WO2016032227A1 - Procédé de préparation de nanomatériau in situ pourvu d'un revêtement de matériau fonctionnel, et nanomatériau préparé au moyen de ce procédé - Google Patents

Procédé de préparation de nanomatériau in situ pourvu d'un revêtement de matériau fonctionnel, et nanomatériau préparé au moyen de ce procédé Download PDF

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WO2016032227A1
WO2016032227A1 PCT/KR2015/008923 KR2015008923W WO2016032227A1 WO 2016032227 A1 WO2016032227 A1 WO 2016032227A1 KR 2015008923 W KR2015008923 W KR 2015008923W WO 2016032227 A1 WO2016032227 A1 WO 2016032227A1
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nanomaterial
organic
gas
coating
transition metal
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Korean (ko)
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김성인
최선용
신명선
이규항
김중길
이순직
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재단법인 철원플라즈마 산업기술연구원
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Publication of WO2016032227A1 publication Critical patent/WO2016032227A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
    • B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units

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  • the present invention relates to a method of manufacturing a nanomaterial in situ and simultaneously coating a surface with a functional material. More specifically, an organic material or a transition that provides functionality while simultaneously preparing a nanomaterial in situ using a thermal plasma.
  • the present invention relates to a method for producing a desired functional nanomaterial by coating a surface of a nanomaterial with a metal or the like, and a functional organic-coated nanomaterial prepared thereby.
  • Nanomaterials which represent a significant portion of advanced materials, exceeded $ 1.7 billion in global market size in 2010, with an average annual growth rate of 10.4% over five years (nanotech global market of $ 16 billion).
  • North America has a 38% market and about 25% growth
  • Europe has a 37% market and about 22% growth
  • Asia has a 25% market and about 32% growth.
  • Markets in Asia are expected to grow rapidly, accounting for the largest portion of the global market.
  • the nanomaterials market is expected to grow 23 percent annually to $ 5.8 billion by 2016, led by the health and energy storage industry.
  • Nanomaterials can be said to use materials size dependence in the nanometer-sized region (1-100 nanometers), which is much smaller than the micron-submicron (sub-micron) -sized structures of conventional materials.
  • the peculiarity is that the material properties of the material change continuously in proportion to (or inversely) the size of the material until the material's tissue becomes small to submicron, but when it decreases to the nanometer size area, it shows a sudden change or a completely new property. It is indicated.
  • Nanomaterials can be said to utilize materials that change discontinuously or newly appearing properties in the nanometer range.
  • metal nanoparticles have attracted attention as materials used for wiring and electrode formation due to miniaturization and high functionality of electronic devices.
  • the particle size of the metal particles is about 100 nm, the sintering temperature thereof is lowered to 200 or less, and the metal particles can form bonds between the metal particles even at a relatively low temperature.
  • the metal particles can be used as wiring materials having low resistance regardless of the substrate material.
  • These metal nanoparticles are particularly important because they can be applied to a flexible substrate.
  • metal nanoparticles there are various methods for making metal nanoparticles, such as spray manufacturing, sol-gel method, and electroexplosive method, etc.
  • the manufacturing process is difficult, and it is difficult to obtain high quality powder due to the deterioration of characteristics due to the oxide film formed during manufacturing. It is known.
  • the raw materials are evaporated or made into nano-sized microparticles using plasma, and then the particles are collected using cold traps, sieves, cyclone, etc. Agglomeration occurs in the collection process even when not in contact with the outside, and there has been a problem that the surface is oxidized in contact with air while being transported for other uses.
  • the present inventors while making efforts to find a method for preventing aggregation, improving dispersibility, and solving surface oxidation in manufacturing nanomaterials including metals, metal oxides, ceramic carbon nanocomposites, and the like, By coating organic materials or transition metals with in situ, it was confirmed that the production of nanomaterials and coating of functional materials at the same time was completed.
  • Another object of the present invention is to provide various uses of the organic material or transition metal coated nanomaterial prepared by the above method.
  • the present invention provides an in situ method of manufacturing an organic material or a transition metal-coated nanomaterial, which includes, in one embodiment:
  • step (a)
  • Argon gas is preferably used as the gas used in thermal plasma generation, and the nanomaterial may be a metal or metal oxide present as a solid at room temperature; Magnetic nanomaterials; Alternatively, a nanometal-graphene fusion having a structure in which nanometals are crystallized in a carbon-based material may be used.
  • the metal or metal oxide may be B, C, Mg, Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Y, Zr, Nb, Mo, Ag, In, Sn, Sb, Ta, W and one or more materials selected from the group consisting of a combination thereof, the magnetic nanomaterial may be used Sr-ferrite or Br-ferrite.
  • Ni and SrFe 12 O 19 was used.
  • the nanomaterial is characterized in that the nucleus growth while passing through the plasma by the step (a).
  • quenching may be accomplished by injection of a quenching gas, preferably using argon gas.
  • a quenching gas preferably using argon gas.
  • the size of the nano material can be controlled by the rapid cooling in the range of 10 ⁇ 150nm.
  • the organic material is benzene, aniline, dopamine, phenol, phenol, benzylamine, phenethylamine, pyrocatechol, 2-hydroxypyridine. (hydroxypyridine), 3-hydroxypyridine, 4-hydroxypyridine, anthracene, naphthalene, naphthalene, 2-naphthol, 9-anthracenol, 2-anthra
  • One or more compounds selected from the group consisting of cesenol (anthracenol) and 1-anthracenol can be used, preferably benzene, aniline, or dopamine. In one embodiment of the present invention was used aniline.
  • the thickness of the organic material or the transition metal coating layer is formed to 10 to 50 nm, preferably 20 to 40 nm.
  • the organic material coated nanomaterial prepared by the method is 20 to 40 nm
  • the nanomaterial is Ni or SrFe 12 O 19
  • the organic substance is aniline Nanomaterials can be provided.
  • the present invention manufactures a nanomaterial in situ using a thermal plasma, and simultaneously coats the surface of the nanomaterial with an organic material or a transition metal that imparts functionality, thereby producing a desired functional nanomaterial.
  • a thermal plasma By functionalizing the surface to increase its properties, it is possible to provide a nanomaterial that solves the problems of anti-aggregation, improved dispersibility and surface oxidation, and furthermore, it may be usefully used for various purposes.
  • FIG. 1 is a conceptual diagram of a thermal plasma apparatus that can be used in the in situ manufacturing method of the nanomaterial of the present invention.
  • Figure 2 is a schematic diagram of the temperature profile in the in situ manufacturing method of the nanomaterial of the present invention can determine the introduction of the coating material.
  • FIG. 3 is a FE-SEM photograph of a nanomaterial prepared by coating a nickel (Ni) nanomaterial with aniline.
  • Figure 4 is a graph of the FT-IR results for nanomaterials prepared by coating nickel (Ni) nanomaterials with aniline.
  • FIG. 5 is an FE-SEM photograph of a nanomaterial prepared by coating a SrFe 12 O 19 nanomaterial with aniline.
  • FIG. 6 is a schematic configuration diagram of a plasma processing apparatus according to the present invention.
  • the present invention relates to a method for coating a surface with a functional material while preparing a nanomaterial in situ using a plasma method, preferably a thermal plasma method, and in another aspect, coating a functional material (organic material, transition metal, etc.)-Coating. It may be represented by the prepared nanomaterial manufacturing method.
  • nanomaterial refers to a material using the size dependence of physical properties in the nanometer size region (1 ⁇ 100 nanometers), the present invention includes all the various fields such as metal, ceramic, polymer. Preferably, nanomaterials such as metals, metal oxides and ceramics are included. The application of such nanomaterials is possible in various forms such as powder form, tube form or whisker form, thin film form and bulk form.
  • coating or “surface treatment” refers to a process in which functional materials such as organic materials and transition metals, which are coating materials, are laminated on the surface of the nanomaterial, or a process in which the surface of the nanomaterial is recombined with a gaseous environment and plasma discharge.
  • the method of growing or coating a thin film at the same time as synthesizing a material having various chemical components and crystal structure in a vaporized state can be largely classified into chemical vapor deposition and physical vapor deposition.
  • One of the techniques for coating a thin film in such a gas state is a plasma spray coating method.
  • the method of the present invention is characterized by using a thermal plasma process.
  • Thermal plasma is a gas composed mainly of electrons, ions, and neutral particles generated by arc discharge, and forms a high-speed jet flame having 1,000 to 20,000 and 100 to 2,000 m / s.
  • thermal plasma By using the characteristics of thermal plasma having high temperature, high heat capacity, high speed, and a large amount of active particles, it is used as various and efficient high temperature heat sources or physicochemical reactors which cannot be produced by conventional technology, and is used in various industrial fields.
  • a plasma apparatus for generating a direct current or an alternating arc (Arc) discharge and a high frequency plasma using a radio frequency magnetic field are mainly used.
  • a high frequency plasma is used.
  • the high frequency induction discharge is electrodeless, and there is usually a discharge portion in the quartz tube wound around the outer side.
  • a high frequency current flows through a coil, an induction current flows to a discharge part together with an induction magnetic field that changes at the same cycle, thereby generating heat of resistance and maintaining a thermal plasma state normally.
  • Such high frequency thermal plasma is called inductively coupled plasma, and since the prototype of the quartz tube torch generating high frequency induced plasma has been released in the early 1960s, its structure has not changed fundamentally but various developments have been made. Torch is developed and marketed.
  • Thermal plasma apparatus acts as a heat source that melts and vaporizes a target material at high temperature and high temperature to cause physical phase change, or acts as a chemical reactor to promote chemical reaction by radicals such as ions, excited atoms, and molecules generated.
  • the material process technology related to the present invention has high functional surface modification, new material creation, new material production and processing using heat plasma.
  • Plasma spray coating, plasma synthesis, thermal plasma chemical vapor deposition (TPCVD), metallurgy, material densification, physical property analysis, cutting welding, and surface strengthening, which are used in the present invention, are examples.
  • the present invention provides a technique for creating a new material by using a thermal plasma and creating a new material coated with a heterogeneous material (organic material, transition metal) on the surface of the generated new nano material.
  • the present invention provides a method for producing a nanomaterial coated with a functional material, characterized in that the coating of the desired functional material at the same time to produce a nanomaterial using the thermal plasma method (Fig. 1).
  • the method of the present invention is carried out in-situ.
  • the in-situ method of the present invention is a functional material, for example, an organic material or a transition metal, during the production of the nanomaterial, for example, a metal or a metal oxide, during the step of producing the nanomaterial using a thermal plasma.
  • a functional material for example, an organic material or a transition metal
  • the surface of the nanomaterial is functionalized to improve its properties, or to produce functional nanomaterials for preventing aggregation, improving dispersibility and solving surface oxidation.
  • In-situ method has the following advantages compared to the method of coating the organic material separately after manufacturing the nano-material.
  • Nanomaterial synthesis and nanomaterial coating are carried out in-situ in a thermal plasma device, resulting in lower process manufacturing costs, shorter process times, and simplified process steps.
  • Conventional coating process has a disadvantage in that the process manufacturing cost is high, the process time is long, and the process step is very complicated because the separate coating process to build a nanomaterial synthesis equipment, nanomaterial coating equipment separately.
  • the simultaneously coated surface is very uniform and free of defects since the synthesis and coating of the nanomaterials takes place in a short time.
  • the present invention may provide a method for preparing an in situ of an organic material or a transition metal-coated nanomaterial, comprising the following steps:
  • Nanomaterial raw material (nanomaterial) injection step Nanomaterial raw material (nanomaterial) injection step
  • the desired coating material is put in the temperature range that can be vaporized or activated
  • the desired coating material is vaporized or activated
  • the gases used may be classified into sheath gas, central gas, carrier gas, and the like according to their function, and include such gases as inert gas such as argon, hydrogen and nitrogen. Or a gas mixed with these may be used. Preferably argon gas is used.
  • the sheath gas is injected to prevent the vaporized particles from adhering to the inner surface of the wall and also to protect the wall from the ultra-high temperature plasma, and may use an argon gas of 30 to 150 lpm (liters per minute). Is a gas injected to generate a high temperature thermal plasma, argon gas of 30 ⁇ 120 lpm can be used, the carrier gas is a gas for supplying the mixed powder into the plasma reactor, argon gas of 3 ⁇ 20 lpm Can be used.
  • the gas supplier 1 supplies various auxiliary gases such as hydrogen and oxygen gas other than argon gas supplied to the plasma discharge and the plasma torch electrode unit and the cooling unit in the plasma reaction unit and the cooling unit 7, Through the central gas supply line 4b, the sheath gas supply line 4c, and the carrier gas supply line 4a, respectively, through the injection nozzles of the plasma generating electrode part 6, the plasma reaction part, and the cooling part 7, respectively. Supply.
  • auxiliary gases such as hydrogen and oxygen gas other than argon gas supplied to the plasma discharge and the plasma torch electrode unit and the cooling unit in the plasma reaction unit and the cooling unit 7, Through the central gas supply line 4b, the sheath gas supply line 4c, and the carrier gas supply line 4a, respectively, through the injection nozzles of the plasma generating electrode part 6, the plasma reaction part, and the cooling part 7, respectively.
  • the nanomaterial is a material in the range of 1 to 100 billion minutes, in the present invention, a metal or metal oxide present as a solid at room temperature; Or a carbon-based or ceramic-based material, and more preferably selected from any of alkali metals, alkaline earth metals, lanthanum groups, actinium groups, transition metals, post-transition metals, and metalloids on the periodic table of the elements.
  • B, C, Mg, Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Sr, Y, Zr, Nb, Mo, Ag, In, Sn, Sb , Ta, W, or a combination thereof may be used.
  • the raw material feeder 3 is a quantitative powder feeder, and supplies the nanomaterial to the plasma reaction part and the cooling part 7 together with the auxiliary gas. At this time, the raw material feeder 3 is preferably configured to apply the rotation and vibration of a constant speed so that the nanomaterial can be smoothly supplied.
  • the following nanomaterial can be used.
  • Si is a lithium secondary battery anode material, can minimize the reduction of capacity due to surface oxidation when manufacturing nano-Si to achieve the maximum theoretical capacity of 4,200 mA /, by coating the nanomaterial individual particles through the surface coating to maximize the dispersion,
  • a lithium secondary battery anode material it is possible to minimize damage to the battery due to expansion during charging and discharging caused by agglomeration of nano silicon in one place.
  • the magnetic polymer particles in which iron oxide nanoparticles are dispersed therein include, for example, ferrite nanomaterials (SrFe 12 O 19 , BaFe x O x, etc.) such as Sr-ferrite and Br-ferrite.
  • ferrite nanomaterials SrFe 12 O 19 , BaFe x O x, etc.
  • the magnetic polymer particles may be prepared by various methods.
  • the simplest method is to encapsulate iron oxide nanoparticles having superparamagnetism into a polymer. Emulsifying and polymerizing the monomer in the presence of stabilized iron oxide nanoparticles such as ferrofluid can obtain magnetic polymer particles in which the iron oxide nanoparticles are encapsulated.
  • Hydrothermal, glicinenitrate, citric acid, sol-gel, etc. may be used for nano-sized ferrite preparation, which may be referred to known techniques [M. Serkol, Y. Koseoglu, A. Batkal, H. Kavas, and A. C. Basaran, J. Magn. Magn. Mater. 321, 157 (2009); S. Hajarpour, A. H.
  • the nano-magnetic material may be improved dispersibility and orientation properties by coating the organic material, such as aniline, dopamine.
  • the organic material such as aniline, dopamine.
  • inverted spheres at the grain boundary due to nuclear growth are easily generated at the joint surface of the magnetic material, and the coercive force is lowered to about 20% of the theoretical value. Because there is.
  • other types of ferrites having a large saturation magnetization value, or core-shell structured hexaferrite nanoparticles having a metal such as Co, Ni, Mn, Ti, or nitrogen doped with nitrogen Metal hexaferrite nanoparticles may be prepared to improve magnetic properties.
  • the nanomaterial of the present invention may use a nanometal-graphene fusion form in which a nanometal is crystallized in a carbon-based material (eg, graphene, graphite, etc.).
  • a nanometal-graphene fusion form in which a nanometal is crystallized in a carbon-based material (eg, graphene, graphite, etc.).
  • a carbon-based material eg, graphene, graphite, etc.
  • a low melting metal (Sn, Ag, Al, etc.) of the transition metal By coating a low melting metal (Sn, Ag, Al, etc.) of the transition metal to the nanometal can be given a special functionality.
  • the injected nanomaterials are vaporized using thermal plasma (3).
  • the thermal plasma is an ionization gas composed of electrons, ions, atoms, and molecules generated by a plasma torch using a direct current arc or a high frequency inductively coupled discharge, and is a high-temperature jet having a high temperature and high activity ranging from thousands to tens of thousands of K. .
  • the power supply of the plasma apparatus supplies power of 10 to 70 kW, and an arc is formed by electric energy and about 10,000 K is generated by argon gas used as a thermal plasma generating gas. Ultra high temperature plasma is generated.
  • the ultra high temperature thermal plasma generated by argon gas as the generating gas while maintaining the power of 10 to 70 kW has an effect that is generated at a higher temperature than the thermal plasma generated by the heat treatment method or the combustion method.
  • the raw material vaporized by the ultra-high temperature thermal plasma forms a nucleus in the intrinsic nucleation temperature range of each material as it passes through the plasma region, and particles are grown from the nucleus formed into seeds to crystallize into nanomaterials (4).
  • Coating materials such as organic materials and transition metals, which are injected into the plasma high temperature region, are rapidly vaporized and adsorbed onto the surface of the moving nanomaterial with a flow to form a coating, which forms a core-shell structure. do.
  • the growth of the nanomaterial is suppressed by condensation or quenching by the quenching gas, and is determined as a nanomaterial having a predetermined size in the range of 10 to 150 nm. That is, the nanomaterial grown to a predetermined size is transferred by the vacuum pump 70 or the compressor, and the temperature is lowered while passing through the cyclone unit 30 connected to the plasma reaction unit and the cooling unit 7, and the cooling gas ( As the quenching gas), argon gas of 0 to 200 lpm may be injected through graphite nozzles of 2 to 4 different positions (heights), respectively.
  • the coating material that can be used can be appropriately selected by those skilled in the art according to the desired function, preferably transition metals (Co, Ni, Mn, Ti, etc.), organic matter (ammonia, dopamine, aniline, benzene, etc.) ) And the like can be used.
  • the selected coating material is added in the temperature range that can be vaporized or activated. That is, the introduction of the coating material may be determined by checking the temperature profile of the entire thermal plasma system (FIG. 2).
  • benzene, aniline, dopamine, phenol, benzylamine, phenethylamine, pyrocatechol, 2-hydroxypyridine hydroxypyridine, 3-hydroxypyridine, 4-hydroxypyridine, anthracene, naphthalene, naphthalene, 2-naphthol, 9-anthracenol, 2-anthracenol (anthracenol), and one or more compounds selected from the group consisting of 1-anthracenol can be used.
  • “Aniline” (aniline) used in one embodiment of the present invention is C 6 H 5 NH 2 , the melting point is -6.3 by maintaining the liquid state at room temperature has the advantage of easy supply to the gaseous state.
  • Aniline can be obtained by commercially hydrogenating nitrobenzene under a catalyst, by reacting chlorobenzene and ammonia, or by reducing nitrobenzene with an iron catalyst in an aqueous acid solution.
  • Aniline a primary aromatic amine, is a weak base and reacts with inorganic acids to form salts.
  • the aniline was used as a starting material.
  • dopamine may be used as a coating instead of aniline.
  • the dopamine is a monomolecular substance having a molecular weight of 153 (Da) having a catechol and an amine functional group (C 8 H 11 NO 2 ).
  • catecholamine precursor materials described above may be appropriately selected and used.
  • pyrocatechol with hydroxyl functional group (-OH) attached to the benzene ring and benzylamine with one and two methylene bridges and one amine group attached to the benzene ring, respectively.
  • Coatings such as naphthylmethylamine can also be used.
  • the coating film may be synthesized by inducing a hydroxylation reaction or an amination reaction by controlling plasma chemistry on benzene, cyclohexane and the base unit, respectively.
  • a coating layer may be formed on the surface of the nanomaterial described above. That is, the nanomaterial of the present invention is prepared by coating an organic material (metals having a low melting point, if necessary) on the nanomaterial.
  • the nano-materialization and coating process reaction for 1/100 sec to 1 / 1,000 sec at 100 MHz to 500 Torr pressure, high frequency RF (Radio Frequench) of 2MHz, 20kW ⁇ 60kW power conditions Do this.
  • the thickness of the organic coating layer can be appropriately adjusted by those skilled in the art according to the type of nanomaterial, but the coating is preferably performed in a thickness of 10 to 50 nm. In an embodiment of the present invention, the surface of the nanomaterial was coated with about 30 nm.
  • the functional material of the desired organic material or transition metal is coated on the surface of the nanomaterial (9), and finally, the functional material-coated nanomaterial is recovered (10).
  • the nanomaterial generated in the metal filter 55 made of stainless material is adsorbed, and various fluorine gas generated in the plasma process is transferred through an external tube through the vacuum pump 70. Final discharge.
  • the discharged gas may be purified and stored under pressure in the gas tank using a booster to be reused.
  • the nanomaterial collecting unit 60 provided at the lower end of the collector 50 by desorbing the nanomaterial using a blowback gas inside the filter. ).
  • the nanomaterial may be recovered in the glove box in order to avoid a reaction by contact with air.
  • the present invention encompasses various uses of nanomaterials coated with functional materials of organics or transition metals obtained by the process of the invention described above.
  • Electronic components that can be manufactured by, for example, printing methods such as printable displays, RFID, photovoltaic cells, computer memories, etc .; Heat dissipation materials for extending the life of electronic devices such as displays, lighting equipment such as LEDs, and computer parts; It is expected to be used in various fields including electrochemical devices such as next-generation electronic devices, solar cells and fuel cells.
  • the "electrochemical device” includes an energy storage device, an energy conversion device, a sensor, and other devices for converting electrical energy into chemical energy or converting chemical energy into electrical energy.
  • energy storage device as used herein includes a battery and a super capacitor.
  • Ultracapacitors and organic solar cells that use polymer materials are highly useful as clean energy storage and conversion media based on their flexibility and structure control, and organic light-emitting devices can be bent, folded and expanded in the future.
  • the company's progress is expected to cover a wide range of applications, from clothing to buildings to new types of display and lighting industries.
  • the present invention may be useful in various fields of the nanomaterial coated with a functional material of an organic material or a transition metal having excellent properties.
  • Plasma gas Ar central gas 30 lpm, sheath gas 50 lpm
  • Figure 3 shows the FE-SEM image measurement results of the aniline-coated nickel (Ni) nanomaterial (nano composite) prepared in Example 1-1.
  • Plasma gas Ar central gas 30 lpm, sheath gas 120 lpm
  • “About” means 30, 25, 20, 25, 10, 9, 8, 7, 6, 5, 4 for reference quantities, levels, values, numbers, frequencies, percentages, dimensions, sizes, quantities, weights, or lengths. , Amount, level, value, number, frequency, percentage, dimension, size, amount, weight or length, varying by about 3, 2 or 1%.

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Abstract

La présente invention concerne un procédé de préparation et de revêtement de nanomatériau in situ et, plus particulièrement, un procédé de revêtement, à l'aide d'un plasma thermique, de la surface du nanomatériau pourvu d'une matière organique qui assure la fonctionnalité, et produit simultanément un nanomatériau désiré ou nanomatériau fonctionnel; et un nanomatériau, revêtu d'une matière organique, préparé au moyen d'un plasma thermique.
PCT/KR2015/008923 2014-08-27 2015-08-26 Procédé de préparation de nanomatériau in situ pourvu d'un revêtement de matériau fonctionnel, et nanomatériau préparé au moyen de ce procédé WO2016032227A1 (fr)

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KR102600019B1 (ko) * 2016-05-19 2023-11-08 주식회사 아모그린텍 그래핀-그래핀 융합체의 제조방법 및 상기 그래핀-그래핀 융합체를 이용한 그래핀-기질 복합체의 제조방법
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KR20190099837A (ko) 2018-02-20 2019-08-28 강원대학교산학협력단 3d 구조를 갖는 탄소소재금속나노입자복합체 및 그 제조방법
KR20190100084A (ko) 2019-08-02 2019-08-28 강원대학교산학협력단 3d 구조를 갖는 탄소소재금속나노입자복합체 및 그 제조방법

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