, energy efficiency may be lowered.
  • the frequency of the ultrasonic wave is not particularly limited, and any frequency can be used as long as the frequency of the ultrasonic wave is commonly used, but it is preferable to use ultrasonic waves in the frequency range of 20 to 100 kHz.
  • an antimicrobial agent and a method of manufacturing the same provide an antimicrobial composition exhibiting excellent antimicrobial effect, and since the carbon group non-oxide nanoparticles having a thin oxide layer are used, there is no need to use a dispersant or a separate additive. It is inexpensive and has an excellent effect of simplifying the manufacturing process.
  • the antimicrobial agent containing functional group-substituted carbon group non-oxide nanoparticles exhibiting excellent antimicrobial effect even in a small amount has a low surface tension and excellent coating power, and thus can be applied to various products such as various electronic products, clothing, bags and shoes. It can be used in new drug development, resin, cosmetics and the like.
  • 1 is a SEM image before contacting the antibacterial agent and Staphylococcus aureus according to an embodiment of the present invention.
  • Figure 2 is an SEM image immediately after contact with the antibacterial agent and Staphylococcus aureus according to an embodiment of the present invention.
  • FIG. 3 is a SEM image after 24 hours after contact with the antibacterial agent and Staphylococcus aureus according to an embodiment of the present invention.
  • FIG. 4 is a SEM image of the antimicrobial agent and Staphylococcus aureus before and after 24 hours of contact according to an embodiment of the present invention.
  • FIG. 5 is a schematic diagram illustrating a method for preparing an antimicrobial agent according to an embodiment of the present invention.
  • FIG. 6 is a schematic diagram illustrating a method for preparing an antimicrobial agent according to another embodiment of the present invention.
  • FIG. 7 is a TEM image of silicon nanoparticles according to an embodiment of the present invention.
  • Silicon nanoparticles can be prepared according to (1) or (2) in Scheme 1 below.
  • a mixed gas obtained by mixing 100 parts by volume of monosilane (SiH 4 ) as a source gas, 400 parts by volume of nitrogen (N 2 ) as a control gas, and 40 parts by volume of sulfur hexafluoride (SF 6 ) catalyst gas
  • the internal pressure is supplied into the reaction chamber with 500torr, and the laser generated by the CO 2 laser generator is supplied to the mixed gas supplied into the reaction chamber in the form of a line beam of continuous wave having a wavelength of 10.6 ⁇ m through the laser irradiation unit. Irradiation for a time to produce a silicon nanoparticles (Si-NPs) in which the oxide layer was formed.
  • the average particle size of the prepared silicon nanoparticles having the oxide layer is 5 to 400 nm, the thickness of the oxide layer is 0.32 nm, and the yield is 97.1%.
  • Silicon-boron alloy nanoparticles or silicon boride nanoparticles may be prepared according to Scheme 2 below.
  • Monosilane (SiH 4 ), diborane (B 2 H 6 ), and nitrogen are mixed and injected into the reaction chamber to irradiate a CO 2 laser beam.
  • the diborane acts as a catalyst gas and a source gas, the energy absorbed at 10.6 ⁇ m wavelength is efficiently transferred to the monosilane, and the Si-H bond of the monosilane is well broken so that the silicon-boron alloy nanoparticles ( SiBx-NPs) are generated.
  • diborane is decomposed into boron and hydrogen atoms, boron alloys with silicon nanoparticles, and prevents oxidation of silicon.
  • Monosilane as a source gas is 90% or more of the total volume (volume of the raw material gas and the catalyst gas combined), and the catalyst gas is adjusted to the range of 10% or less of the total volume.
  • the carrier gas nitrogen is not more than 400 parts by volume compared to the source gas monosilane.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reaction chamber is prepared by setting in the range of 100 ⁇ 400torr. In this range, silicon-boron alloy nanoparticles (SiBx-NPs) having an average particle size of 5 to 400 nm and an oxide layer thickness of 0.57 nm are prepared.
  • Silicon-carbon alloy nanoparticles or silicon carbide nanoparticles can be prepared according to (1) or (2) in Scheme 3 below.
  • Monosilane (SiH 4 ), acetylene (C 2 H 2 ), and nitrogen are mixed and injected into the reaction chamber to irradiate a CO 2 laser beam.
  • Acetylene decomposes into carbon and hydrogen atoms, and carbon forms alloys with silicon nanoparticles, preventing the oxidation of silicon.
  • the source gas monosilane and acetylene are each injected at a volume ratio of 2: 1.
  • nitrogen as the carrier gas is not more than 400 parts by volume relative to the source gas monosilane.
  • the gas flow rate is in sccm.
  • the process pressure inside the reaction chamber is set in the range of 100 to 500 torr. In this range, silicon-carbon alloy nanoparticles (SiC-NPs) having an average particle size of 5 to 400 nm and an oxide layer thickness of 0.53 nm are prepared.
  • Silicon-germanium alloy nanoparticles can be prepared according to (1) or (2) in Scheme 4 below.
  • SiGe-NPs silicon-germanium alloy nanoparticles
  • Silicon-germanium-boron alloy nanoparticles can be prepared according to Scheme 5 below.
  • a mixed gas containing 400 parts by volume is supplied into a reaction chamber having an internal pressure of 80 to 400 torr, and a laser generated by a CO 2 laser generator to a mixed gas supplied into the reaction chamber has a wavelength of 10.6 ⁇ m. Irradiation for 3 hours in the form of a line beam of continuous waves to produce silicon-germanium-boron alloy nanoparticles (SiGeB-NPs).
  • the average particle size of SiGeB-NPs is 5 to 400 nm, and the thickness of the oxide layer formed on the surface thereof is 0.75 nm.
  • Silicon-germanium-carbon alloy nanoparticles may be prepared according to Scheme 6 below.
  • a continuous gas having a wavelength of 10.6 ⁇ m is supplied through a irradiation unit by supplying a mixed gas of 400 parts by volume into a reaction chamber having an internal pressure of 80 to 400 torr, and irradiating a laser generated by a CO 2 laser generator to a mixed gas supplied into the reaction chamber. Irradiated for 3 hours in the form of a line beam (Line Beam) of silicon-germanium-carbon alloy nanoparticles (SiGeC-NPs) was prepared.
  • the average particle size of SiGeC-NPs is 5 to 400 nm, and the thickness of the oxide layer formed on the surface thereof is 0.68 nm.
  • Germanium nanoparticles can be prepared according to (1) or (2) in Scheme 7 below.
  • a mixed gas is mixed with 100 parts by volume of germane (GeH 4 ) as a source gas, 400 parts by volume of hydrogen (H 2 ) as a control gas, and 40 parts by volume of sulfur hexafluoride (SF 6 ) catalyst gas. It is supplied into the reaction chamber with a pressure of 500torr, and the laser generated by the CO 2 laser generator is supplied to the mixed gas supplied into the reaction chamber in the form of a continuous beam line beam having a wavelength of 10.6 ⁇ m through the laser irradiation unit for 3 hours. During irradiation, germanium nanoparticles (Ge-NPs) in which an oxide layer was formed were prepared.
  • the average particle size of the germanium nanoparticles having the prepared oxide layer is 5 to 400 nm, the thickness of the oxide layer is 0.47 nm, and the yield is 98.7%.
  • Germanium-boron alloy nanoparticles or germanium boride nanoparticles may be prepared according to Scheme 8 below.
  • a mixed gas obtained by mixing 100 parts of germane (GeH 4 ), diborane (B 2 H 6 ), 40 to 80 parts of gas, and 400 parts by volume of nitrogen (N 2 ) as a carrier gas is mixed.
  • the internal pressure is supplied into the reaction chamber of 100 to 400 torr, and the laser generated by the CO 2 laser generator is supplied to the mixed gas supplied into the reaction chamber in the form of a continuous beam line beam having a wavelength of 10.6 ⁇ m through the irradiation unit. Irradiation for 3 hours to prepare germanium-boron alloy nanoparticles (GeBx-NPs).
  • the particle size of GeBx-NPs is 5-400 nm, and the thickness of the oxide layer formed on the surface is 0.52 nm.
  • Germanium-carbon alloy nanoparticles or germanium carbide nanoparticles may be prepared according to (1) or (2) in Scheme 9 below.
  • Jermaine (GeH 4 ), acetylene (C 2 H 2 ), and nitrogen are mixed and injected into the reaction chamber to irradiate a CO 2 laser beam.
  • Acetylene decomposes into carbon and hydrogen atoms, and carbon forms alloys with silicon nanoparticles, preventing the oxidation of silicon.
  • Jermaine and acetylene, raw material gases are injected at a volume ratio of 2: 1, respectively.
  • the carrier gas nitrogen does not exceed 400 parts by volume relative to the silane gas as the raw material gas.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reaction chamber is prepared by setting in the range of 100 ⁇ 500torr. In this range, germanium-carbon alloy nanoparticles (GeC-NPs) having an average particle size of 5 to 400 nm and an oxide layer thickness of 0.58 nm are produced.
  • Carbon-boron alloy nanoparticles or boron carbide nanoparticles may be prepared according to Scheme 10 below.
  • the internal pressure is supplied into the reaction chamber of 100 to 400 torr, and the laser generated by the CO 2 laser generator is supplied to the mixed gas supplied into the reaction chamber in the form of a continuous beam line beam having a wavelength of 10.6 ⁇ m through the irradiation unit. Irradiation for 3 hours to prepare carbon-boron alloy nanoparticles (CBx-NPs).
  • the particle size of CBx-NPs is 5 to 400 nm, and the thickness of the oxide layer formed on the surface thereof is 0.46 nm.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and Si-NPs of 5 to 400 nm of Preparation Example 1 are poured into the reactor chamber and then irradiated with a CO 2 laser beam. At this time, the CH bond of the acetylene gas may generate a carbon layer on the surface of Si-NPs. Nitrogen gas prevents oxidation of Si-NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr. When carbon is coated on Si-NPs in this range (C @ Si-NPs), the inner core is Si-NPs having a size of 5 to 400 nm, and a carbon layer in the range of 1 to 100 nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and SiB 4 -NPs of Preparation Example 2 of 5 to 400nm of Preparation Example 2 is poured into the reactor chamber, and then irradiated with a CO 2 laser beam. Let's do it. At this time, the CH bond of the acetylene gas may generate a carbon layer on the surface of SiB 4 -NPs. Nitrogen gas prevents oxidation of SiB 4 -NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is SiB 4 -NPs having a size of 5 ⁇ 400nm, a carbon layer in the range of 1 ⁇ 100nm is formed on the surface.
  • the mixture of acetylene gas (C 2 H 2 ) and nitrogen is injected into the reactor chamber, and SiC-NPs of Preparation Example 3 of 5 to 400 nm of Preparation Example 3 are poured into the reactor chamber, followed by irradiating a CO 2 laser beam. .
  • the CH bond of the acetylene gas may generate a carbon layer on the surface of the SiC-NPs. Nitrogen gas prevents oxidation of SiC-NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is SiC-NPs having a size of 5 to 400 nm, and a carbon layer in the range of 1 to 100 nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and SiGe-NPs of 5 to 400 nm of Preparation Example 4 are poured into the reactor chamber and then irradiated with a CO 2 laser beam. At this time, the CH bond of the acetylene gas may generate a carbon layer on the surface of SiGe-NPs. Nitrogen gas prevents oxidation of SiGe-NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is SiGe-NPs having a size of 5 to 400 nm, and a carbon layer in the range of 1 to 100 nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and SiGeB-NPs of 5 to 400 nm of Preparation Example 5 are poured into the reactor chamber and then irradiated with a CO 2 laser beam. At this time, the CH bond of the acetylene gas may generate a carbon layer on the surface of SiGeB-NPs. Nitrogen gas prevents oxidation of SiGeB-NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is SiGeB-NPs having a size of 5 to 400 nm, and a carbon layer in the range of 1 to 100 nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and SiGeC-NPs of 5 to 400 nm of Preparation Example 6 are poured into the reactor chamber and then irradiated with a CO 2 laser beam. At this time, the CH bond of the acetylene gas may generate a carbon layer on the surface of SiGeC-NPs. Nitrogen gas prevents oxidation of SiGeC-NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is SiGeC-NPs having a size of 5 to 400 nm, and a carbon layer in the range of 1 to 100 nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and the CO 2 laser beam is irradiated after flowing Ge-NPs of 5 to 400 nm of Preparation Example 7 into the reactor chamber. At this time, the CH bond of the acetylene gas may generate a carbon layer on the surface of Ge-NPs. Nitrogen gas prevents the oxidation of Ge-NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is Ge-NPs having a size of 5 to 400 nm, and a carbon layer in the range of 1 to 100 nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and the CO 2 laser beam is irradiated after flowing GeB 4 -NPs of 5 to 400 nm of Preparation Example 8 into the reactor chamber.
  • the CH bond of acetylene gas may generate a carbon layer on the surface of GeB 4 -NPs.
  • Nitrogen gas prevents oxidation of GeB 4 -NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is GeB 4 -NPs having a size of 5 ⁇ 400nm, a carbon layer in the range of 1 ⁇ 100nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and the CO 2 laser beam is irradiated after flowing GeC-NPs of 5 to 400 nm of Preparation Example 9 into the reactor chamber.
  • the CH bond of the acetylene gas may generate a carbon layer on the surface of GeC-NPs. Nitrogen gas prevents the oxidation of GeC-NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is GeC-NPs having a size of 5 to 400 nm, and a carbon layer in the range of 1 to 100 nm is formed on the surface.
  • Acetylene gas (C 2 H 2 ) and nitrogen are mixed and injected into the reactor chamber, and CB 4 -NPs of 5 to 400 nm of Preparation Example 10 are poured into the reactor chamber and then irradiated with a CO 2 laser beam. At this time, the CH bond of the acetylene gas may generate a carbon layer on the surface of the CB 4 -NPs. Nitrogen gas prevents oxidation of CB 4 -NPs.
  • the acetylene gas as the raw material gas contains 60 or more of the total volume part (volume part combined with acetylene gas and nitrogen gas), and nitrogen gas is adjusted to the range which does not exceed 40 or more of the total volume part.
  • the flow rate of gas is in sccm.
  • Process pressure inside the reactor chamber is prepared by setting in the range of 100 ⁇ 400torr.
  • the inner core is CB 4 -NPs having a size of 5 ⁇ 400nm, a carbon layer in the range of 1 ⁇ 100nm is formed on the surface.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare surface-modified Si-NPs with methoxy groups.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in 25 ml of ethanol, and ultrasonic waves were irradiated for 5 minutes to prepare Si-NPs surface-modified with an ethoxy group.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in 25 ml of isopropyl alcohol, and ultrasonic waves were irradiated for 5 minutes to prepare surface-modified Si-NPs with isopropoxy group.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic waves were irradiated for 5 minutes to prepare Si-NPs surface-modified with 2-aminoalkoxy groups.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in a mixture consisting of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified Si-NPs with butylphenoxy group.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified Si-NPs with an acetic acid.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in a mixture consisting of 0.5 g of stearic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified Si-NPs with stearic acid.
  • Si-NPs of Preparation Example 1 100 mg were dispersed in a mixture consisting of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified Si-NPs with acetylsalicylic acid.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in 25 ml of an aqueous boric acid solution (mixed at 5 parts by weight of boric acid and distilled water), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified Si-NPs with a hydroxyl group of boric acid.
  • Si-NPs of Preparation Example 1 100 mg was dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride were mixed at 1: 1 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified Si-NPs with a hydroxyl group of water.
  • an aqueous organic solvent solution water and methylene chloride were mixed at 1: 1 parts by weight
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare surface-modified SiB 4 -NPs.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiB 4 -NPs with ethoxy groups.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in 25 ml of isopropyl alcohol, and ultrasonic wave was irradiated for 5 minutes to prepare SiB 4 -NPs surface-modified with isopropoxy.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare SiB 4 -NPs surface-modified with 2-aminoalkoxy group.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in a mixture of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiB 4 -NPs with butylphenoxy group.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiB 4 -NPs with an acetic acid.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in a mixture of 0.5 g of stearic acid and 25 ml of dichloromethane, and irradiated with ultrasound for 5 minutes to prepare surface-modified SiB 4 -NPs with stearic acid.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in a mixture of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiB 4 -NPs with acetylsalicylic acid.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in 25 ml of an aqueous boric acid solution (mixed with boric acid and distilled water at 5:95 parts by weight), and ultrasonically irradiated for 5 minutes to prepare surface-modified SiB 4 -NPs with a hydroxyl group of boric acid. It was.
  • SiB 4 -NPs of Preparation Example 2 100 mg was dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride mixed at 1: 1 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiB 4 -NPs with a hydroxyl group of water. It was.
  • an aqueous organic solvent solution water and methylene chloride mixed at 1: 1 parts by weight
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare surface-modified SiC-NPs with methoxy groups.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare SiC-NPs surface-modified with an ethoxy group.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in 25 ml of isopropyl alcohol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiC-NPs with isopropoxy group.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic waves were irradiated for 5 minutes to prepare SiC-NPs surface-modified with 2-aminoalkoxy groups.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in a mixture consisting of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiC-NPs with butylphenoxy group.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiC-NPs with an acetic acid.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in a mixture consisting of 0.5 g of stearic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiC-NPs with stearic acid.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in a mixture of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiC-NPs with acetylsalicylic acid.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in 25 ml of an aqueous boric acid solution (mixed at 5 parts by weight of boric acid and distilled water), and ultrasonically irradiated for 5 minutes to prepare surface-modified SiC-NPs with a hydroxyl group of boric acid.
  • SiC-NPs of Preparation Example 3 100 mg was dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride were mixed at 1: 1 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiC-NPs with a hydroxyl group of water.
  • an aqueous organic solvent solution water and methylene chloride were mixed at 1: 1 parts by weight
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare SiGe-NPs surface-modified with a methoxy group.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGe-NPs with ethoxy groups.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in 25 ml of isopropyl alcohol, and ultrasonic wave was irradiated for 5 minutes to prepare SiGe-NPs surface-modified with isopropoxy group.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare SiGe-NPs surface-modified with 2-aminoalkoxy group.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in a mixture of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGe-NPs with butylphenoxy group.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGe-NPs with an acetic acid.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in a mixture of 0.5 g of stearic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGe-NPs.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in a mixture of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGe-NPs with acetylsalicylic acid.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in 25 ml of an aqueous boric acid solution (mixed with boric acid and distilled water at 5:95 parts by weight), and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGe-NPs with a hydroxyl group of boric acid.
  • SiGe-NPs of Preparation Example 4 100 mg was dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride were mixed at 1: 1 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGe-NPs with a hydroxyl group of water.
  • an aqueous organic solvent solution water and methylene chloride were mixed at 1: 1 parts by weight
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare SiGeB-NPs surface-modified with a methoxy group.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGeB-NPs with ethoxy groups.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in 25 ml of isopropyl alcohol, and ultrasonically irradiated for 5 minutes to prepare SiGeB-NPs surface-modified with isopropoxy.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare SiGeB-NPs surface-modified with 2-aminoalkoxy group.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in a mixture consisting of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGeB-NPs with butylphenoxy.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeB-NPs with an acetic acid.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in a mixture of 0.5 g of stearic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeB-NPs.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in a mixture consisting of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeB-NPs with acetylsalicylic acid.
  • SiGeB-NPs of Preparation Example 5 100 mg were dispersed in 25 ml of an aqueous boric acid solution (mixed with boric acid and distilled water at 5:95 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeB-NPs with a hydroxyl group of boric acid.
  • SiGeB-NPs of Preparation Example 5 100 mg was dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride were mixed at 1: 1 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeB-NPs with a hydroxyl group of water.
  • an aqueous organic solvent solution water and methylene chloride were mixed at 1: 1 parts by weight
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in 25 ml of methanol and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeC-NPs.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in 25 ml of ethanol, and ultrasonic waves were irradiated for 5 minutes to prepare SiGeC-NPs surface-modified with an ethoxy group.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in 25 ml of isopropyl alcohol, and ultrasonic wave was irradiated for 5 minutes to prepare SiGeC-NPs surface-modified with isopropoxy group.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare SiGeC-NPs surface-modified with 2-aminoalkoxy group.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in a mixture consisting of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGeC-NPs with butylphenoxy group.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeC-NPs with an acetic acid.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in a mixture of 0.5 g of stearic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeC-NPs.
  • SiGeC-NPs of Preparation Example 6 100 mg were dispersed in a mixture consisting of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeC-NPs with acetylsalicylic acid.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in 25 ml of an aqueous boric acid solution (mixed at 5 parts by weight of boric acid and distilled water), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeC-NPs with a hydroxyl group of boric acid.
  • SiGeC-NPs of Preparation Example 6 100 mg was dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride were mixed at 1: 1 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeC-NPs with a hydroxyl group of water.
  • an aqueous organic solvent solution water and methylene chloride were mixed at 1: 1 parts by weight
  • Ge-NPs of Preparation Example 7 100 mg were dispersed in 25 ml of isopropyl alcohol, and ultrasonic waves were irradiated for 5 minutes to prepare Ge-NPs surface-modified with isopropoxy group.
  • Ge-NPs of Preparation Example 7 100 mg were dispersed in 25 ml of 2-aminoalcohol, and ultrasonic waves were irradiated for 5 minutes to prepare Ge-NPs surface-modified with 2-aminoalkoxy groups.
  • Ge-NPs of Preparation Example 7 100 mg were dispersed in a mixture of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified Ge-NPs with butylphenoxy group.
  • Ge-NPs of Preparation Example 7 100 mg were dispersed in a mixture of 0.5 ml of acetic acid and 25 ml of dichloromethane, and ultrasonic waves were irradiated for 5 minutes to prepare Ge-NPs surface-modified with an acetic acid.
  • Ge-NPs of Preparation Example 7 were dispersed in a mixture consisting of 0.5 g of stearic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified Ge-NPs with stearic acid.
  • Ge-NPs of Preparation Example 7 100 mg were dispersed in a mixture of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and ultrasonic waves were irradiated for 5 minutes to prepare Ge-NPs surface-modified with acetylsalicylic acid.
  • Ge-NPs of Preparation Example 7 were dispersed in 25 ml of an aqueous boric acid solution (mixed at 5 parts by weight of boric acid and distilled water), and ultrasonically irradiated for 5 minutes to prepare surface-modified Ge-NPs with a hydroxyl group of boric acid.
  • Ge-NPs of Preparation Example 7 were dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride were mixed at 1: 1 parts by weight), and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified Ge-NPs with a hydroxyl group of water.
  • an aqueous organic solvent solution water and methylene chloride were mixed at 1: 1 parts by weight
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with a methoxy group.
  • GeB 4 -NPs of Preparation Example 8 100 mg was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with an ethoxy group.
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in 25 ml of isopropyl alcohol, and ultrasonic waves were irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with isopropoxy.
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in 25 ml of 2-aminoalcohol, and ultrasonic waves were irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with 2-aminoalkoxy groups.
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in a mixture of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with butylphenoxy group.
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and ultrasonic waves were irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with an acetic acid.
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in a mixture consisting of 0.5 g of stearic acid and 25 ml of dichloromethane, and ultrasonic waves were irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with stearic acid.
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in a mixture consisting of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with acetylsalicylic acid.
  • GeB 4 -NPs of Preparation Example 8 100 mg were dispersed in 25 ml of an aqueous boric acid solution (boric acid and distilled water mixed at 5:95 parts by weight), and ultrasonically irradiated for 5 minutes to prepare GeB 4 -NPs that were surface-modified with a hydroxyl group of boric acid. It was.
  • GeC-NPs of Preparation Example 9 100 mg was dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare GeC-NPs surface-modified with a methoxy group.
  • GeC-NPs of Preparation Example 9 100 mg was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare GeC-NPs surface-modified with an ethoxy group.
  • GeC-NPs of Preparation Example 9 100 mg was dispersed in 25 ml of isopropyl alcohol, and ultrasound was irradiated for 5 minutes to prepare GeC-NPs surface-modified with isopropoxy group.
  • GeC-NPs of Preparation Example 9 100 mg were dispersed in 25 ml of 2-aminoalcohol, and ultrasonic waves were irradiated for 5 minutes to prepare GeC-NPs surface-modified with 2-aminoalkoxy groups.
  • GeC-NPs of Preparation Example 9 100 mg was dispersed in a mixture consisting of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified GeC-NPs with butylphenoxy group.
  • GeC-NPs of Preparation Example 9 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified GeC-NPs with an acetic acid.
  • GeC-NPs of Preparation Example 9 100 mg were dispersed in a mixture consisting of 0.5 g of stearic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare surface-modified GeC-NPs with stearic acid.
  • GeC-NPs of Preparation Example 9 100 mg were dispersed in a mixture consisting of 0.1 g of acetylsalicylic acid and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare GeC-NPs surface-modified with acetylsalicylic acid.
  • GeC-NPs of Preparation Example 9 100 mg were dispersed in 25 ml of an aqueous boric acid solution (mixed at 5 parts by weight of boric acid and distilled water), and ultrasonically irradiated for 5 minutes to prepare surface-modified GeC-NPs with a hydroxyl group of boric acid.
  • GeC-NPs of Preparation Example 9 100 mg were dispersed in 25 ml of an aqueous organic solvent solution (water and methylene chloride were mixed at 1: 1 parts by weight), and ultrasonically irradiated for 5 minutes to prepare surface-modified GeC-NPs with a hydroxyl group of water.
  • an aqueous organic solvent solution water and methylene chloride were mixed at 1: 1 parts by weight
  • CB 4 -NPs of Preparation Example 10 100 mg was dispersed in a mixture consisting of 0.5 ml of butylphenol and 25 ml of dichloromethane, and ultrasonically irradiated for 5 minutes to prepare CB 4 -NPs surface-modified with butylphenoxy group.
  • CB 4 -NPs of Preparation Example 10 100 mg was dispersed in a mixture consisting of 0.5 ml of acetic acid and 25 ml of dichloromethane, and ultrasonic waves were irradiated for 5 minutes to prepare CB 4 -NPs surface-modified with an acetic acid.
  • CB 4 -NPs of Preparation Example 10 100 mg was dispersed in a mixture consisting of 0.5 g of stearic acid and 25 ml of dichloromethane, and ultrasonic wave was irradiated for 5 minutes to prepare CB 4 -NPs surface-modified with stearic acid.
  • examples with water By diluting the carbon group non-oxide nanoparticles prepared by the preparation examples, examples with water to prepare an antimicrobial composition having a concentration of the carbon group non-oxide nanoparticles 2mM / L.
  • an antimicrobial composition having a concentration of the carbon group non-oxide nanoparticles 2mM / L.
  • the antimicrobial performance against bacteria A Staphylococcus aureus ATCC 6538
  • bacteria B Klebsiella pneumoniae ATCC 4352
  • Comparative Example 1 in Table 1 to Table 4 shows the results of the antimicrobial test through silica (SiO 2 , Aldrich) nanoparticles. Specifically, the silica nanoparticles were prepared in a 10ppm solution and sprayed onto the shoe insole, followed by antimicrobial treatment.
  • Comparative Example 2 is a result of the antibacterial test through zinc oxide (ZnO, Aldrich) nanoparticles. Specifically, the zinc oxide nanoparticles were prepared as a 10ppm solution and sprayed onto a shoe insole, resulting in antibacterial treatment after drying.
  • the antimicrobial effect through the nanoparticles according to the preparation examples and examples of the present invention showed the antibacterial effect of the first 95.8%, up to 99.9%, which is Comparative Example 1 And it can be seen that the numerical value is significantly higher than the antibacterial test results according to Comparative Example 2.

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Abstract

Un mode de réalisation de l'invention concerne : un agent antimicrobien contenant des nanoparticules non oxydiques du groupe carbone dotées d'une taille de particule moyenne comprise entre 5 et 400 nm ; et un procédé de production associé.
PCT/KR2017/005748 2016-06-01 2017-06-01 Agent antimicrobien contenant des nanoparticules non oxydiques du groupe carbone et procédé de production associé Ceased WO2017209545A1 (fr)

Priority Applications (4)

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JP2019515756A JP6782836B2 (ja) 2016-06-01 2017-06-01 炭素族非酸化物ナノ粒子を含む抗菌剤およびその製造方法
EP17807038.9A EP3466263A1 (fr) 2016-06-01 2017-06-01 Agent antimicrobien contenant des nanoparticules non oxydiques du groupe carbone et procédé de production associé
CN201780033856.0A CN109310084A (zh) 2016-06-01 2017-06-01 包含碳族非氧化物纳米粒子的抗菌剂及其制备方法
US16/306,339 US20190159459A1 (en) 2016-06-01 2017-06-01 Antimicrobial agent comprising carbon-group non-oxide nanoparticles, and production method therefor

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5985175A (en) * 1998-08-19 1999-11-16 Osram Sylvania Inc. Boron oxide coated phosphor and method of making same
KR20050084212A (ko) * 2005-06-09 2005-08-26 이튼 나노베이션 게엠베하 나노크기 코어/쉘 입자 및 그의 제조방법
KR20070098781A (ko) * 2004-10-04 2007-10-05 라이브니츠-인스티투트 퓌어 노이에 마테리알리엔 게마인누찌게 게엠베하 맞춤형 표면 화학을 갖는 나노입자 및 상응하는 콜로이드의제조방법
KR100836260B1 (ko) * 2007-01-05 2008-06-10 연세대학교 산학협력단 상압조건하의 결정성 탄소 나노입자 생성 방법
WO2010015801A2 (fr) * 2008-08-04 2010-02-11 Intrinsiq Materials Limited Composition biocide
KR101724415B1 (ko) * 2016-03-10 2017-04-11 주식회사 쇼나노 실리콘 항균제 조성물 및 그 제조방법

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5985175A (en) * 1998-08-19 1999-11-16 Osram Sylvania Inc. Boron oxide coated phosphor and method of making same
KR20070098781A (ko) * 2004-10-04 2007-10-05 라이브니츠-인스티투트 퓌어 노이에 마테리알리엔 게마인누찌게 게엠베하 맞춤형 표면 화학을 갖는 나노입자 및 상응하는 콜로이드의제조방법
KR20050084212A (ko) * 2005-06-09 2005-08-26 이튼 나노베이션 게엠베하 나노크기 코어/쉘 입자 및 그의 제조방법
KR100836260B1 (ko) * 2007-01-05 2008-06-10 연세대학교 산학협력단 상압조건하의 결정성 탄소 나노입자 생성 방법
WO2010015801A2 (fr) * 2008-08-04 2010-02-11 Intrinsiq Materials Limited Composition biocide
KR101724415B1 (ko) * 2016-03-10 2017-04-11 주식회사 쇼나노 실리콘 항균제 조성물 및 그 제조방법

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