WO2012150804A2 - Procédé de préparation d'une nanopoudre au moyen d'un support - Google Patents

Procédé de préparation d'une nanopoudre au moyen d'un support Download PDF

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Publication number
WO2012150804A2
WO2012150804A2 PCT/KR2012/003422 KR2012003422W WO2012150804A2 WO 2012150804 A2 WO2012150804 A2 WO 2012150804A2 KR 2012003422 W KR2012003422 W KR 2012003422W WO 2012150804 A2 WO2012150804 A2 WO 2012150804A2
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WO
WIPO (PCT)
Prior art keywords
carrier
nanoparticles
metal
vapor
stirring
Prior art date
Application number
PCT/KR2012/003422
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English (en)
Korean (ko)
Other versions
WO2012150804A3 (fr
Inventor
고석근
Original Assignee
주식회사 나노케미
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Filing date
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Publication of WO2012150804A2 publication Critical patent/WO2012150804A2/fr
Publication of WO2012150804A3 publication Critical patent/WO2012150804A3/fr

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Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/20—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • the present invention relates to a method for producing nanopowder using a carrier.
  • Nanoparticles are formed by the chemical process in the initial process of converting metal ions into metal solid particles by adding a reducing agent and a dispersant to the metal ions present in an aqueous solution.
  • Such chemical method is not easy to control the nanoparticle size and separation of the nanoparticles, and the characteristics of the nanoparticles vary depending on the type of redox agent, dispersant, PH, temperature, etc., the flammability side in the production of nanoparticles Has many problems.
  • a method of physically making nanoparticles by using a metal atom vapor which rapidly converts a metal atom vapor into a gas at a high temperature and expands it to a low temperature.
  • the method uses a high temperature to the metal or metal compound to produce a vapor, or by using a DC sputtering, DC-RF sputter, ECR, laser beam sputtering (electron or energy)
  • the atomic vapor generated by irradiating a solid having a particle with a solid is injected into a gas of a low temperature or passed through a region of a low temperature so that the atomic vapor is rapidly condensed to form nano-sized particles.
  • Another physical method is a mechanical grinding method in which a mechanical force is applied to the material to grind the material into fine particles. In order to process the material into nano particles having a size of 10 nm, a long grinding process is required.
  • the physical methods are 80 to 90% of the particles in the powder is formed in a micrometer size significantly larger than the nanoparticles, when the nano-particles are made by the physical method using the vacuum equipment, the particle size is uneven and productivity is low due to low productivity There is a problem falling.
  • the present invention provides a nano-powder manufacturing method characterized by generating nano-particle vapor using physical vapor deposition, and depositing nanoparticles on a carrier
  • a nano-powder manufacturing method characterized by generating nano-particle vapor using physical vapor deposition, and depositing nanoparticles on a carrier
  • an object of the present invention is to provide a method for producing a nano-powder that can effectively control the size and content of the nanoparticles by controlling the growth of the nanoparticles.
  • a vacuum deposition tank a stirring tank provided in the vacuum deposition tank; A screw provided in the stirring tank and stirring the carrier; And a nanopowder manufacturing apparatus attached to a carrier, which is provided on the stirring vessel in the vacuum deposition tank and constitutes a deposition source for generating steam particles for forming nanoparticles.
  • the nanoparticles can be uniformly formed on the carrier, so that nanoparticles attached to the carrier can be prepared with a uniform size.
  • Figure 1 is a schematic diagram showing that the movement of the nanoparticle vapor in the method of manufacturing nanopowder of the present invention using the average free path.
  • FIG. 2 is a photograph before (left) and after (right) the formation of silver nanopowders of about 40 ppm concentration on a salt carrier.
  • 3A is a photograph of before (left) and after (right) formation of silver nanoparticles on a hydroxyl ethyl cellulose (HEC) carrier.
  • HEC hydroxyl ethyl cellulose
  • 3B is a photograph of a solution in which silver nanoparticles are uniformly dispersed, obtained by dissolving HEC carrier to which silver nanoparticles are attached.
  • FIG. 4 is a photograph before (left) and after (right) before forming silver nanoparticles on a sand support.
  • FIG. 6 is a photograph of before (left) and after (right) the formation of gold nanoparticles on a sugar carrier.
  • Figure 7 is a gold nanoparticles / sugar made in Figure 6 is dissolved in water. It can be seen that the gold nanoparticles are completely dispersed to form colloids.
  • FIG. 10 is a photograph when Pd / glucose is dissolved in water in FIG. 8. It can be seen that a gray colloid is formed as a whole.
  • FIG. 11 is a photograph of the formation of silver nanoparticles on the PET plastic grains (left) and melting them at 180 degrees Celsius (right). As you can see in the picture, the silver nanoparticles are completely dissolved in PET plastic polymer and yellow.
  • the present invention a vacuum deposition tank, a stirring tank provided in the vacuum deposition tank; A screw provided in the stirring tank and stirring the carrier; And using a nano-powder manufacturing apparatus attached to the carrier, consisting of a deposition source which is provided on the stirring tank in the vacuum deposition tank and generates vapor particles for forming nanoparticles,
  • Nano powder production method of the present invention a vacuum deposition tank, the stirring tank provided in the vacuum deposition tank; A screw provided in the stirring tank and stirring the carrier; And a deposition source provided on the stirring vessel in the vacuum deposition tank and configured to generate vapor particles for forming nanoparticles, wherein the powder manufacturing apparatus attached to the carrier is used.
  • Nanoparticle manufacturing method characterized in that for controlling the vacuum degree of the vacuum deposition tank to 10 "4 to 1 torr.
  • the vacuum degree of the vacuum deposition tank to 10 "4 to 1 torr.
  • vapor particles for forming nanoparticles Two vapor particles for nanoparticle formation are deposited on the carrier near the evaporation source, but as the carriers move away from the evaporation source, the average free path of vapor particles decreases so that the vapor particles do not deposit on the carrier. do.
  • the vaporization direction of the atomized vapor is opposite to the carrier so that the metal vapor is scattered upwards, but the vacuum degree is 10 _4 to 1 torr, so that a layer stone is formed between the metal vapor particles and the inert gas particles due to the inert gas filled therein.
  • the path is shortened so that the metal vapor particles move downward by gravity and are deposited on the stirred carrier to form nanoparticles.
  • the vacuum degree of the vacuum deposition tank is controlled by including an inert gas, and the inert gas may be argon (Ar), ne (Ne), N 2 , 0 2 , CH 4, etc., but is not limited thereto.
  • the step of generating steam particles for forming nanoparticles using the deposition source may use physical vapor deposition, for example, resistance heating, plasma heating, induction heating. , Thermal deposition such as laser heating, DC sputtering, DC RF sputtering, laser sputtering, electron beam deposition (E-Beam Evaproation), and the like, but are not necessarily limited thereto.
  • metals, metal compounds, organic materials, and the like may be used, but are not necessarily limited thereto.
  • Cobalt, copper, silver, nickel, manganese, palladium, indium, iron, tungsten, titanium, alloys thereof may be used as the metal, but is not necessarily limited thereto.
  • the metal compound may be a metal oxide, a metal nitride, a metal carbide, or a metal carbon nitride, but is not limited thereto.
  • the metal compound examples include alumina (A1 2 0 3 ), a metal oxide, tungsten carbide (WC), a metal carbide, nitrogen aluminum (A1N), a metal nitride, and titanium carbonitride (TiCN), a metal carbon nitride. It is not necessarily limited thereto.
  • the carrier may be activated carbon, a hydrocarbon compound, alumina (A1 2 0 3 ), tungsten carbide (WC), glass, sand, or a material soluble in water or a solvent, such as glucose, sugar, Salt, PMMA, hydroxyl ethyl cellulose (HEC), PET, PTFE and the like can be used.
  • a hydrocarbon compound such as alumina (A1 2 0 3 ), tungsten carbide (WC), glass, sand, or a material soluble in water or a solvent, such as glucose, sugar, Salt, PMMA, hydroxyl ethyl cellulose (HEC), PET, PTFE and the like can be used.
  • stirring speed is less than 1 rpm, there is a problem that the steam particles are not uniformly adhered to the surface of the carrier because the stirring is not made sufficiently, there is a problem that the stirred carrier is scattered when the stirring speed exceeds 200 rpm.
  • a method for manufacturing nanopowders may control the growth of nanoparticles by controlling the degree of vacuum degree of a deposition screw and the like, thereby effectively controlling the size and content of the nanopowders.
  • Nanoparticle manufacturing method characterized in that it comprises the step of depositing vapor particles on the carrier to form nanoparticles.
  • vapor particles for forming nanoparticles are deposited on the carrier to form a nucleus for forming the nanoparticles, and then the nucleus further forms the vapor particles.
  • the carrier is stirred and rotated to mix, and vapor particles are deposited on a new carrier on which no vapor particles are deposited or on a carrier site on which no vapor particles are deposited, thereby providing a uniform size. Nanoparticles can be formed.
  • the vapor particles for forming the nanoparticles are deposited on the carrier at a thickness of 1 A to 10 per unit area per minute.
  • further reaction may be performed to synthesize the final male material. That is, the carrier and the vapor particles to be deposited can react to form oxide, nitride, carbide or carbonitride nanopowders.
  • nitrogen aluminum (A1N), alumina (A1 2 0 3 ), metal carbide, metal nitride, and the like which have been conventionally synthesized at a high temperature / high pressure, are manufactured at low temperature according to the manufacturing method of the present invention. Can be synthesized and coated.
  • tungsten carbide (WC) or cobalt (Co) is doped by forming tungsten nanoparticles on an activated carbon carrier or cobalt (Co) nanoparticles on a tungsten powder and then carbonizing in an inert gas atmosphere.
  • Nano tungsten carbide can be synthesized.
  • the male product can be manufactured by subsequent treatment.
  • a substance that is well soluble in water, a polar organic solvent and a non-polar organic solvent is used as a carrier, and after the nanoparticles are formed on such a carrier, the carrier is dissolved and removed. It can also be recovered.
  • the salt is agitated by a rotating screw provided in the stirring vessel, wherein the stirring speed of the salt by the screw is maintained below lOOrpm.
  • the silver vapor was deposited on a salt carrier to prepare a salt-silver nanopowder in which silver nanoparticles were attached to salt at a concentration of about 40 ppm.
  • Example 1 except that the use of hydroxyl ethyl cellulose (HEC) as a carrier and silver as a deposition source was carried out in the same manner as in Example 1, HEC-silver nano Powder was prepared.
  • HEC hydroxyl ethyl cellulose
  • Example 1 except that water is used as a carrier and silver is used as a deposition source, the water-silver nanopowder was prepared in the same manner as in Example 1.
  • Example 1 except that sand is used as a carrier and silver is used as a deposition source, it was carried out in the same manner as in Example 1, to prepare a sand ⁇ nanopowder.
  • Example 1 except that salt is used as a carrier and Si is used as a deposition source, it was carried out in the same manner as in Example 1, to prepare a salt-Si nano powder.
  • Example 1 except that sugar is used as a carrier and gold is used as a deposition source, it was carried out in the same manner as in Example 1, to prepare a sugar-gold nanopowder.
  • Example 1 except that sugar is used as a carrier and platinum is used as a deposition source, it was carried out in the same manner as in Example 1, to prepare a sugar-platinum nano powder.
  • Example 8 Preparation of Glucose-Pd Nanopowder
  • glucose was used as a carrier and Pd was used as a deposition source
  • the same procedure as in Example 1 was performed to prepare glucose-Pd nanopowder.
  • PET-silver nanopowder was prepared in the same manner as in Example 1 except for using PET as a carrier and silver as a deposition source.
  • Example 1 PTFE-silver nanopowder was prepared in the same manner as in Example 1 except that PTFE (Teflon) was used as the carrier and silver was used as the deposition source. In Examples 1 to 10, the appearance change of the carrier was visually observed.
  • Figure 2 is a photograph before and after making the silver nano powder of about 40ppm concentration on a salt carrier. As shown in the picture, the initial salt color was white, but it turned to pale yellow, which shows that silver nanoparticles were formed.
  • FIG. 3A is a photograph before and after forming silver nanoparticles on a hydroxyl ethyl cellulose (HEC) carrier.
  • HEC hydroxyl ethyl cellulose
  • sand has a bright color before forming silver nanoparticles, and then turned to a light dark color after forming silver nanoparticles.
  • 5 is a photograph of before (left) and after (right) the formation of Si nanoparticles on a salt carrier. As shown in the picture, the salt carrier was white before the formation of the nanoparticles, but after the Si nanoparticles were formed on the salt carrier, it was found to be pale yellow green.
  • 6 is a photograph of before (left) and after (right) the formation of gold nanoparticles on a sugar carrier. As shown in the picture, the sugar carrier has a deep purple color, which is inherent in the gold nanoparticles, after the gold nanoparticles are formed.
  • FIG. 7 shows the gold nanoparticles / sugar made in FIG. 6 dissolved in water. It can be seen that the gold nanoparticles are completely dispersed to form colloids.
  • FIG 8 is a photograph of before (left) and after (right) the formation of platinum nanoparticles on a sugar carrier. As shown in the picture, it can be seen that the sugar carrier has gray, which is intrinsic color of the platinum nanoparticles after the formation of the platinum nanoparticles.
  • FIG. 9 is a photograph of before (left) and after (right) the formation of Pd nanoparticles on a glucose carrier. As shown in the photo, glucose is gray after Pd nanoparticles are formed on the glucose carrier , because Pd becomes nanoparticles.
  • FIG. 10 is a photograph when Pd / glucose is dissolved in water in FIG. 8. It can be seen that a gray colloid is formed as a whole.
  • FIG. 11 is a photograph of silver nanoparticles formed on PET plastic grains (left) and melted at 180 degrees Celsius (right). As you see in the picture
  • the silver nanoparticles are completely dissolved in the PET plastic polymer and are yellow in general.
  • FIG. 12 is a photograph of silver nanoparticles formed on PTFE (teflon) powder (left) and melted at 250 ° C. high temperature (right). As you can see in the picture, the yellow nanoparticles appear to be uniformly mixed with Teflon polymer.

Abstract

La présente invention concerne un procédé de préparation d'une nanopoudre fixée à un support. Ledit procédé utilise un dispositif pour préparer une nanopoudre fixée à un support, et le dispositif comprend une chambre d'évaporation sous vide; une chambre d'agitation disposée à l'intérieur de la chambre d'évaporation sous vide; une vis placée à l'intérieur de la chambre d'agitation pour agiter un support; et une source d'évaporation disposée sur la partie supérieure de la chambre d'agitation dans la chambre d'évaporation sous vide pour produire une particule vapeur de manière à former une nanoparticule. Ledit procédé consiste à introduire un gaz inerte dans la chambre d'évaporation sous vide de sorte que le degré de vide la chambre d'évaporation atteigne 10-4-1 torr; b) générer la particule vapeur pour former la nanoparticule au moyen de la source d'évaporation; c) agiter le support conjointement à l'ajustement de la vitesse de la vis à 1-200rpm; et d) former la nanoparticule par évaporation de la particule vapeur sur le support.
PCT/KR2012/003422 2011-05-02 2012-05-02 Procédé de préparation d'une nanopoudre au moyen d'un support WO2012150804A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020110041584A KR20120123940A (ko) 2011-05-02 2011-05-02 담체를 이용한 나노 파우더 제조 방법
KR10-2011-0041584 2011-05-02

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WO2012150804A2 true WO2012150804A2 (fr) 2012-11-08
WO2012150804A3 WO2012150804A3 (fr) 2013-03-21

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KR102157222B1 (ko) * 2020-04-21 2020-09-17 박정덕 식품에 미네랄 성분을 보충하는 방법, 장치 및 식품
KR102400125B1 (ko) * 2021-03-09 2022-06-23 주식회사 삼우엠스 항균 부직포, 그 제조방법 및 이를 포함하는 제품

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070044879A (ko) * 2005-10-26 2007-05-02 주식회사 피앤아이 금속, 합금 및 세라믹 나노 입자가 균일하게 진공 증착된파우더의 형성 방법 및 그 제조 장치
KR100835207B1 (ko) * 2007-05-31 2008-06-09 대한민국(관리부서:농촌진흥청장) 은 나노입자를 함유한 천연실크 및 그의 제조방법
JP2009079251A (ja) * 2007-09-26 2009-04-16 Ulvac Japan Ltd 金属蒸着装置および同装置における粉体状担体の撹拌方法
KR20100086907A (ko) * 2009-01-23 2010-08-02 세종대학교산학협력단 진공 건식 증착 분말 교반장치

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20070044879A (ko) * 2005-10-26 2007-05-02 주식회사 피앤아이 금속, 합금 및 세라믹 나노 입자가 균일하게 진공 증착된파우더의 형성 방법 및 그 제조 장치
KR100835207B1 (ko) * 2007-05-31 2008-06-09 대한민국(관리부서:농촌진흥청장) 은 나노입자를 함유한 천연실크 및 그의 제조방법
JP2009079251A (ja) * 2007-09-26 2009-04-16 Ulvac Japan Ltd 金属蒸着装置および同装置における粉体状担体の撹拌方法
KR20100086907A (ko) * 2009-01-23 2010-08-02 세종대학교산학협력단 진공 건식 증착 분말 교반장치

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WO2012150804A3 (fr) 2013-03-21

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