WO2017209545A1 - Antimicrobial agent comprising carbon-group non-oxide nanoparticles, and production method therefor - Google Patents

Antimicrobial agent comprising carbon-group non-oxide nanoparticles, and production method therefor 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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carbon
preparation example
irradiated
group
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PCT/KR2017/005748
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Korean (ko)
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조원일
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주식회사 쇼나노
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Priority claimed from KR1020170035634A external-priority patent/KR101804570B1/en
Application filed by 주식회사 쇼나노 filed Critical 주식회사 쇼나노
Priority to JP2019515756A priority Critical patent/JP6782836B2/en
Priority to CN201780033856.0A priority patent/CN109310084A/en
Priority to US16/306,339 priority patent/US20190159459A1/en
Priority to EP17807038.9A priority patent/EP3466263A1/en
Publication of WO2017209545A1 publication Critical patent/WO2017209545A1/en

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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
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/358—Inorganic compounds
    • 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.

Abstract

One embodiment of the present invention provides: an antimicrobial agent comprising carbon-group non-oxide nanoparticles having an average particle size of 5-400 nm; and a production method therefor.

Description

탄소족 비산화물 나노입자를 포함하는 항균제 및 그 제조방법Antimicrobial agent containing carbon group non-oxide nanoparticles and preparation method thereof
본 발명은 탄소족 비산화물 나노입자를 포함하는 항균제 및 그 제조방법에 관한 것이다.The present invention relates to an antimicrobial agent comprising carbon group non-oxide nanoparticles and a method for producing the same.
탄소족(4A족 또는 14족) 원소 나노입자는 차세대 실리콘기반 광전자 소자(optoelectronic device)로서의 응용과 나노 소자 개발의 핵심 요소로 많은 연구자들에게 높은 관심의 대상이 되고 있는데, 탄소족 나노입자는 디스플레이의 전계효과 트랜지스터(TFT), PN정션을 이용한 태양전지, 다이오드 및 생체의 표시제 등으로 그 응용범위가 매우 넓다.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.
종래에는 탄소족 중 하나인 실리콘 나노입자를 제조하는 가장 일반적인 방법으로 실리콘 테트라클로라이드, 실리콘 트리에틸오소실리케이트와 같은 실리콘 소스를 화학적인 방법으로 환원하는 방법이 이용되었는데, 이 방법은 실리콘 나노입자의 과도한 캡핑, 실리콘 나노입자의 산화 및 소결과정 후의 탄소 등의 분순물이 잔존하는 문제가 있다.Conventionally, the most common method of preparing silicon nanoparticles, which is one of the carbon groups, has been a method of chemically reducing silicon sources such as silicon tetrachloride and silicon triethyl orthosilicate, which is an excessive amount of silicon nanoparticles. There is a problem that impurities such as carbon after capping, oxidation and sintering of silicon nanoparticles remain.
이러한 문제점을 해결하기 위해 vapor-liquid-solid (VLS) 또는 solid-liquid-solid (SLS)에 의해 실리콘 소스를 증착하는 방법이 이용되고 있으나, 이 방법 또한 실리콘 소스가 높은 압력, 높은 온도에서 증착되어 반응조건이 가혹할 뿐만 아니라 핸들링이 어렵고 고가인 장비가 필요하며, 실리콘 나노입자의 수율도 낮은 문제가 있다.In order to solve this problem, a method of depositing a silicon source by vapor-liquid-solid (VLS) or solid-liquid-solid (SLS) is used, but this method is also used to deposit a silicon source at high pressure and high temperature. In addition to harsh reaction conditions, handling is difficult and expensive equipment is required, and the yield of silicon nanoparticles is low.
한편, 종래에는 실리콘과 같은 탄소족 나노입자는 주로 전자제품 등에 적용되었으며, 탄소족 나노입자의 표면을 개질하여 항균제로 사용한 예는 없었다.Meanwhile, conventionally, 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.
<선행기술문헌><Preceding technical literature>
<특허문헌><Patent Documents>
(특허문헌 0001) 한국특허공개 제10-2012-0010901호(2012.02.06)(Patent Document 0001) Korean Patent Publication No. 10-2012-0010901 (2012.02.06)
(특허문헌 0002) 한국특허공개 제10-2014-0072663호(2014.06.13)(Patent Document 0002) Korean Patent Publication No. 10-2014-0072663 (2014.06.13)
본 발명은 전술한 종래 기술의 문제점을 해결하기 위한 것으로, 본 발명의 목적은 소량으로도 우수한 항균 효과를 나타내며, 제조공정이 간소하여 제조비용이 저렴한 탄소족 비산화물 나노입자를 포함하는 항균제 및 그 제조방법을 제공하는 것이다.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.
본 발명의 일 측면은, 평균 입도가 5~400nm인 탄소족 비산화물 나노입자를 포함하는 항균제를 제공한다.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.
본 발명의 탄소족 비산화물 나노입자는 종래 유기 항균제와 버금가는 현저히 우수한 항균 효과를 나타낸다는 것을 발견하고 본 발명을 완성하였다.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.
본 명세서에 사용된 용어, "탄소족 비산화물 나노입자"는 C, Si, Ge, Sn 중 적어도 하나의 탄소족(14족) 원소를 포함하고, 필요에 따라, B를 더 포함하는 입자를 의미하며, 이종의 탄소족 원소가 합금되거나 적어도 하나의 탄소족 원소에 붕소(B)가 합금된 입자, 이종의 탄소족 원소로 이루어진 화합물, 및 탄소족 원소와 붕소로 이루어진 화합물를 포함하는 개념으로 이해될 수 있다.As used herein, the term "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.
예를 들어, 상기 탄소족 비산화물 나노입자는 Si 나노입자, Si/B 합금 나노입자, SiBx 나노입자, Si/C 합금 나노입자, Si/Ge 합금 나노입자, Si/Ge/B 합금 나노입자, Si/Ge/C 합금 나노입자, Ge 나노입자, Ge/B 합금 나노입자, GeBx 나노입자, Ge/C 합금 나노입자, C/B 합금 나노입자, CB4 나노입자, Sn 나노입자일 수 있다.For example, 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.
본 명세서에 사용된 용어, "비산화물 나노입자"는 실질적으로 산소 원소(O)를 포함하지 않는 입자를 의미하며, 자연적으로 발생한 산화반응에 의해 비산화물 나노입자의 표면에 생성된 산화물층(oxide layer, 제1 산화물층)을 포함하는 개념으로 이해될 수 있다.As used herein, the term "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).
상기 제1 산화물층의 두께는 바람직하게는, 1nm일 수 있다. 상기 제1 산화물층이 1nm 이하의 두께로 형성된 탄소족 비산화물 나노입자는 알코올, 카르복실산, 물 등과의 반응성이 높기 때문에, 표면이 알콕시기, 카르복실기, 하이드록실기로 개질되는 효율성이 향상되며 입자 간의 전기적 반발력에 의한 분산성이 우수하다. Preferably, 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.
상기 탄소족 비산화물 나노입자의 항균 효과는 다음과 같은 메커니즘에 의해 구현될 수 있다. 먼저, 세균의 표면에는 항원물질이 존재하는데 실리콘 나노입자 등의 탄소족 비산화물 나노입자가 이러한 세균에 접촉, 흡착하게 되면 항원물질이 응집원으로 작용하여 그들에 대한 항체인 응집소화 결합하여 군집을 이루게 된다. 세균 표면에 흡착된 탄소족 비산화물 나노입자는 세균의 인지질 운동(수축, 팽창)에 의해 세균 내부로 침투하여 세균의 사멸이 일어날 수 있다. 또한, 상기 탄소족 비산화물 나노입자는 세균의 생존에 필요한 영양소로 작용할 수 있다. 세균은 무기 영양소를 섭취하기 위해 세균이 군집된 인지질은 수축과 팽창을 반복하면서 탄소족 비산화물 나노입자를 흡수하려 하지만 나노입의 크기로 인해 인지질 사이에 걸리게 된다. 그렇게 되면 인지질 사이의 간극이 서서히 증가하여 세균 내부의 전해질 등이 외부로 배출되어 세균의 사멸이 일어날 수 있다.The antimicrobial effect of the carbon group non-oxide nanoparticles can be implemented by the following mechanism. First, antigens exist on the surface of bacteria. When carbon-based non-oxide nanoparticles, such as silicon nanoparticles, come into contact with and adsorb these bacteria, 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. In addition, 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.
상기 탄소족 비산화물 나노입자의 평균 입도는 5~400nm일 수 있다. 상기 탄소족 비산화물 나노입자의 평균 입도가 5nm 미만이면 나노입자 제조 시 임의적인 입자 응집이 발생할 수 있고, 400nm 초과이면 상기 메커니즘에 따른 세포 사멸 효과를 구현할 수 없다.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.
도 1 내지 도 4는 본 발명의 일 실시예에 따른 실리콘 비산화물 나노입자로 이루어진 항균제를 50ppm 황색포도상구균과 접촉시키기 전, 접촉 직후, 항균 처리 24시간 후의 SEM 이미지이다.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.
도 2에서 황색포도상구균에 항균 처리 직후 실리콘 비산화물 나노입자가 세균에 접촉, 흡착되는 모습을 볼 수 있고, 도 3에서 항균 처리 후 황색포도상구균이 사멸된 모습을 확인할 수 있다. 또한, 도 4를 통해 항균 처리 전과 24시간 후의 결과를 비교해보면, 항균 처리 전 황색포도상구균은 500nm의 구형을 가지지만, 항균 처리 후 실리콘 비산화물 나노입자가 접촉, 흡착되면서 구형이 찌그러지고 세균이 사멸되었다.In FIG. 2, immediately after the antibacterial treatment with Staphylococcus aureus, the silicon non-oxide nanoparticles are contacted with and adsorbed to the bacteria. In FIG. 3, the Staphylococcus aureus is killed after the antibacterial treatment. In addition, when comparing the results before and after the antimicrobial treatment 24 hours through Figure 4, before the antimicrobial 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.
또한, 상기 탄소족 비산화물 나노입자는 입자의 표면에 일정 두께, 예를 들어, 100nm 이하, 바람직하게는, 1~100nm, 더 바람직하게는, 1~10nm의 탄소층이 형성된 나노입자일 수 있다. 상기 탄소층은 탄소족 비산화물 나노입자와 공기의 접촉에 의한 과산화 및 그에 따른 상기 제1 산화물층의 후막화를 방지하여 탄소족 비산화물 나노입자의 항균 성능이 안정적으로 구현되도록 한다. 상기 탄소층의 두께가 1nm 미만이면 나노입자와 공기의 접촉을 적절히 차단하기 어렵고, 100nm 초과이면 나노입자가 과도하게 비대해져 상기 메커니즘에 따른 세포 사멸 효과를 구현할 수 없다.In addition, 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. If 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.
한편, 상기 제1 산화물층의 표면에 결합된 카르복실기, 하이드록실기 및 알콕시기로 이루어진 군에서 선택된 하나 이상의 작용기를 더 포함할 수 있다.On the other hand, 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.
상기 카르복실기, 하이드록실기, 알콕시기는 상기 탄소족 비산화물 나노입자를 알코올, 카르복실산, 붕산 수용액, 물 등으로 처리함으로써 상기 탄소족 비산화물 나노입자의 표면, 구체적으로, 상기 제1 산화물층의 표면에 결합될 수 있다.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.
상기 작용기가 표면에 결합된 탄소족 비산화물 나노입자는 우수한 항균 효과를 나타낼 뿐만 아니라, 제조공정이 간소화되며, 소량의 사용으로도 우수한 항균 효과를 나타내기 때문에, 각종 전자제품, 의류, 가방 및 신발 등과 같은 다양한 제품에 대해 우수한 도포력 가지므로 범용성, 안정성이 우수하다.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.
상기 제1 산화물층의 표면에 형성된 붕소 산화물로 이루어진 제2 산화물층을 더 포함할 수 있다. 상기 제2 산화물층은 탄소족 비산화물 나노입자와 공기의 접촉에 의한 과산화 및 그에 따른 상기 제1 산화물층의 후막화를 방지하여 탄소족 비산화물 나노입자의 항균 성능이 안정적으로 구현되도록 한다.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.
필요에 따라, 상기 항균제는 물 등에 의해 일정 농도, 예를 들어, 1~1,000ppm의 농도로 희석된 용액의 형태로 제공될 수 있으나, 상기 항균제가 희석될 수 있는 매질의 종류는 특별히 제한되지 않는다.If necessary, 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. .
도 5를 참고하면, 본 발명의 다른 일 측면은, (a) 제1 산화물층이 형성된 탄소족 비산화물 나노입자를 제조하는 단계; (b1) 상기 탄소족 비산화물 나노입자를 알코올, 카르복실산, 붕산 수용액 및 물로 이루어진 군에서 선택된 하나와 혼합하여 혼합액을 제조하는 단계; 및 (c1) 상기 혼합액에 초음파를 인가하는 단계;를 포함하는 항균제의 제조방법을 제공한다.Referring to Figure 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.
도 6을 참고하면, 본 발명의 다른 일 측면은, (a) 제1 산화물층이 형성된 탄소족 비산화물 나노입자를 제조하는 단계; (b2) 상기 탄소족 비산화물 나노입자를 붕산 및 유기용매를 포함하는 제1 용액과 혼합하여 제1 혼합액을 제조하는 단계; (c2) 상기 제1 혼합액에 초음파를 인가하여 상기 제1 산화물층 상에 붕소 산화물로 이루어진 제2 산화물층이 형성된 탄소족 비산화물 나노입자를 수득하는 단계; (d) 상기 탄소족 비산화물 나노입자를 알코올, 카르복실산, 붕산 수용액 및 물로 이루어진 군에서 선택된 하나와 혼합하여 제2 혼합액을 제조하는 단계; 및 (e) 상기 제2 혼합액에 초음파를 인가하는 단계;를 포함하는 항균제의 제조방법을 제공한다.Referring to Figure 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.
상기 (a) 단계는 탄소족 원소를 포함하는 하나 이상의 원료가스와 육불화황 촉매가스를 포함하는 혼합가스에 레이저를 조사하여 이루어질 수 있다.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.
상기 (b) 단계에서 사용 가능한 알코올, 카르복실산은 1,10-데칸디올, 1,2-프로판디올, 1,2-헥산디올, 1,4-부탄디올, 1,5-펜탄디올, 1,8-옥탄디올, 1-데카놀, 2,2,4-트리메틸펜탄디올, 2-부톡시에탄올, 2-브로모펜탄산, 2-브로모헥사데칸산, 2-브로모헥산산, 2-에틸헥사노익산, 2-클로로부탄산, 2-프로판디올, 2-프로펜산, 2-하이드록시에틸메타크릴레이트, DHA, 갈라타민, 갈락토스, 갈란타민, 구연산, 글라이신, 글루코네이트, 글루코스, 글루타르산, 글루타민, 글리세롤, 글리시레틴산, 글리시리진산디칼륨, 글리신, 나트륨글루코네이트, 나트륨카르복시메틸셀룰로오스, 네오마이신설페이트, 네오펜틸글리콜, 독소루비신, 디글리세리드, 디에틸렌글리콜, 디프로필렌글리콜, 라놀린, 락트산, 레티놀, 리놀레산, 말레산, 메타크릴산, 메탄올, 메톡시프로판올, 메트포민, 메틸렌클로라이드, 멘톨, 모노글리세리드, 미네랄오일, 바세린, 베타페닐에틸알코올, 벤조산, 벤질알코올, 부탄올, 부틸페놀, 뷰티르산, 뷰틸하이드록시아니솔(BHA), 브로멜라인, 비스페놀A, 비타민C, 비타민D, 사이클로파이록스, 생리식염수, 세라펩타제, 세테아릴알코올, 세틸알코올, 셀룰로오스, 소듐시트레이트, 소르비톨, 소팔콘, 스테아르산, 스테아릴알코올, 아디프산, 아디핀산, 아릴알코올, 아미노레불린산, 아미노알코올, 아세클로페낙, 아세클로페낙산, 아세트산, 아세트아미노펜, 아세틸살리실산, 아졸렌, 알긴산, 일라이트, 알렌드론산, 에르고스테롤, 에탄올, 에틸렌글리콜, 에틸렌비닐알코올, 옥탄올, 유제놀, 이부프로펜, 이소펜틸디올, 이소프로필알코올, 이소프탈산, 이타콘산, 자일리톨, 카르바조크롬, 카사트리올, 크로틸알코올, 클로록실레놀, 클로베타솔프로피오네이트, 타닌산, 테레프탈산, 트라넥삼산, 트리암시놀론아세토나이드, 티몰, 팔미톨레산, 페녹시에탄올, 펙틴, 펜타에리스리톨, 폴리아크릴산암모늄염, 폴리에스터폴리올, 폴리에틸렌글리콜, 푸시딘산, 프레도니솔론, 프로판올, 프로폴리스, 프로피온산, 프로필렌글리콜, 피로피론산, 피브로인, 헤파린, 헥산디올산, 후루벤다졸, 히노키티올, 및 히알루론산으로 이루어진 군에서 선택된 하나 이상일 수 있으나, 이에 한정되는 것은 아니다.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, glycyrrhizin acid potassium, glycine, sodium gluconate, sodium carboxymethyl cellulose, neomycin sulfate, neopentyl glycol, doxorubicin, diglyceride, diethylene glycol, dipropylene glycol, lanolin, lactic acid, Retinol, linoleic acid, maleic acid, methacrylic acid, methanol, methoxypropanol, metformin, Lene chloride, menthol, monoglycerides, mineral oil, petrolatum, betaphenylethyl alcohol, benzoic acid, benzyl alcohol, butanol, butylphenol, butyric acid, butylhydroxyanisole (BHA), bromelain, bisphenol A, vitamin C, Vitamin D, cyclopyrox, physiological saline, cerapeptase, cetearyl alcohol, cetyl alcohol, cellulose, sodium citrate, sorbitol, sofalcone, stearic acid, stearyl alcohol, adipic acid, adipic acid, aryl alcohol, Aminolevulinic acid, aminoalcohol, aceclofenac, aceclofenacic acid, acetic acid, acetaminophen, acetylsalicylic acid, azolene, alginic acid, illite, alendronic acid, ergosterol, ethanol, ethylene glycol, ethylene vinyl alcohol, octanol, eugenol , Ibuprofen, isopentyldiol, isopropyl alcohol, isophthalic acid, itaconic acid, xylitol, carbazochrome, castriol, crotyl alcohol, chloroxylenol , Clobetasolpropionate, tannic acid, terephthalic acid, tranexamic acid, triamcinolone acetonide, thymol, palmitoleic acid, phenoxyethanol, pectin, pentaerythritol, ammonium polyacrylate salt, polyester polyol, polyethylene glycol, fudic acid, prepre It may be one or more selected from the group consisting of donisolone, propanol, propolis, propionic acid, propylene glycol, pyropyonic acid, fibroin, heparin, hexanediolic acid, furbendazole, hinokithiol, and hyaluronic acid, but is not limited thereto. .
상기 (a) 단계 이후에 상기 탄소족 비산화물 나노입자 및 탄소계 가스, 예를 들어, 아세틸렌 가스 또는 에틸렌 가스를 포함하는 혼합물에 레이저를 조사하여 상기 탄소족 비산화물 나노입자의 표면에 탄소층을 형성하는 단계를 더 포함할 수 있다.After the 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.
상기 (b2) 단계에서 상기 유기용매는 비극성일 수 있다. 상기 유기용매가 비극성인 경우 하기 반응식 A에 따라 상기 (c2) 단계에서 상기 제1 산화물층의 상에 붕소 산화물로 이루어진 제2 산화물층이 생성될 수 있다. 반면, 상기 (b2) 단계에서 물과 같은 극성 용매에 용해된 붕산 용액을 처리하는 경우 붕소 산화물로 이루어진 추가의 산화물층이 생성되는 것이 아니라, 붕산 유래의 하이드록실기가 상기 제1 산화물층의 표면에 결합하게 된다.In the step (b2), the organic solvent may be nonpolar. When the organic solvent is non-polar, 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. On the other hand, when 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. To be bound to
<반응식 A>Scheme A
나노입자 + B(OH)3 → 나노입자-OB(OH)2 + 1/2 H2 Nanoparticle + B (OH) 3 → Nanoparticle-OB (OH) 2 + 1/2 H 2
→ 나노입자(-O)2BOH + 2/2 H2 ¡Æ nanoparticles (-O) 2 BOH + 2/2 H 2
→ 나노입자(-O)3B + 3/2 H2 ¡Æ nanoparticles (-O) 3 B + 3/2 H 2
상기 (c1) 또는 (c2) 단계에서 일정 시간, 예를 들어, 4~6분 간 초음파를 인가함으로써 상기 탄소족 비산화물 나노입자의 표면에 작용기를 결합시킬 수 있다.In the step (c1) or (c2), 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.
상기 초음파에 의해 상기 탄소족 비산화물 나노입자의 표면이 알콕시기로 개질되는 과정은 하기 반응식 B와 같다.The process of modifying the surface of the carbon group non-oxide nanoparticles by the ultrasonic wave is an alkoxy group, as shown in Scheme B below.
<반응식 B>Scheme B
나노입자 + nROH → 나노입자-(O-R)n + n/2H2↑Nanoparticle + nROH → nanoparticle- (OR) n + n / 2H 2 ↑
(R은 알킬기 또는 알킬케톤기, 아로마틱 또는 아로마틱 케톤기임)(R is an alkyl or alkyl ketone group, aromatic or aromatic ketone group)
상기 초음파의 조사시간이 4분 미만이면 탄소족 비산화물 나노입자의 표면에 대한 작용기의 결합 효율이 저하될 수 있고, 6분 초과이면 필요 이상의 초음파가 인가되므로 에너지 효율이 저하될 수 있다.If the irradiation time of the ultrasonic wave is less than 4 minutes, 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.
상기 초음파의 주파수는 특별히 한정되지 않고, 통상적으로 사용되는 초음파의 주파수라면 어떠한 것이든 사용가능하나, 20~100kHz 주파수 범위의 초음파를 사용하는 것이 바람직하다.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.
본 발명의 일 측면에 따른 항균제 및 그 제조방법은 우수한 항균 효과를 나타내는 항균제 조성물을 제공하며, 산화층이 얇게 형성된 탄소족 비산화물 나노입자가 사용되어 분산제나 별도의 첨가제를 사용할 필요가 없기 때문에, 제조비용이 저렴하며 제조공정이 간소화되는 탁월한 효과를 나타낸다.According to an aspect of the present invention, 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.
또한, 소량으로도 우수한 항균 효과를 나타내는 작용기 치환된 탄소족 비산화물 나노입자를 함유하는 항균제는 표면장력이 낮고 도포력이 우수하기 때문에, 각종 전자제품, 의류, 가방 및 신발 등과 같은 다양한 제품에 적용될 수 있고, 신약개발이나 수지, 화장품 등에도 사용될 수 있다. In addition, 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.
본 발명의 효과는 상기한 효과로 한정되는 것은 아니며, 본 발명의 상세한 설명 또는 청구범위에 기재된 발명의 구성으로부터 추론 가능한 모든 효과를 포함하는 것으로 이해되어야 한다.It is to be understood that the effects of the present invention are not limited to the above effects, and include all effects deduced from the configuration of the invention described in the detailed description or claims of the present invention.
도 1은 본 발명의 일 실시예에 따른 항균제와 황색포도상구균을 접촉시키기 전의 SEM 이미지이다.1 is a SEM image before contacting the antibacterial agent and Staphylococcus aureus according to an embodiment of the present invention.
도 2는 본 발명의 일 실시예에 따른 항균제와 황색포도상구균을 접촉시킨 직후의 SEM 이미지이다.Figure 2 is an SEM image immediately after contact with the antibacterial agent and Staphylococcus aureus according to an embodiment of the present invention.
도 3은 본 발명의 일 실시예에 따른 항균제와 황색포도상구균을 접촉시킨 후 24시간 경과 후의 SEM 이미지이다.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.
도 4는 본 발명의 일 실시예에 따른 항균제와 황색포도상구균의 접촉 전 및 24시간 접촉 후를 대비한 SEM 이미지이다.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.
도 5는 본 발명의 일 실시예에 따른 항균제의 제조방법을 도식화한 것이다.5 is a schematic diagram illustrating a method for preparing an antimicrobial agent according to an embodiment of the present invention.
도 6은 본 발명의 다른 일 실시예에 따른 항균제의 제조방법을 도식화한 것이다.6 is a schematic diagram illustrating a method for preparing an antimicrobial agent according to another embodiment of the present invention.
도 7은 본 발명의 일 실시예에 따른 실리콘 나노입자의 TEM 이미지이다.7 is a TEM image of silicon nanoparticles according to an embodiment of the present invention.
이하에서는 첨부한 도면을 참조하여 본 발명을 설명하기로 한다. 그러나 본 발명은 여러 가지 상이한 형태로 구현될 수 있으며, 따라서 여기에서 설명하는 실시예로 한정되는 것은 아니다. 그리고 도면에서 본 발명을 명확하게 설명하기 위해서 설명과 관계없는 부분은 생략하였다.Hereinafter, with reference to the accompanying drawings will be described the present invention. As those skilled in the art would realize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. In the drawings, parts irrelevant to the description are omitted in order to clearly describe the present invention.
명세서 전체에서, 어떤 부분이 다른 부분과 "연결"되어 있다고 할 때, 이는 "직접적으로 연결"되어 있는 경우뿐 아니라, 그 중간에 다른 부재를 사이에 두고 "간접적으로 연결"되어 있는 경우도 포함한다. 또한 어떤 부분이 어떤 구성요소를 "포함"한다고 할 때, 이는 특별히 반대되는 기재가 없는 한 다른 구성요소를 제외하는 것이 아니라 다른 구성요소를 더 구비할 수 있다는 것을 의미한다.Throughout the specification, when a part is "connected" to another part, it includes not only "directly connected" but also "indirectly connected" with another member in between. . In addition, when a part is said to "include" a certain component, this means that it may further include other components, without excluding the other components unless otherwise stated.
이하, 본 발명의 실시예에 관해 상세히 설명하기로 한다.Hereinafter, embodiments of the present invention will be described in detail.
제조예 1Preparation Example 1
실리콘 나노입자는 하기 반응식 1 중 (1) 또는 (2)에 따라 제조될 수 있다.Silicon nanoparticles can be prepared according to (1) or (2) in Scheme 1 below.
<반응식 1><Scheme 1>
(1) SiH4 + SF6 + N2 → Si (-S, -F) + H2 + N2 (1) SiH 4 + SF 6 + N 2 → Si (-S, -F) + H 2 + N 2
(2) SiH4 + N2 → Si + 2H2 + N2 (2) SiH 4 + N 2 → Si + 2H 2 + N 2
원료가스 공급노즐을 통해 원료가스인 모노실란(SiH4) 100 부피부, 제어가스인 질소(N2) 400 부피부, 및 육불화황(SF6) 촉매가스 40 부피부를 혼합한 혼합가스를 내부 압력이 500torr인 반응챔버 내부로 공급하고, 반응챔버 내부로 공급된 혼합가스에 CO2 레이저 발생기에서 발생시킨 레이저를 레이저 조사부를 통해 파장이 10.6㎛인 연속파의 라인 빔(Line Beam) 형태로 3시간 동안 조사하여 산화층이 형성된 실리콘 나노입자(Si-NPs)를 제조하였다.Through a feed gas supply nozzle, 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㎛ through the laser irradiation unit. Irradiation for a time to produce a silicon nanoparticles (Si-NPs) in which the oxide layer was formed.
도 7을 참고하면, 제조된 산화층이 형성된 실리콘 나노입자의 평균 입도는 5~400nm이고, 산화층의 두께는 0.32nm이며, 생성수율은 97.1%이다.Referring to FIG. 7, 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%.
제조예 2Preparation Example 2
실리콘-붕소 합금 나노입자 또는 붕화규소 나노입자는 하기 반응식 2에 따라 제조될 수 있다.Silicon-boron alloy nanoparticles or silicon boride nanoparticles may be prepared according to Scheme 2 below.
<반응식 2><Scheme 2>
2SiH4 + 2B2H6 + N2 → SiB4 + 8H2 + N2 2SiH 4 + 2B 2 H 6 + N 2 → SiB 4 + 8H 2 + N 2
모노실란(SiH4), 디보레인(B2H6), 질소를 혼합하여 반응챔버 내부로 주입하여 CO2 레이저빔을 조사시킨다. 이 때, 디보레인은 촉매가스 및 원료가스로 작용하며, 10.6㎛ 파장에서 흡수한 에너지가 효율적으로 모노실란으로 전달되고, 모노실란의 Si-H 결합이 잘 끊어지도록 하여 실리콘-붕소 합금 나노입자(SiBx-NPs)를 생성시킨다.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. At this time, the diborane acts as a catalyst gas and a source gas, the energy absorbed at 10.6㎛ 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.
또한, 디보레인은 붕소와 수소 원자로 분해되어 붕소는 실리콘 나노입자와 합금을 이루며, 실리콘의 산화를 방지한다. 원료가스인 모노실란은 전체 부피(원료가스 및 촉매가스를 합친 부피)의 90%이상 이고, 촉매가스는 전체 부피의 10% 이하의 범위로 조절한다. 또한, 캐리어가스인 질소는 원료가스인 모노실란 대비 400 부피부를 넘지 않도록 한다. 가스의 유량은 sccm 단위를 사용한다. 반응챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 평균 입도가 5~400nm이고, 산화층의 두께가 0.57nm인 실리콘-붕소 합금 나노입자(SiBx-NPs)가 제조된다.In addition, 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. In addition, 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.
제조예 3Preparation Example 3
실리콘-탄소 합금 나노입자 또는 탄화규소 나노입자는 하기 반응식 3 중 (1) 또는 (2)에 따라 제조될 수 있다.Silicon-carbon alloy nanoparticles or silicon carbide nanoparticles can be prepared according to (1) or (2) in Scheme 3 below.
<반응식 3><Scheme 3>
(1) 2SiH4 + C2H2 + SF6 → S + 2SiC + 6HF + 2H2 (1) 2SiH 4 + C 2 H 2 + SF 6 → S + 2SiC + 6HF + 2H 2
(2) 2SiH4 + C2H2 → 2SiC + 5H2 (2) 2SiH 4 + C 2 H 2 → 2SiC + 5H 2
모노실란(SiH4), 아세틸렌(C2H2), 질소를 혼합하여 반응챔버 내부로 주입하여 CO2 레이저빔을 조사시킨다. 아세틸렌은 탄소와 수소 원자로 분해되어 탄소는 실리콘 나노입자와 합금을 이루며, 실리콘의 산화를 방지한다. 원료가스인 모노실란 및 아세틸렌은 각각 2 : 1의 부피비로 주입된다.~또한, 캐리어가스인 질소는 원료가스인 모노실란 대비 400 부피부를 넘지 않도록 한다. 가스의 유량은 sccm 단위를 사용한다.~반응챔버 내부의 공정압력은 100~500torr 범위로 설정하여 제조한다. 이 범위에서 평균 입도가 5~400nm이고, 산화층의 두께가 0.53nm인 실리콘-탄소 합금 나노입자(SiC-NPs)가 제조된다.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. Further, 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.
제조예 4Preparation Example 4
실리콘-게르마늄 합금 나노입자는 하기 반응식 4 중 (1) 또는 (2)에 따라 제조될 수 있다.Silicon-germanium alloy nanoparticles can be prepared according to (1) or (2) in Scheme 4 below.
<반응식 4><Scheme 4>
(1) SiH4 + GeH4 + SF6 → S + SiGe + 6HF + H2 (1) SiH 4 + GeH 4 + SF 6 → S + SiGe + 6HF + H 2
(2) SiH4 + GeH4 → SiGe + 4H2 (2) SiH 4 + GeH 4 → SiGe + 4H 2
원료가스 공급노즐을 통해 원료가스인 저메인(GeH4) 100부피부(원료가스 1), 모노실란(SiH4) 100부피부(원료가스 2), 및 캐리어가스인 질소(N2) 400 부피부를 혼합한 혼합가스를 내부 압력이 100~500torr인 반응챔버 내부로 공급하고, 반응챔버 내부로 공급된 혼합가스에 CO2 레이저 발생기에서 발생시킨 레이저를 조사부를 통해 파장이 10.6㎛인 연속파의 라인 빔(Line Beam) 형태로 3시간 동안 조사하여 실리콘-게르마늄 합금 나노입자(SiGe-NPs)를 제조하였다. SiGe-NPs의 평균 입도는 5~400nm이고, 그 표면에 형성된 산화층의 두께는 0.47nm이다. 400 parts by volume of raw gas (GeH 4 ), 100 parts by volume of raw gas (raw gas 1), monosilane (SiH 4 ) by 100 parts by volume of raw gas (raw gas 2), and nitrogen (N 2 ) by carrier gas Is supplied to the inside of the reaction chamber of the internal pressure of 100 ~ 500torr, the continuous gas line beam having a wavelength of 10.6㎛ through the irradiation section of the laser generated by the CO 2 laser generator to the mixed gas supplied into the reaction chamber Irradiation for 3 hours in the form of (Line Beam) to prepare silicon-germanium alloy nanoparticles (SiGe-NPs). The average particle size of SiGe-NPs is 5 to 400 nm, and the thickness of the oxide layer formed on the surface thereof is 0.47 nm.
제조예 5Preparation Example 5
실리콘-게르마늄-붕소 합금 나노입자는 하기 반응식 5에 따라 제조될 수 있다.Silicon-germanium-boron alloy nanoparticles can be prepared according to Scheme 5 below.
<반응식 5> Scheme 5
2SiH4 + 2GeH4 + B2H6 → 2SiGeB + 11H2 2SiH 4 + 2GeH 4 + B 2 H 6 → 2SiGeB + 11H 2
원료가스 공급노즐을 통해 원료가스인 모노실란(SiH4) 100부피부, 저메인(GeH4) 100부피부, 및 디보레인(B2H6) 40~80부피부와 캐리어가스인 질소(N2) 400 부피부를 혼합한 혼합가스를 내부 압력이 80~400torr인 반응챔버 내부로 공급하고, 반응챔버 내부로 공급된 혼합가스에 CO2 레이저 발생기에서 발생시킨 레이저를 조사부를 통해 파장이 10.6㎛인 연속파의 라인 빔(Line Beam) 형태로 3시간 동안 조사하여 실리콘-게르마늄-붕소 합금 나노입자(SiGeB-NPs)를 제조하였다. SiGeB-NPs의 평균 입도는 5~400nm이고, 그 표면에 형성된 산화층의 두께는 0.75nm이다.100 parts by weight of monosilane (SiH 4 ), 100 parts by weight of germane (GeH 4 ), and diborane (B 2 H 6 ) by 40 to 80 parts by volume through the feed gas supply nozzle and nitrogen (N 2) ) 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 μm. 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.
제조예 6Preparation Example 6
실리콘-게르마늄-탄소 합금 나노입자는 하기 반응식 6에 따라 제조될 수 있다.Silicon-germanium-carbon alloy nanoparticles may be prepared according to Scheme 6 below.
<반응식 6><Scheme 6>
2SiH4 + 2GeH4 + C2H2 → 2SiGeC + 9H2 2SiH 4 + 2GeH 4 + C 2 H 2 → 2SiGeC + 9H 2
원료가스 공급노즐을 통해 원료가스인 모노실란(SiH4) 100부피부, 저메인(GeH4) 100부피부, 및 아세틸렌(C2H2) 40~80부피부와 캐리어가스인 질소(N2) 400 부피부를 혼합한 혼합가스를 내부 압력이 80~400torr인 반응챔버 내부로 공급하고, 반응챔버 내부로 공급된 혼합가스에 CO2 레이저 발생기에서 발생시킨 레이저를 조사부를 통해 파장이 10.6㎛인 연속파의 라인 빔(Line Beam) 형태로 3시간 동안 조사하여 실리콘-게르마늄-탄소 합금 나노입자(SiGeC-NPs)를 제조하였다. SiGeC-NPs의 평균 입도는 5~400nm이고, 그 표면에 형성된 산화층의 두께는 0.68nm이다.100 parts by weight of monosilane (SiH 4 ), 100 parts by weight of germane (GeH 4 ), and 40 to 80 parts by weight of acetylene (C 2 H 2 ) and nitrogen (N 2 ) A continuous gas having a wavelength of 10.6 μm 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.
제조예 7Preparation Example 7
게르마늄 나노입자는 하기 반응식 7 중 (1) 또는 (2)에 따라 제조될 수 있다.Germanium nanoparticles can be prepared according to (1) or (2) in Scheme 7 below.
<반응식 7>Scheme 7
(1) 2GeH4 + SF6 → S + 2GeF4 + 2HF + 3H2 (1) 2GeH 4 + SF 6 → S + 2GeF 4 + 2HF + 3H 2
(2) GeH4 + N2 → 2Ge + 2H2 + N2 (2) GeH 4 + N 2 → 2Ge + 2H 2 + N 2
원료가스 공급노즐을 통해 원료가스인 저메인(GeH4) 100 부피부, 제어가스인 수소(H2) 400 부피부, 및 육불화황(SF6) 촉매가스 40 부피부를 혼합한 혼합가스를 내부 압력이 500torr인 반응챔버 내부로 공급하고, 반응챔버 내부로 공급된 혼합가스에 CO2 레이저 발생기에서 발생시킨 레이저를 레이저 조사부를 통해 파장이 10.6㎛인 연속파의 라인 빔(Line Beam) 형태로 3시간 동안 조사하여 산화층이 형성된 게르마늄 나노입자(Ge-NPs)를 제조하였다.Through the feed gas supply nozzle, 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㎛ through the laser irradiation unit for 3 hours. During irradiation, germanium nanoparticles (Ge-NPs) in which an oxide layer was formed were prepared.
제조된 산화층이 형성된 게르마늄 나노입자의 평균 입도는 5~400nm이고, 산화층의 두께는 0.47nm이며, 생성수율은 98.7%이다.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%.
제조예 8Preparation Example 8
게르마늄-붕소 합금 나노입자 또는 붕화게르마늄 나노입자는 하기 반응식 8에 따라 제조될 수 있다.Germanium-boron alloy nanoparticles or germanium boride nanoparticles may be prepared according to Scheme 8 below.
<반응식 8>Scheme 8
2GeH4 + 2B2H6 + N2 → GeB4 + 8H2 + N2 2GeH 4 + 2B 2 H 6 + N 2 → GeB 4 + 8H 2 + N 2
원료가스 공급노즐을 통해 원료가스인 저메인(GeH4) 100부피부, 디보레인(B2H6) 40~80부피부, 및 캐리어가스인 질소(N2) 400 부피부를 혼합한 혼합가스를 내부 압력이 100~400torr인 반응챔버 내부로 공급하고, 반응챔버 내부로 공급된 혼합가스에 CO2 레이저 발생기에서 발생시킨 레이저를 조사부를 통해 파장이 10.6㎛인 연속파의 라인 빔(Line Beam) 형태로 3시간 동안 조사하여 게르마늄-붕소 합금 나노입자(GeBx-NPs)를 제조하였다. GeBx-NPs의 입도는 5~400nm이고, 그 표면에 형성된 산화층의 두께는 0.52nm이다.Through the feed gas supply nozzle, 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 μm 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.
제조예 9Preparation Example 9
게르마늄-탄소 합금 나노입자 또는 탄화게르마늄 나노입자는 하기 반응식 9 중 (1) 또는 (2)에 따라 제조될 수 있다.Germanium-carbon alloy nanoparticles or germanium carbide nanoparticles may be prepared according to (1) or (2) in Scheme 9 below.
<반응식 9>Scheme 9
(1) 2GeH4 + C2H2 + SF6 → S + 2GeC + 6HF + 2H2 (1) 2GeH 4 + C 2 H 2 + SF 6 → S + 2GeC + 6HF + 2H 2
(2) 2GeH4 + C2H2 → 2GeC + 5H2 (2) 2GeH 4 + C 2 H 2 → 2GeC + 5H 2
저메인(GeH4), 아세틸렌(C2H2), 질소를 혼합하여 반응챔버 내부로 주입하여 CO2 레이저빔을 조사시킨다. 아세틸렌은 탄소와 수소 원자로 분해되어 탄소는 실리콘 나노입자와 합금을 이루며, 실리콘의 산화를 방지한다. 원료가스인 저메인 및 아세틸렌은 각각 2 : 1의 부피비로 주입된다. 또한, 캐리어가스인 질소는 원료가스인 실란가스 대비 400 부피부를 넘지 않도록 한다. 가스의 유량은 sccm 단위를 사용한다. 반응챔버 내부의 공정압력은 100~500torr 범위로 설정하여 제조한다. 이 범위에서 평균 입도가 5~400nm이고, 산화층의 두께가 0.58nm인 게르마늄-탄소 합금 나노입자(GeC-NPs)가 제조된다.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. In addition, 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.
제조예 10Preparation Example 10
탄소-붕소 합금 나노입자 또는 탄화붕소 나노입자는 하기 반응식 10에 따라 제조될 수 있다.Carbon-boron alloy nanoparticles or boron carbide nanoparticles may be prepared according to Scheme 10 below.
<반응식 10>Scheme 10
C2H2 + 4B2H6 + N2 → 2B4C + 13H2 + N2 C 2 H 2 + 4 B 2 H 6 + N 2 → 2B 4 C + 13 H 2 + N 2
원료가스 공급노즐을 통해 원료가스인 아세틸렌(C2H2) 100부피부, 디보레인(B2H6) 400부피부, 및 캐리어가스인 질소(N2) 400 부피부를 혼합한 혼합가스를 내부 압력이 100~400torr인 반응챔버 내부로 공급하고, 반응챔버 내부로 공급된 혼합가스에 CO2 레이저 발생기에서 발생시킨 레이저를 조사부를 통해 파장이 10.6㎛인 연속파의 라인 빔(Line Beam) 형태로 3시간 동안 조사하여 탄소-붕소 합금 나노입자(CBx-NPs)를 제조하였다. CBx-NPs의 입도는 5~400nm이고, 그 표면에 형성된 산화층의 두께는 0.46nm이다.A mixed gas obtained by mixing 100 parts by volume of acetylene (C 2 H 2 ), 400 parts by weight of diborane (B 2 H 6 ) and 400 parts by weight of nitrogen (N 2 ) as a carrier gas through a source gas supply nozzle 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 μm 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.
제조예 11Preparation Example 11
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 1의 5~400nm의 Si-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 Si-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 Si-NPs의 산화를 방지한다.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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 Si-NPs에 탄소를 코팅하게 되면(C@Si-NPs), 내부 코어는 5~400nm 크기를 갖는 Si-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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.
제조예 12Preparation Example 12
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 2의 5~400nm의 제조예 2의 SiB4-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 SiB4-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 SiB4-NPs의 산화를 방지한다.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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 SiB4-NPs에 탄소를 코팅하게 되면(C@SiB4-NPs), 내부 코어는 5~400nm 크기를 갖는 SiB4-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 SiB 4 -NPs in this range (C @ SiB 4 -NPs), 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.
제조예 13Preparation Example 13
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 3의 5~400nm의 제조예 3의 SiC-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 SiC-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 SiC-NPs의 산화를 방지한다.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. . At this time, 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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 SiC-NPs에 탄소를 코팅하게 되면(C@SiC-NPs), 내부 코어는 5~400nm 크기를 갖는 SiC-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 SiC-NPs in this range (C @ SiC-NPs), 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.
제조예 14Preparation Example 14
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 4의 5~400nm의 SiGe-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 SiGe-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 SiGe-NPs의 산화를 방지한다.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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 SiGe-NPs에 탄소를 코팅하게 되면(C@SiGe-NPs), 내부 코어는 5~400nm 크기를 갖는 SiGe-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 SiGe-NPs in this range (C @ SiGe-NPs), 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.
제조예 15Preparation Example 15
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 5의 5~400nm의 SiGeB-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 SiGeB-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 SiGeB-NPs의 산화를 방지한다.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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 SiGeB-NPs에 탄소를 코팅하게 되면(C@SiGeB-NPs), 내부 코어는 5~400nm 크기를 갖는 SiGeB-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 SiGeB-NPs in this range (C @ SiGeB-NPs), 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.
제조예 16Preparation Example 16
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 6의 5~400nm의 SiGeC-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 SiGeC-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 SiGeC-NPs의 산화를 방지한다.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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 SiGeC-NPs에 탄소를 코팅하게 되면(C@SiGeC-NPs), 내부 코어는 5~400nm 크기를 갖는 SiGeC-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 SiGeC-NPs in this range (C @ SiGeC-NPs), 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.
제조예 17Preparation Example 17
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 7의 5~400nm의 Ge-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 Ge-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 Ge-NPs의 산화를 방지한다.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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 Ge-NPs에 탄소를 코팅하게 되면(C@Ge-NPs), 내부 코어는 5~400nm 크기를 갖는 Ge-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 Ge-NPs in this range (C @ Ge-NPs), 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.
제조예 18Preparation Example 18
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 8의 5~400nm의 GeB4-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 GeB4-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 GeB4-NPs의 산화를 방지한다.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. At this time, 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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 GeB4-NPs에 탄소를 코팅하게 되면(C@GeB4-NPs), 내부 코어는 5~400nm 크기를 갖는 GeB4-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 GeB4-NPs in this range (C @ GeB 4 -NPs), 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.
제조예 19Preparation Example 19
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 9의 5~400nm의 GeC-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 GeC-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 GeC-NPs의 산화를 방지한다.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. At this time, 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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 GeC-NPs에 탄소를 코팅하게 되면(C@GeC-NPs), 내부 코어는 5~400nm 크기를 갖는 GeC-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 GeC-NPs in this range (C @ GeC-NPs), 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.
제조예 20Preparation Example 20
아세틸렌 가스(C2H2) 및 질소를 혼합하여 반응기 챔버 내부로 주입하고, 반응기 챔버 내부로 제조예 10의 5~400nm의 CB4-NPs를 흘려준 후 CO2 레이저빔을 조사시킨다. 이때, 아세틸렌가스의 C-H 결합이 CB4-NPs 표면에 탄소층을 생성시킬 수 있다. 질소 가스는 CB4-NPs의 산화를 방지한다.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.
원료가스인 아세틸렌 가스는 전체 부피부(아세틸렌가스 및 질소 가스를 합친 부피부)의 60 이상을 함유하고, 질소 가스는 전체 부피부의 40 이상을 넘지 않는 범위로 조절한다. 가스의 유량은 sccm 단위를 사용한다. 반응기 챔버 내부의 공정압력은 100~400torr 범위로 설정하여 제조한다. 이 범위에서 CB4-NPs에 탄소를 코팅하게 되면(C@CB4-NPs), 내부 코어는 5~400nm 크기를 갖는 CB4-NPs이고, 표면에 1~100nm 범위의 탄소층이 형성된다.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 CB 4 -NPs in this range (C @ CB 4 -NPs), 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.
실시예 1Example 1
제조예 1의 Si-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 was dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare surface-modified Si-NPs with methoxy groups.
실시예 2Example 2
제조예 1의 Si-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 3Example 3
제조예 1의 Si-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 4Example 4
제조예 1의 Si-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 5Example 5
제조예 1의 Si-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 6Example 6
제조예 1의 Si-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 7Example 7
제조예 1의 Si-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 8Example 8
제조예 1의 Si-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 9Example 9
제조예 1의 Si-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 10Example 10
제조예 1의 Si-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 Si-NPs를 제조하였다.100 mg of Si-NPs of Preparation Example 1 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.
실시예 11Example 11
제조예 2의 SiB4-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare surface-modified SiB 4 -NPs.
실시예 12Example 12
제조예 2의 SiB4-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiB 4 -NPs with ethoxy groups.
실시예 13Example 13
제조예 2의 SiB4-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 14Example 14
제조예 2의 SiB4-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 15Example 15
제조예 2의 SiB4-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 16Example 16
제조예 2의 SiB4-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 17Example 17
제조예 2의 SiB4-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 18Example 18
제조예 2의 SiB4-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 19Example 19
제조예 2의 SiB4-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 20Example 20
제조예 2의 SiB4-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 SiB4-NPs를 제조하였다.100 mg of SiB 4 -NPs of Preparation Example 2 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.
실시예 21Example 21
제조예 3의 SiC-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 was dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare surface-modified SiC-NPs with methoxy groups.
실시예 22Example 22
제조예 3의 SiC-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare SiC-NPs surface-modified with an ethoxy group.
실시예 23Example 23
제조예 3의 SiC-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 was dispersed in 25 ml of isopropyl alcohol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiC-NPs with isopropoxy group.
실시예 24Example 24
제조예 3의 SiC-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 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.
실시예 25Example 25
제조예 3의 SiC-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 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.
실시예 26Example 26
제조예 3의 SiC-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 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.
실시예 27Example 27
제조예 3의 SiC-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 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.
실시예 28Example 28
제조예 3의 SiC-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 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.
실시예 29Example 29
제조예 3의 SiC-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 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.
실시예 30Example 30
제조예 3의 SiC-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 SiC-NPs를 제조하였다.100 mg of SiC-NPs of Preparation Example 3 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.
실시예 31Example 31
제조예 4의 SiGe-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 32Example 32
제조예 4의 SiGe-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGe-NPs with ethoxy groups.
실시예 33Example 33
제조예 4의 SiGe-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 34Example 34
제조예 4의 SiGe-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 35Example 35
제조예 4의 SiGe-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 36Example 36
제조예 4의 SiGe-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 37Example 37
제조예 4의 SiGe-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 38Example 38
제조예 4의 SiGe-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 39Example 39
제조예 4의 SiGe-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 40Example 40
제조예 4의 SiGe-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 SiGe-NPs를 제조하였다.100 mg of SiGe-NPs of Preparation Example 4 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.
실시예 41Example 41
제조예 5의 SiGeB-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 42Example 42
제조예 5의 SiGeB-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 was dispersed in 25 ml of ethanol, and ultrasonically irradiated for 5 minutes to prepare surface-modified SiGeB-NPs with ethoxy groups.
실시예 43Example 43
제조예 5의 SiGeB-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 was dispersed in 25 ml of isopropyl alcohol, and ultrasonically irradiated for 5 minutes to prepare SiGeB-NPs surface-modified with isopropoxy.
실시예 44Example 44
제조예 5의 SiGeB-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 45Example 45
제조예 5의 SiGeB-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 46Example 46
제조예 5의 SiGeB-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 47Example 47
제조예 5의 SiGeB-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 48Example 48
제조예 5의 SiGeB-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 49Example 49
제조예 5의 SiGeB-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 50Example 50
제조예 5의 SiGeB-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 SiGeB-NPs를 제조하였다.100 mg of SiGeB-NPs of Preparation Example 5 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.
실시예 51Example 51
제조예 6의 SiGeC-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 was dispersed in 25 ml of methanol and irradiated with ultrasonic waves for 5 minutes to prepare surface-modified SiGeC-NPs.
실시예 52Example 52
제조예 6의 SiGeC-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 53Example 53
제조예 6의 SiGeC-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 54Example 54
제조예 6의 SiGeC-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 55Example 55
제조예 6의 SiGeC-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 56Example 56
제조예 6의 SiGeC-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 57Example 57
제조예 6의 SiGeC-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 58Example 58
제조예 6의 SiGeC-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 59Example 59
제조예 6의 SiGeC-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 60Example 60
제조예 6의 SiGeC-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 SiGeC-NPs를 제조하였다.100 mg of SiGeC-NPs of Preparation Example 6 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.
실시예 61Example 61
제조예 7의 Ge-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 Ge-NPs를 제조하였다.100 mg of Ge-NPs of Preparation Example 7 was dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare surface-modified Ge-NPs with methoxy groups.
실시예 62Example 62
제조예 7의 Ge-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 Ge-NPs를 제조하였다.100 mg of Ge-NPs of Preparation Example 7 were dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare Ge-NPs surface-modified with an ethoxy group.
실시예 63Example 63
제조예 7의 Ge-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 Ge-NPs를 제조하였다.100 mg of Ge-NPs of Preparation Example 7 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.
실시예 64Example 64
제조예 7의 Ge-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 Ge-NPs를 제조하였다.100 mg of Ge-NPs of Preparation Example 7 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.
실시예 65Example 65
제조예 7의 Ge-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 Ge-NPs를 제조하였다.100 mg of Ge-NPs of Preparation Example 7 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.
실시예 66Example 66
제조예 7의 Ge-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 Ge-NPs를 제조하였다.100 mg of Ge-NPs of Preparation Example 7 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.
실시예 67Example 67
제조예 7의 Ge-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 Ge-NPs를 제조하였다.100 mg of 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.
실시예 68Example 68
제조예 7의 Ge-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 Ge-NPs를 제조하였다.100 mg of Ge-NPs of Preparation Example 7 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.
실시예 69Example 69
제조예 7의 Ge-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 Ge-NPs를 제조하였다.100 mg of 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.
실시예 70Example 70
제조예 7의 Ge-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 Ge-NPs를 제조하였다.100 mg of 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.
실시예 71Example 71
제조예 8의 GeB4-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 72Example 72
제조예 8의 GeB4-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 73Example 73
제조예 8의 GeB4-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 74Example 74
제조예 8의 GeB4-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 75Example 75
제조예 8의 GeB4-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 76Example 76
제조예 8의 GeB4-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 77Example 77
제조예 8의 GeB4-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 78Example 78
제조예 8의 GeB4-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 79Example 79
제조예 8의 GeB4-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 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.
실시예 80Example 80
제조예 8의 GeB4-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 GeB4-NPs를 제조하였다.100 mg of GeB 4 -NPs of Preparation Example 8 were dispersed in 25 ml of an organic solvent aqueous solution (water and methylene chloride mixed at 1: 1 parts by weight), and ultrasonically irradiated for 5 minutes to prepare GeB 4 -NPs surface-modified with a hydroxyl group of water. It was.
실시예 81Example 81
제조예 9의 GeC-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 82Example 82
제조예 9의 GeC-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare GeC-NPs surface-modified with an ethoxy group.
실시예 83Example 83
제조예 9의 GeC-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 was dispersed in 25 ml of isopropyl alcohol, and ultrasound was irradiated for 5 minutes to prepare GeC-NPs surface-modified with isopropoxy group.
실시예 84Example 84
제조예 9의 GeC-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 85Example 85
제조예 9의 GeC-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 86Example 86
제조예 9의 GeC-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 87Example 87
제조예 9의 GeC-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 88Example 88
제조예 9의 GeC-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 89Example 89
제조예 9의 GeC-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 90Example 90
제조예 9의 GeC-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 GeC-NPs를 제조하였다.100 mg of GeC-NPs of Preparation Example 9 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.
실시예 91Example 91
제조예 10의 CB4-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 was dispersed in 25 ml of methanol, and ultrasonic waves were irradiated for 5 minutes to prepare CB 4 -NPs surface-modified with a methoxy group.
실시예 92Example 92
제조예 10의 CB4-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare CB 4 -NPs surface-modified with an ethoxy group.
실시예 93Example 93
제조예 10의 CB4-NPs 100mg을 이소프로필알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 이소프로폭시기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 was dispersed in 25 ml of isopropyl alcohol, and ultrasonic wave was irradiated for 5 minutes to prepare CB 4 -NPs surface-modified with isopropoxy.
실시예 94Example 94
제조예 10의 CB4-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare CB 4 -NPs surface-modified with 2-aminoalkoxy group.
실시예 95Example 95
제조예 10의 CB4-NPs 100mg을 부틸페놀 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 부틸페녹시기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 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.
실시예 96Example 96
제조예 10의 CB4-NPs 100mg을 아세트산 0.5ml와 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 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.
실시예 97Example 97
제조예 10의 CB4-NPs 100mg을 스테아르산 0.5g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 스테아르산기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 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.
실시예 98Example 98
제조예 10의 CB4-NPs 100mg을 아세틸살리실산 0.1g과 디클로로메탄 25ml로 이루어진 혼합물에 분산시키고, 초음파를 5분 동안 조사하여 아세틸살리실산기로 표면개질된 CB4-NPs를 제조하였다.Dispersing the CB 4 -NPs 100mg of Preparation 10 To a mixture consisting of acetylsalicylic acid 0.1g and 25ml of dichloromethane, and applying ultrasonic waves for 5 minutes to prepare a surface-modified CB 4 -NPs group acetylsalicylic acid.
실시예 99Example 99
제조예 10의 CB4-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 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 CB 4 -NPs with a hydroxyl group of boric acid. It was.
실시예 100Example 100
제조예 10의 CB4-NPs 100mg을 유기용매 수용액(물과 메틸렌클로라이드가 1:1 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 물의 수산화기로 표면개질된 CB4-NPs를 제조하였다.100 mg of CB 4 -NPs of Preparation Example 10 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 CB 4 -NPs with a hydroxyl group of water. It was.
실시예 101Example 101
제조예 11의 C@Si-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@Si-NPs를 제조하였다.100 mg of C @ Si-NPs of Preparation Example 11 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ Si-NPs surface-modified with a methoxy group.
실시예 102Example 102
제조예 11의 C@Si-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@Si-NPs를 제조하였다.100 mg of C @ Si-NPs of Preparation Example 11 was dispersed in 25 ml of ethanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ Si-NPs surface-modified with an ethoxy group.
실시예 103Example 103
제조예 11의 C@Si-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@Si-NPs를 제조하였다.100 mg of C @ Si-NPs of Preparation Example 11 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ Si-NPs surface-modified with 2-aminoalkoxy group.
실시예 104Example 104
제조예 11의 C@Si-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@Si-NPs를 제조하였다.100 mg of C @ Si-NPs of Preparation Example 11 was dispersed in 25 ml of acetic acid, and ultrasonic wave was irradiated for 5 minutes to prepare C @ Si-NPs surface-modified with an acetic acid.
실시예 105Example 105
제조예 11의 C@Si-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@Si-NPs를 제조하였다.100 mg of C @ Si-NPs of Preparation Example 11 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 irradiated with ultrasonic waves for 5 minutes to modify the surface of C @ Si-NPs with a hydroxyl group of boric acid. Was prepared.
실시예 106Example 106
제조예 12의 C@SiB4-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@SiB4-NPs를 제조하였다.100 mg of C @ SiB 4 -NPs of Preparation Example 12 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiB 4 -NPs surface-modified with a methoxy group.
실시예 107Example 107
제조예 12의 C@SiB4-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@SiB4-NPs를 제조하였다.100 mg of C @ SiB 4 -NPs of Preparation Example 12 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare C @ SiB 4 -NPs surface-modified with an ethoxy group.
실시예 108Example 108
제조예 12의 C@SiB4-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@SiB4-NPs를 제조하였다.100 mg of C @ SiB 4 -NPs of Preparation Example 12 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiB 4 -NPs surface-modified with 2-aminoalkoxy group.
실시예 109Example 109
제조예 12의 C@SiB4-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@SiB4-NPs를 제조하였다.100 mg of C @ SiB 4 -NPs of Preparation Example 12 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ SiB 4 -NPs surface-modified with an acetic acid.
실시예 110Example 110
제조예 12의 C@SiB4-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@SiB4-NPs를 제조하였다.100 mg of C @ SiB 4 -NPs of Preparation Example 12 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 irradiated with ultrasonic waves for 5 minutes to modify the surface of C @ SiB 4 with a hydroxyl group of boric acid. -NPs were prepared.
실시예 111Example 111
제조예 13의 C@SiC-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@SiC-NPs를 제조하였다.100 mg of C @ SiC-NPs of Preparation Example 13 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiC-NPs surface-modified with a methoxy group.
실시예 112Example 112
제조예 13의 C@SiC-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@SiC-NPs를 제조하였다.100 mg of C @ SiC-NPs of Preparation Example 13 was dispersed in 25 ml of ethanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiC-NPs surface-modified with an ethoxy group.
실시예 113Example 113
제조예 13의 C@SiC-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@SiC-NPs를 제조하였다.100 mg of C @ SiC-NPs of Preparation Example 13 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiC-NPs surface-modified with 2-aminoalkoxy group.
실시예 114Example 114
제조예 13의 C@SiC-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@SiC-NPs를 제조하였다.100 mg of C @ SiC-NPs of Preparation Example 13 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ SiC-NPs surface-modified with an acetic acid.
실시예 115Example 115
제조예 13의 C@SiC-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@SiC-NPs를 제조하였다.100 mg of C @ SiC-NPs of Preparation Example 13 was dispersed in 25 ml of 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 modify the surface of C @ SiC-NPs with a hydroxyl group of boric acid. Was prepared.
실시예 116Example 116
제조예 14의 C@SiGe-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@SiGe-NPs를 제조하였다.100 mg of C @ SiGe-NPs of Preparation Example 14 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGe-NPs surface-modified with a methoxy group.
실시예 117Example 117
제조예 14의 C@SiGe-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@SiGe-NPs를 제조하였다.100 mg of C @ SiGe-NPs of Preparation Example 14 was dispersed in 25 ml of ethanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGe-NPs surface-modified with an ethoxy group.
실시예 118Example 118
제조예 14의 C@SiGe-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@SiGe-NPs를 제조하였다.100 mg of C @ SiGe-NPs of Preparation Example 14 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGe-NPs surface-modified with 2-aminoalkoxy group.
실시예 119Example 119
제조예 14의 C@SiGe-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@SiGe-NPs를 제조하였다.100 mg of C @ SiGe-NPs of Preparation Example 14 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ SiGe-NPs surface-modified with an acetic acid.
실시예 120Example 120
제조예 14의 C@SiGe-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@SiGe-NPs를 제조하였다.100 mg of C @ SiGe-NPs of Preparation Example 14 was dispersed in 25 ml of aqueous boric acid solution (boric acid and distilled water mixed at 5:95 parts by weight), and ultrasonically irradiated for 5 minutes to modify the surface of C @ SiGe-NPs with a hydroxyl group of boric acid. Was prepared.
실시예 121Example 121
제조예 15의 C@SiGeB-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@SiGeB-NPs를 제조하였다.100 mg of C @ SiGeB-NPs of Preparation Example 15 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGeB-NPs surface-modified with a methoxy group.
실시예 122Example 122
제조예 15의 C@SiGeB-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@SiGeB-NPs를 제조하였다.100 mg of C @ SiGeB-NPs of Preparation Example 15 was dispersed in 25 ml of ethanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGeB-NPs surface-modified with an ethoxy group.
실시예 123Example 123
제조예 15의 C@SiGeB-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@SiGeB-NPs를 제조하였다.100 mg of C @ SiGeB-NPs of Preparation Example 15 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGeB-NPs surface-modified with 2-aminoalkoxy group.
실시예 124Example 124
제조예 15의 C@SiGeB-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@SiGeB-NPs를 제조하였다.100 mg of C @ SiGeB-NPs of Preparation Example 15 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ SiGeB-NPs surface-modified with an acetic acid.
실시예 125Example 125
제조예 15의 C@SiGeB-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@SiGeB-NPs를 제조하였다.100 mg of C @ SiGeB-NPs of Preparation Example 15 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 ultrasonically irradiated for 5 minutes to surface-modify C @ SiGeB-NPs with a hydroxyl group of boric acid. Was prepared.
실시예 126Example 126
제조예 16의 C@SiGeC-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@SiGeC-NPs를 제조하였다.100 mg of C @ SiGeC-NPs of Preparation Example 16 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGeC-NPs surface-modified with a methoxy group.
실시예 127Example 127
제조예 16의 C@SiGeC-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@SiGeC-NPs를 제조하였다.100 mg of C @ SiGeC-NPs of Preparation Example 16 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare C @ SiGeC-NPs surface-modified with an ethoxy group.
실시예 128Example 128
제조예 16의 C@SiGeC-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@SiGeC-NPs를 제조하였다.100 mg of C @ SiGeC-NPs of Preparation Example 16 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ SiGeC-NPs surface-modified with 2-aminoalkoxy group.
실시예 129Example 129
제조예 16의 C@SiGeC-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@SiGeC-NPs를 제조하였다.100 mg of C @ SiGeC-NPs of Preparation Example 16 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ SiGeC-NPs surface-modified with an acetic acid.
실시예 130Example 130
제조예 16의 C@SiGeC-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@SiGeC-NPs를 제조하였다.100 mg of C @ SiGeC-NPs of Preparation Example 16 was dispersed in 25 ml of an aqueous boric acid solution (boric acid and distilled water mixed at a weight of 5:95 parts by weight), and ultrasonically irradiated for 5 minutes to surface-modify C @ SiGeC-NPs with a hydroxyl group of boric acid. Was prepared.
실시예 131Example 131
제조예 17의 C@Ge-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@Ge-NPs를 제조하였다.100 mg of C @ Ge-NPs of Preparation Example 17 was dispersed in 25 ml of methanol, and ultrasound was irradiated for 5 minutes to prepare C @ Ge-NPs surface-modified with a methoxy group.
실시예 132Example 132
제조예 17의 C@Ge-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@Ge-NPs를 제조하였다.100 mg of C @ Ge-NPs of Preparation Example 17 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare C @ Ge-NPs surface-modified with an ethoxy group.
실시예 133Example 133
제조예 17의 C@Ge-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@Ge-NPs를 제조하였다.100 mg of C @ Ge-NPs of Preparation Example 17 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ Ge-NPs surface-modified with 2-aminoalkoxy group.
실시예 134Example 134
제조예 17의 C@Ge-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@Ge-NPs를 제조하였다.100 mg of C @ Ge-NPs of Preparation Example 17 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ Ge-NPs surface-modified with an acetic acid.
실시예 135Example 135
제조예 17의 C@Ge-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@Ge-NPs를 제조하였다.100 mg of C @ Ge-NPs of Preparation Example 17 was dispersed in 25 ml of aqueous boric acid solution (mixed with boric acid and distilled water at 5:95 parts by weight), and ultrasonically irradiated for 5 minutes, thereby modifying C @ Ge-NPs surface-modified with a hydroxyl group of boric acid. Was prepared.
실시예 136Example 136
제조예 18의 C@GeB4-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@GeB4-NPs를 제조하였다.100 mg of C @ GeB 4 -NPs of Preparation Example 18 was dispersed in 25 ml of methanol, and ultrasound was irradiated for 5 minutes to prepare C @ GeB 4 -NPs surface-modified with a methoxy group.
실시예 137Example 137
제조예 18의 C@GeB4-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@GeB4-NPs를 제조하였다.100 mg of C @ GeB 4 -NPs of Preparation Example 18 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare C @ GeB 4 -NPs surface-modified with an ethoxy group.
실시예 138Example 138
제조예 18의 C@GeB4-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@GeB4-NPs를 제조하였다.100 mg of C @ GeB 4 -NPs of Preparation Example 18 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ GeB 4 -NPs surface-modified with 2-aminoalkoxy group.
실시예 139Example 139
제조예 18의 C@GeB4-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@GeB4-NPs를 제조하였다.100 mg of C @ GeB 4 -NPs of Preparation Example 18 was dispersed in 25 ml of acetic acid, and ultrasonic wave was irradiated for 5 minutes to prepare C @ GeB 4 -NPs surface-modified with an acetic acid.
실시예 140Example 140
제조예 18의 C@GeB4-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@GeB4-NPs를 제조하였다.100 mg of C @ GeB 4 -NPs of Preparation Example 18 was dispersed in 25 ml of an aqueous boric acid solution (boric acid and distilled water mixed at a weight of 5:95 parts by weight), and ultrasonically irradiated for 5 minutes to surface-modify C @ GeB 4 with a hydroxyl group of boric acid. -NPs were prepared.
실시예 141Example 141
제조예 19의 C@GeC-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@GeC-NPs를 제조하였다.100 mg of C @ GeC-NPs of Preparation Example 19 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ GeC-NPs surface-modified with a methoxy group.
실시예 142Example 142
제조예 19의 C@GeC-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@GeC-NPs를 제조하였다.100 mg of C @ GeC-NPs of Preparation Example 19 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare C @ GeC-NPs surface-modified with an ethoxy group.
실시예 143Example 143
제조예 19의 C@GeC-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@GeC-NPs를 제조하였다.100 mg of C @ GeC-NPs of Preparation Example 19 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ GeC-NPs surface-modified with 2-aminoalkoxy group.
실시예 144Example 144
제조예 19의 C@GeC-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@GeC-NPs를 제조하였다.100 mg of C @ GeC-NPs of Preparation Example 19 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ GeC-NPs surface-modified with an acetic acid.
실시예 145Example 145
제조예 19의 C@GeC-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@GeC-NPs를 제조하였다.100 mg of C @ GeC-NPs of Preparation Example 19 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 modify the surface of C @ GeC-NPs with a hydroxyl group of boric acid. Was prepared.
실시예 146Example 146
제조예 20의 C@CB4-NPs 100mg을 메탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 메톡시기로 표면개질된 C@CB4-NPs를 제조하였다.100 mg of C @ CB 4 -NPs of Preparation Example 20 was dispersed in 25 ml of methanol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ CB 4 -NPs surface-modified with a methoxy group.
실시예 147Example 147
제조예 20의 C@CB4-NPs 100mg을 에탄올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 에톡시기로 표면개질된 C@CB4-NPs를 제조하였다.100 mg of C @ CB 4 -NPs of Preparation Example 20 was dispersed in 25 ml of ethanol, and ultrasound was irradiated for 5 minutes to prepare C @ CB 4 -NPs surface-modified with an ethoxy group.
실시예 148Example 148
제조예 20의 C@CB4-NPs 100mg을 2-아미노알코올 25ml에 분산시키고, 초음파를 5분 동안 조사하여 2-아미노알콕시기로 표면개질된 C@CB4-NPs를 제조하였다.100 mg of C @ CB 4 -NPs of Preparation Example 20 was dispersed in 25 ml of 2-aminoalcohol, and ultrasonic wave was irradiated for 5 minutes to prepare C @ CB 4 -NPs surface-modified with 2-aminoalkoxy group.
실시예 149Example 149
제조예 20의 C@CB4-NPs 100mg을 아세트산 25ml에 분산시키고, 초음파를 5분 동안 조사하여 아세트산기로 표면개질된 C@CB4-NPs를 제조하였다.100 mg of C @ CB 4 -NPs of Preparation Example 20 was dispersed in 25 ml of acetic acid, and ultrasonic waves were irradiated for 5 minutes to prepare C @ CB 4 -NPs surface-modified with an acetic acid.
실시예 150Example 150
제조예 20의 C@CB4-NPs 100mg을 붕산 수용액(붕산과 증류수가 5:95의 중량부로 혼합) 25ml에 분산시키고, 초음파를 5분 동안 조사하여 붕산의 수산화기로 표면개질된 C@CB4-NPs를 제조하였다.100 mg of C @ CB 4 -NPs of Preparation Example 20 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 modify the surface of C @ CB 4 with hydroxylated boric acid. -NPs were prepared.
실험예Experimental Example
상기 제조예, 실시예를 통해 제조된 탄소족 비산화물 나노입자를 물로 희석하여 탄소족 비산화물 나노입자의 농도가 2mM/L인 항균제 조성물을 제조하였다. 상기 항균제 조성물을 신발 깔창에 스프레이 코팅하고 6시간 동안 온풍 건조한 후에 항균시험인 KS K 0693:2011의 시험방법에 따라 세균 A(Staphylococcus aureus ATCC 6538) 및 세균 B(Klebsiella pneumoniae ATCC 4352)에 대한 항균 성능을 측정하여 아래 표 1 내지 표 4에 나타내었다.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. After spray coating the antimicrobial composition on a shoe insole and drying for 6 hours with warm air, the antimicrobial performance against bacteria A (Staphylococcus aureus ATCC 6538) and bacteria B (Klebsiella pneumoniae ATCC 4352) according to the test method of the antimicrobial test KS K 0693: 2011. Was measured and shown in Tables 1 to 4 below.
표 1 내지 표 4에서 비교예 1은 실리카(SiO2, 알드리치) 나노입자를 통한 항균 시험 결과이다. 구체적으로, 실리카 나노입자를 10ppm 용액으로 제조하여 신발 깔창에 분무하여 건조 후 항균실시를 한 결과이다. 또한, 비교예 2는 산화아연(ZnO, 알드리치) 나노입자를 통한 항균 시험 결과이다. 구체적으로, 산화아연 나노입자를 10ppm 용액으로 제조하여 신발 깔창에 분무하여 건조 후 항균실시를 한 결과이다. 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. In addition, 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.
<표 1>TABLE 1
Figure PCTKR2017005748-appb-I000001
Figure PCTKR2017005748-appb-I000001
<표 2>TABLE 2
Figure PCTKR2017005748-appb-I000002
Figure PCTKR2017005748-appb-I000002
<표 3>TABLE 3
Figure PCTKR2017005748-appb-I000003
Figure PCTKR2017005748-appb-I000003
<표 4>TABLE 4
Figure PCTKR2017005748-appb-I000004
Figure PCTKR2017005748-appb-I000004
상기 표 1 내지 표 4를 통해 알 수 있는 바와 같이, 본 발명의 제조예 및 실시예에 따른 나노입자를 통한 향균 실험 결과 최초 95.8%, 최대 99.9%의 향균 효과가 나타났으며, 이는 비교예 1 및 비교예 2에 따른 향균 실험 결과에 비해 현저히 높은 수치임을 알 수 있었다. As can be seen through Table 1 to Table 4, 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.
전술한 본 발명의 설명은 예시를 위한 것이며, 본 발명이 속하는 기술분야의 통상의 지식을 가진 자는 본 발명의 기술적 사상이나 필수적인 특징을 변경하지 않고서 다른 구체적인 형태로 쉽게 변형이 가능하다는 것을 이해할 수 있을 것이다. 그러므로 이상에서 기술한 실시예들은 모든 면에서 예시적인 것이며 한정적이 아닌 것으로 이해해야만 한다. 예를 들어, 단일형으로 설명되어 있는 각 구성 요소는 분산되어 실시될 수도 있으며, 마찬가지로 분산된 것으로 설명되어 있는 구성 요소들도 결합된 형태로 실시될 수 있다.The foregoing description of the present invention is intended for illustration, and it will be understood by those skilled in the art that the present invention may be easily modified in other specific forms without changing the technical spirit or essential features of the present invention. will be. Therefore, it should be understood that the embodiments described above are exemplary in all respects and not restrictive. For example, each component described as a single type may be implemented in a distributed manner, and similarly, components described as distributed may be implemented in a combined form.
본 발명의 범위는 후술하는 청구범위에 의하여 나타내어지며, 청구범위의 의미 및 범위 그리고 그 균등 개념으로부터 도출되는 모든 변경 또는 변형된 형태가 본 발명의 범위에 포함되는 것으로 해석되어야 한다.The scope of the invention is indicated by the following claims, and it should be construed that all changes or modifications derived from the meaning and scope of the claims and their equivalents are included in the scope of the invention.

Claims (13)

  1. 평균 입도가 5~400nm인 탄소족 비산화물 나노입자를 포함하는 항균제.An antimicrobial agent comprising carbon group non-oxide nanoparticles having an average particle size of 5 to 400 nm.
  2. 제1항에 있어서,The method of claim 1,
    상기 탄소족 비산화물 나노입자의 표면에 형성된 제1 산화물층을 더 포함하는 항균제.The antimicrobial agent further comprises a first oxide layer formed on the surface of the carbon group non-oxide nanoparticles.
  3. 제1항에 있어서,The method of claim 1,
    상기 탄소족 비산화물 나노입자는 Si, Ge, B, C 및 Sn으로 이루어진 군에서 선택된 하나, 또는 2 이상의 합금 또는 화합물인 항균제.The carbon group non-oxide nanoparticles are Si, Ge, B, C and Sn is one or two or more alloys or compounds selected from the group of antibacterial agents.
  4. 제1항에 있어서,The method of claim 1,
    상기 탄소족 비산화물 나노입자의 표면에 형성된 탄소층을 더 포함하는 항균제.The antimicrobial agent further comprises a carbon layer formed on the surface of the carbon group non-oxide nanoparticles.
  5. 제4항에 있어서,The method of claim 4, wherein
    상기 탄소층의 두께는 100nm 이하인 항균제.An antimicrobial agent having a thickness of the carbon layer is 100 nm or less.
  6. 제2항에 있어서,The method of claim 2,
    상기 제1 산화물층의 표면에 카르복실기, 하이드록실기 및 알콕시기로 이루어진 군에서 선택된 하나 이상의 작용기가 결합된 항균제.An antimicrobial agent having at least one functional group 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.
  7. 제2항에 있어서,The method of claim 2,
    상기 제1 산화물층의 표면에 형성된 붕소 산화물로 이루어진 제2 산화물층을 더 포함하는 항균제.The antimicrobial agent further comprises a second oxide layer made of boron oxide formed on the surface of the first oxide layer.
  8. (a) 제1 산화물층이 형성된 탄소족 비산화물 나노입자를 제조하는 단계;(a) preparing a carbon group non-oxide nanoparticle having a first oxide layer formed thereon;
    (b1) 상기 탄소족 비산화물 나노입자를 알코올, 카르복실산, 붕산 수용액 및 물로 이루어진 군에서 선택된 하나와 혼합하여 혼합액을 제조하는 단계; 및(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) 상기 혼합액에 초음파를 인가하는 단계;를 포함하는 항균제의 제조방법.(c1) applying an ultrasonic wave to the mixed solution.
  9. (a) 제1 산화물층이 형성된 탄소족 비산화물 나노입자를 제조하는 단계;(a) preparing a carbon group non-oxide nanoparticle having a first oxide layer formed thereon;
    (b2) 상기 탄소족 비산화물 나노입자를 붕산 및 유기용매를 포함하는 제1 용액과 혼합하여 제1 혼합액을 제조하는 단계;(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) 상기 제1 혼합액에 초음파를 인가하여 상기 제1 산화물층 상에 붕소 산화물로 이루어진 제2 산화물층이 형성된 탄소족 비산화물 나노입자를 수득하는 단계;(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) 상기 탄소족 비산화물 나노입자를 알코올, 카르복실산, 붕산 수용액 및 물로 이루어진 군에서 선택된 하나와 혼합하여 제2 혼합액을 제조하는 단계; 및(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) 상기 제2 혼합액에 초음파를 인가하는 단계;를 포함하는 항균제의 제조방법.(e) applying an ultrasonic wave to the second mixed solution;
  10. 제8항 또는 제9항에 있어서,The method according to claim 8 or 9,
    상기 (a) 단계는 탄소족 원소를 포함하는 하나 이상의 원료가스와 촉매가스를 포함하는 혼합가스에 레이저를 조사하여 이루어지는 항균제의 제조방법.The step (a) is a method for producing an antimicrobial agent by irradiating a laser to a mixed gas containing at least one source gas and a catalyst gas containing a carbon group element.
  11. 제10항에 있어서,The method of claim 10,
    상기 촉매가스는 육불화황인 항균제의 제조방법.The catalyst gas is a sulfur hexafluoride method of producing an antimicrobial agent.
  12. 제8항 또는 제9항에 있어서,The method according to claim 8 or 9,
    상기 (a) 단계 이후에 상기 탄소족 비산화물 나노입자 및 탄소계 가스를 포함하는 혼합물에 레이저를 조사하여 상기 탄소족 비산화물 나노입자의 표면에 탄소층을 형성하는 단계를 더 포함하는 항균제의 제조방법.After the step (a) to produce a antimicrobial agent further comprises the step of forming a carbon layer on the surface of the carbon group non-oxide nanoparticles by irradiating a laser to the mixture containing the carbon group non-oxide nanoparticles and carbon-based gas Way.
  13. 제9항에 있어서,The method of claim 9,
    상기 (b2) 단계에서 상기 유기용매는 비극성인 항균제의 제조방법.In the step (b2), the organic solvent is a non-polar antimicrobial preparation method.
PCT/KR2017/005748 2016-06-01 2017-06-01 Antimicrobial agent comprising carbon-group non-oxide nanoparticles, and production method therefor WO2017209545A1 (en)

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US5985175A (en) * 1998-08-19 1999-11-16 Osram Sylvania Inc. Boron oxide coated phosphor and method of making same
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US5985175A (en) * 1998-08-19 1999-11-16 Osram Sylvania Inc. Boron oxide coated phosphor and method of making same
KR20070098781A (en) * 2004-10-04 2007-10-05 라이브니츠-인스티투트 퓌어 노이에 마테리알리엔 게마인누찌게 게엠베하 Method for production of nanoparticles with custom surface chemistry and corresponding colloids
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