[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

WO2005066069A1 - Procede de production de microparticules et appareil associe - Google Patents

Procede de production de microparticules et appareil associe Download PDF

Info

Publication number
WO2005066069A1
WO2005066069A1 PCT/JP2004/019354 JP2004019354W WO2005066069A1 WO 2005066069 A1 WO2005066069 A1 WO 2005066069A1 JP 2004019354 W JP2004019354 W JP 2004019354W WO 2005066069 A1 WO2005066069 A1 WO 2005066069A1
Authority
WO
WIPO (PCT)
Prior art keywords
fine particles
liquid
gas
fluid
powder
Prior art date
Application number
PCT/JP2004/019354
Other languages
English (en)
Japanese (ja)
Inventor
Seiichiro Takahashi
Hiroshi Watanabe
Original Assignee
Mitsui Mining & Smelting Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsui Mining & Smelting Co., Ltd. filed Critical Mitsui Mining & Smelting Co., Ltd.
Priority to JP2005516840A priority Critical patent/JP4864459B2/ja
Priority to US10/584,069 priority patent/US20070163385A1/en
Priority to KR1020067013332A priority patent/KR100907735B1/ko
Publication of WO2005066069A1 publication Critical patent/WO2005066069A1/fr

Links

Classifications

    • 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
    • C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
    • C01B13/322—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the solid state
    • 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
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • 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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005—Separating solid material from the gas/liquid stream
    • B01J8/0055—Separating solid material from the gas/liquid stream using cyclones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/026—Spray drying of solutions or suspensions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • 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
    • C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
    • C01B13/326—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process of elements or compounds in the liquid state
    • 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
    • C01B13/34—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of sprayed or atomised solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/0821—Oxynitrides of metals, boron or silicon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G1/00—Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general
    • C01G1/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00108—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant vapours
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00112—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant solids
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2219/00114—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling involving reactant slurries
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00121—Controlling the temperature by direct heating or cooling
    • B01J2219/00123—Controlling the temperature by direct heating or cooling adding a temperature modifying medium to the reactants
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00159—Controlling the temperature controlling multiple zones along the direction of flow, e.g. pre-heating and after-cooling
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0877—Liquid
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0879—Solid
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0894—Processes carried out in the presence of a plasma
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram

Definitions

  • the present invention relates to a method and an apparatus for producing fine particles such as indium tin oxide powder.
  • a sputtering method is known as one of the methods for forming a thin film.
  • the sputtering method is a method of obtaining a thin film by sputtering a sputtering target, and is used industrially because a large area can be easily formed and a high-performance film can be efficiently formed.
  • a reactive sputtering method in which sputtering is performed in a reactive gas
  • a magnetron sputtering method in which a magnet is provided on a back surface of a target to perform high-speed thin film formation are known. I have.
  • an indium oxide-oxide oxide (InO-SnO composite oxide, hereinafter referred to as "ITO”) film has high visible light transmittance.
  • ITO indium oxide-oxide oxide
  • Such a sputtering target is obtained by mixing an indium oxide powder and a tin oxide powder at a predetermined ratio, molding the mixture by a dry or wet method, and sintering it (Patent Document 1).
  • Highly dispersible indium oxide powder for obtaining a compact has been proposed (see Patent Documents 2, 3, and 4).
  • the following method has been proposed as a method for producing metal oxide fine particles, not a method for producing ITO powder.
  • various methods have been proposed in which a metal powder is supplied into a pana flame to produce oxidized ultrafine particles, and solid-phase separation is performed (see Patent Documents 11 to 16).
  • a method has been proposed in which a gas is injected into a molten metal to form a powder, and the powder conveyed by the gas is introduced into a liquid to cause a reaction such as a chemical reaction and concentration to produce a fine powder. (See Patent Document 17).
  • Patent Document 1 JP-A-62-21751
  • Patent Document 2 JP-A-5-193939
  • Patent Document 3 JP-A-6-191846
  • Patent Document 4 JP 2001-261336 A
  • Patent Document 5 JP-A-62-21751
  • Patent Document 6 Japanese Patent Application Laid-Open No. 9-221322
  • Patent Document 7 JP-A-2000-281337
  • Patent Document 8 JP 2001-172018 A
  • Patent Document 9 JP-A-2002-68744
  • Patent Document 10 JP-A-11-11946
  • Patent Document 11 Japanese Patent Publication No. 55201
  • Patent Document 12 Japanese Patent Publication No. 5-77601
  • Patent Document 13 Patent No. 3253338
  • Patent Document 14 Patent No. 3253339
  • Patent Document 15 Patent No. 3229353
  • Patent Document 16 Patent No. 3225073
  • Patent Document 17 JP-A-60-71037
  • Patent Document 18 JP-A-2002-253953
  • Patent Document 19 Japanese Patent Application Laid-Open No. 2002-253954
  • Patent Document 20 JP-A-2002-263474
  • the present invention provides a method and apparatus for producing fine particles, such as fine particles of acid oxide, which can be produced with a simpler apparatus at a low cost and which is suitable for producing ITO powder.
  • the task is to provide.
  • a raw material is supplied as a liquid stream, droplets or powder into a heat source, and a product is atomized liquid fluid.
  • the fine particles are captured as fine particles, and the fine particles are collected as a slurry by gas-liquid separation.
  • the product obtained by supplying the raw material into the heat source is captured as fine particles by the mist-like liquid fluid, and is efficiently recovered by gas-liquid separation.
  • a second aspect of the present invention resides in the method for producing fine particles according to the first aspect, wherein the molten metal power of the raw material is also formed into a liquid flow or droplets and supplied to the heat source.
  • a liquid stream or droplet of a molten metal such as a metal or an alloy as a raw material becomes an oxidizing substance in a heat source in some cases, and is captured as fine particles by a mist-like liquid fluid.
  • a third aspect of the present invention is the first aspect, wherein the atomized powder of the raw material is formed and A method for producing fine particles, characterized in that the fine particles are supplied into a heat source.
  • the metal or alloy as a raw material is supplied as an atomized powder into a heat source and is converted into fine particles.
  • a fourth aspect of the present invention is the method for producing fine particles according to any one of the thirteenth to thirteenth aspects, wherein the gas-liquid separation is performed using a cyclone.
  • gas-liquid separation is performed by the cyclone, and fine particles are collected as a slurry of the liquid fluid.
  • a fifth aspect of the present invention is the method for producing fine particles according to any one of the first to fourteenth aspects, wherein the heat source is acetylene flame or DC plasma flame.
  • the raw material is made into fine particles by acetylene flame or DC plasma flame.
  • a sixth aspect of the present invention is the method for producing fine particles according to any one of the fifteenth to fifteenth aspects, wherein the liquid fluid is water.
  • the product is captured by water and recovered as a slurry.
  • the raw material is at least one selected from the group consisting of metals, alloys, oxides, nitrides, and oxynitrides.
  • the feature lies in the method for producing fine particles.
  • the raw materials such as metals, alloys, oxides, nitrides, and oxynitrides are fine particles.
  • the heat source is any of an oxidizing atmosphere or a nitriding atmosphere, and the heat source is an oxide, a nitride, or an oxynitride.
  • the raw material is converted into fine particles of an oxide, a nitride, or an oxynitride in a heat source under an oxidizing atmosphere or a nitriding atmosphere.
  • a ninth aspect of the present invention is the method according to any one of the first to seventeenth aspects, wherein the raw material is an In-Sn alloy or an ITO powder, and the indium tin oxide powder is produced.
  • the method is characterized by a method for producing fine particles.
  • the In-Sn alloy or the ITO powder is prepared as a slurry of the ITO powder. Built.
  • a tenth aspect of the present invention is the ninth aspect, wherein the tin content is 2.3-4 in terms of SnO.
  • a method for producing fine particles characterized by producing indium oxide-tin oxide powder of 5% by mass.
  • the conductivity of ITO is maintained by a predetermined amount of oxidized tin.
  • An eleventh aspect of the present invention is the method for producing fine particles according to any one of the eleventh to eleventh aspects, wherein a maximum velocity force of capturing the product with the liquid fluid is 150 mZsec or less. In the way.
  • fine particles can be produced at a relatively low flow rate.
  • a twelfth aspect of the present invention provides an inlet for introducing a product obtained by supplying a raw material into a heat source as a liquid stream, droplets or powder together with a gaseous fluid, A liquid ejecting means for ejecting a mist-like liquid fluid, a gas-liquid separating means for gas-liquid separating fine particles captured by the liquid fluid to obtain a slurry of the fine particles, and an atmosphere containing fine particles which cannot be captured by the liquid fluid. And a circulating means for circulating a part of the fluid back to the fluid droplet ejecting position.
  • the product obtained by supplying the raw material into the heat source is captured as fine particles by the mist-like liquid fluid and separated into gas and liquid, and at least a part of the atmosphere fluid is circulated. It is efficiently recovered by being circulated by means and separated into gas and liquid again.
  • a part of the atmospheric fluid containing vibrated fine particles that cannot be captured by the liquid fluid is further introduced downstream of the gas-liquid separation means.
  • An apparatus for producing fine particles further comprising a second gas-liquid separating means for injecting a mist-like liquid fluid and performing gas-liquid separation to obtain a slurry of the fine particles.
  • the second gas-liquid separation means efficiently collects unrecoverable energetic fine particles.
  • a part of the atmospheric fluid containing vibrated fine particles that cannot be captured by the liquid fluid is further provided downstream of the gas-liquid separation means. 2.
  • a vibrating atmosphere gas that cannot be recovered as a slurry by the second gas-liquid separation means is subjected to gas-liquid separation again, and fine particles are efficiently recovered.
  • a fifteenth aspect of the present invention is the apparatus for producing fine particles according to any one of the twelfth to fourteenth aspects, wherein the gas-liquid separation means is a cyclone.
  • gas-liquid separation can be performed continuously and efficiently by the cyclone.
  • the maximum velocity at which fine particles are captured by the liquid fluid ejected by the fluid ejecting means is 150 mZsec or less.
  • the present invention resides in an apparatus for producing fine particles.
  • fine particles can be produced at a relatively low flow rate.
  • a product obtained by introducing a raw material metal or alloy into a heat source as a liquid stream, droplets, or powder is captured by a mist-like liquid fluid.
  • FIG. 1 is a schematic configuration diagram of an apparatus for producing fine particles according to one embodiment of the present invention.
  • FIG. 2 is a view showing a result of X-ray diffraction of the ITO powder of Example 1 of the present invention.
  • FIG. 3 is a view showing the result of X-ray diffraction of the ITO powder of Example 2 of the present invention.
  • FIG. 4 is a view showing the result of X-ray diffraction of the ITO powder of Comparative Example 1 of the present invention.
  • FIG. 5 is a view showing the result of X-ray diffraction of the ITO powder of Comparative Example 2 of the present invention.
  • FIG. 6 is a view showing the result of X-ray diffraction of the ITO powder of Comparative Example 3 of the present invention.
  • FIG. 7 is a view showing the result of X-ray diffraction of the ITO powder of Example 3 of the present invention.
  • FIG. 8 is a view showing the result of X-ray diffraction of the ITO powder of Comparative Example 4 of the present invention.
  • a raw material is supplied as a liquid stream, droplets or powder into a heat source.
  • the raw material is, for example, a metal or an alloy
  • the metal or the alloy is, for example, a metal such as Mg, Al, Zr, Fe, Si, In, or Sn, or an alloy thereof.
  • raw materials For example, oxides, nitrides, and oxynitrides of the above metals or alloys can be used.
  • the oxide includes a composite oxide
  • the nitride includes a composite nitride.
  • Such a raw material may be supplied as a liquid stream or droplets in a molten state, or may be supplied in a powder state.
  • the molten metal may be dropped continuously as a liquid stream or as droplets, or an atomized powder may be formed and supplied.
  • an ITO powder when used as a raw material, an ITO powder can be obtained. In addition, even if ITO powder is used as a raw material, ITO powders having different properties can be obtained.
  • Examples of the heat source include a heat source capable of performing an oxidizing atmosphere or a nitriding atmosphere, such as an acetylene flame and a DC plasma flame.
  • the temperature of the heat source is not particularly limited as long as the metal, alloy, oxide, nitride, or oxynitride can be melted and sufficiently oxidized or nitrided.
  • acetylene flame it is said that the temperature is several thousands ° C or more, and in the case of DC plasma flame, it is tens of thousands ° C or more.
  • a product is obtained as it is or as an oxide, nitride or oxynitride together with a gas stream.
  • the raw material is obtained as it is as a product of a metal or an alloy, or an oxide, a nitride or an oxynitride of a metal or an alloy is determined by the state of the flame of the heat source, and is set in an oxidizing atmosphere.
  • a product of an oxide or an oxynitride of the metal or alloy is obtained, and when the atmosphere is a nitriding atmosphere, a nitride or an oxynitride of the metal or alloy is obtained. Further, even if an oxidized product, a nitride or an oxynitride is used as a raw material, an oxidized product, a nitride or an oxynitride having a different property can be obtained.
  • the obtained product is captured by a mist-like liquid fluid. That is, a mist-like liquid fluid, preferably mist-like water, is sprayed on the product flowing with the jet of the acetylene flame or the DC plasma flame. As a result, the product is rapidly cooled to fine particles, and becomes a slurry of the sprayed liquid fluid.
  • a mist-like liquid fluid preferably mist-like water
  • the supply of the atomized liquid fluid is not particularly limited as long as the obtained product can be captured and cooled.
  • room temperature water preferably room temperature pure water may be used !, but cooling water may be used!
  • the maximum speed at which the product is captured is, for example, 150 m
  • the liquid fluid containing the fine particles captured by the sprayed liquid fluid is separated into gas and liquid, and the fine particles are collected as a slurry.
  • the method for recovering the slurry is not particularly limited, but preferably can be performed using a cyclone.
  • an In—Sn alloy or an ITO powder can be used as a raw material.
  • ITO Indium oxide oxide tin
  • a high-density sintered body can be easily obtained, and as a result, a long-lived target can be obtained.
  • ITO powder manufactured by various manufacturing methods or ITO powder obtained by pulverizing sintered ITO sintered body is used as the raw material, the properties differ from those of the raw material, and the SnO solid solution in In O
  • ITO powder with a high level of 232.
  • strong ITO powder can be used as a material for an ITO sputtering target.
  • the tin content is 2 in SnO conversion.
  • it is 3 to 45% by mass.
  • a raw material 2 such as a metal or an alloy supplied to a flame 1 composed of acetylene flame or a DC plasma flame, which is a heat source capable of oxidizing atmosphere or nitriding atmosphere, is subjected to a liquid flow, a liquid drop or An inlet 10 for introducing the product 3 obtained by supplying as a powder together with a gaseous fluid, a fluid ejection means 20 for ejecting a mist-like liquid fluid to the introduced fine particles, and fine particles captured by the liquid fluid. And a circulating means for returning a part of the atmospheric fluid containing entrained fine particles that cannot be captured by the liquid fluid to the fluid droplet ejecting position and circulating them. 40.
  • the inlet 10 is not particularly limited as long as the gas flow containing the product can be introduced, but the gas flow may be sucked.
  • the fluid ejecting means 20 is provided downstream of the introduction pipe 11 provided with the introduction port It has a plurality of injection nozzles 21 for injecting water, for example, water, a pump 22 for introducing a fluid to the injection nozzles 21, and a fluid tank 23 filled with fluid.
  • the direction of the jet of the fluid from the jet nozzle 21 is not particularly limited, but it is preferable to jet the fluid in the direction in which it flows in the direction of the flow of the gas flow introduced from the inlet 10.
  • the product 3 contained in the gas stream introduced from the inlet 10 is cooled by the sprayed fluid, for example, water, and is captured as fine particles.
  • a part of the venturi 12 with a narrowed flow path is provided downstream of the injection nozzle 21 of the introduction pipe 11 to prevent a decrease in the flow rate of the gas-liquid mixture, but a part 12 of the bench lily is necessarily provided. No need.
  • the injection nozzle 21 and the pump 22 may be configured to suck and eject the liquid by the suction force of the gas flow which is not necessarily provided.
  • the introduction pipe 11 provided with the introduction port 10 communicates with the introduction port 31 of the cyclone 30, which is a gas-liquid separation unit.
  • the gas-liquid mixture introduced from the inlet 31 of the cyclone 30 is separated into gas and liquid by a vortex 33 circulating along the inner wall of the cyclone main body 32, and the liquid component, that is, the slurry containing the fine particles is separated into the lower part. , And the gaseous component is discharged from the exhaust port 34.
  • a circulation means 40 is provided at the exhaust port 34. That is, a circulation pipe 41 communicating with the introduction pipe 10 near the introduction port 10 is provided at the exhaust port 34, and a blower 42 is interposed in the middle of the circulation pipe 41, and these constitute the circulation means 40. are doing.
  • the circulating means 40 returns the energized powder that could not be captured to the upstream side of the injection nozzle 21 to improve the capturing efficiency.
  • the liquid component gas-liquid separated by the cyclone 30 is discharged from the water outlet 36 and filled in the fluid tank 23. Since the supernatant water of the slurry filled in the fluid tank 23 is circulated by the circulating means 40, a slurry having a fine particle component concentration is gradually obtained.
  • the second exhaust port 35 is provided with a second cyclo 5050 is connected via an exhaust pipe 43.
  • the second cyclone 50 has basically the same structure as the cyclone 30 and has a gas-liquid separation action. That is, the gas-liquid mixture introduced from the inlet 51 to which the exhaust pipe 43 is connected is separated into gas and liquid as a vortex 53 circulating along the inner wall of the cyclone body 52, and contains a liquid component, that is, fine particles. The slurry falls to the lower part, is discharged from the water discharge port 54, and accumulates in the fluid tank 61.
  • a bench lily part 44 having a narrow flow path is provided in the middle of the exhaust pipe 43, and a water circulation pipe 62 communicating the part of the bench lily 44 and the fluid tank 61 is provided.
  • a water circulation pipe 62 communicating the part of the bench lily 44 and the fluid tank 61 is provided.
  • an exhaust pipe 71 is connected to the exhaust port 55, and a second blower 72 is provided in the exhaust pipe 71, so that gas is exhausted from the exhaust port 55 through the second blower 72.
  • the water in the water tank 61 may be sprayed into the exhaust pipe 43 by using a pump and a spray nozzle as in the cyclone 30 described above. Further, the fluid tank 61 may be provided with a filter as described above, or may be provided with a sedimentation separation tank for neutralizing and separating fine particles. Furthermore, the trapping efficiency may be further increased by circulating a part of the exhaust gas from the exhaust port 55 to the exhaust pipe 43 upstream of the bench lily part 44.
  • the second cyclone 50 is not necessarily provided, or when it is desired to further increase the capture efficiency, a plurality of cyclones are further provided. You may connect.
  • the powder was collected by a dry method using a filter to obtain the ITO powder of Example 1.
  • Example 1 ITO powder dry-synthesized from acetylene flame in the same manner as in Example 1 was wet-recovered with spray water and used as the ITO powder of Example 2. (Comparative Example 1)
  • the ITO powder wet-synthesized by the coprecipitation method was used as the ITO powder of Comparative Example 2.
  • aqueous ammonia (special reagent grade) was mixed with the mixed acid to neutralize the mixture to pH 6.5, whereby a white precipitate was deposited.
  • 25% aqueous ammonia special reagent grade
  • ICP spectroscopy inductively coupled high frequency plasma spectroscopy
  • the volume ratio was calculated.
  • the amount of SnO deposited (% by mass) is calculated from the integrated diffraction intensity ratio of X-ray diffraction.
  • the amount of SnO that was not output was defined as the amount of SnO dissolved in InO.
  • the solid solution amount of SnO was 2.35 wt% and 2.42 wt%.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

L'invention concerne un procédé permettant de produire des microparticules telles que celles des oxydes au moyen d'un appareil simple et peu onéreux approprié pour la production de poudre d'ITO; elle concerne également un appareil destiné à cet effet. Elle concerne en outre un procédé de production de microparticules qui consiste à alimenter une source thermique d'une matière première sous la forme d'un flux liquide, de gouttelettes liquides ou de poudre; à piéger tout produit sous la forme de microparticules au moyen d'un fluide liquide sous forme nébuleuse; et à récupérer les microparticules sous la forme de suspension épaisse par la biais de la séparation gaz-liquide.
PCT/JP2004/019354 2003-12-25 2004-12-24 Procede de production de microparticules et appareil associe WO2005066069A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
JP2005516840A JP4864459B2 (ja) 2003-12-25 2004-12-24 微粒子の製造方法
US10/584,069 US20070163385A1 (en) 2003-12-25 2004-12-24 Process for producing microparticles and apparatus therefor
KR1020067013332A KR100907735B1 (ko) 2003-12-25 2004-12-24 미립자의 제조 방법 및 제조 장치

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2003-431586 2003-12-25
JP2003431586 2003-12-25

Publications (1)

Publication Number Publication Date
WO2005066069A1 true WO2005066069A1 (fr) 2005-07-21

Family

ID=34746853

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2004/019354 WO2005066069A1 (fr) 2003-12-25 2004-12-24 Procede de production de microparticules et appareil associe

Country Status (6)

Country Link
US (1) US20070163385A1 (fr)
JP (1) JP4864459B2 (fr)
KR (1) KR100907735B1 (fr)
CN (1) CN100522800C (fr)
TW (1) TW200536776A (fr)
WO (1) WO2005066069A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009095685A (ja) * 2007-10-12 2009-05-07 Tokyo Electron Ltd 粉体製造装置および方法
JP2015515361A (ja) * 2012-02-28 2015-05-28 ユニバーシティ オブ レスターＵｎｉｖｅｒｓｉｔｙ Ｏｆ Ｌｅｉｃｅｓｔｅｒ 気相法と湿式化学法との組合せによる化学反応
JPWO2018030106A1 (ja) * 2016-08-10 2019-01-24 国立大学法人 熊本大学 ナノ粒子集合体、及びナノ粒子集合体の製造方法

Families Citing this family (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050195966A1 (en) * 2004-03-03 2005-09-08 Sigma Dynamics, Inc. Method and apparatus for optimizing the results produced by a prediction model
EP2153157A4 (fr) 2007-05-11 2014-02-26 Sdcmaterials Inc Système de refroidissement par eau et système de transfert de chaleur
US8507401B1 (en) 2007-10-15 2013-08-13 SDCmaterials, Inc. Method and system for forming plug and play metal catalysts
US8652992B2 (en) 2009-12-15 2014-02-18 SDCmaterials, Inc. Pinning and affixing nano-active material
US9126191B2 (en) 2009-12-15 2015-09-08 SDCmaterials, Inc. Advanced catalysts for automotive applications
US8545652B1 (en) 2009-12-15 2013-10-01 SDCmaterials, Inc. Impact resistant material
US8470112B1 (en) 2009-12-15 2013-06-25 SDCmaterials, Inc. Workflow for novel composite materials
US9149797B2 (en) 2009-12-15 2015-10-06 SDCmaterials, Inc. Catalyst production method and system
US8803025B2 (en) * 2009-12-15 2014-08-12 SDCmaterials, Inc. Non-plugging D.C. plasma gun
US9090475B1 (en) 2009-12-15 2015-07-28 SDCmaterials, Inc. In situ oxide removal, dispersal and drying for silicon SiO2
US8557727B2 (en) 2009-12-15 2013-10-15 SDCmaterials, Inc. Method of forming a catalyst with inhibited mobility of nano-active material
US8669202B2 (en) 2011-02-23 2014-03-11 SDCmaterials, Inc. Wet chemical and plasma methods of forming stable PtPd catalysts
CN103945919A (zh) 2011-08-19 2014-07-23 Sdc材料公司 用于催化和催化转化器中的涂覆基质和将基质用修补基面涂料组合物涂覆的方法
US9511352B2 (en) 2012-11-21 2016-12-06 SDCmaterials, Inc. Three-way catalytic converter using nanoparticles
US9156025B2 (en) 2012-11-21 2015-10-13 SDCmaterials, Inc. Three-way catalytic converter using nanoparticles
JP6248318B2 (ja) * 2013-02-14 2017-12-20 セイコーエプソン株式会社 印刷装置
EP3024571B1 (fr) 2013-07-25 2020-05-27 Umicore AG & Co. KG Revêtements catalytiques et substrats revêtus pour convertisseurs catalytiques
JP2016535664A (ja) 2013-10-22 2016-11-17 エスディーシーマテリアルズ， インコーポレイテッド リーンＮＯｘトラップの組成物
CN106061600A (zh) 2013-10-22 2016-10-26 Sdc材料公司 用于重型柴油机的催化剂设计
WO2015143225A1 (fr) 2014-03-21 2015-09-24 SDCmaterials, Inc. Compositions pour systèmes d'adsorption de nox passive (pna) et leurs procédés de fabrication et d'utilisation
KR101902123B1 (ko) * 2017-07-21 2018-09-27 김태석 산화물 분말 제조장치 및 그 제조방법
NO345196B1 (en) * 2018-10-25 2020-11-02 N2 Applied As Low pressure plasma reactor loop process and system
CN109502553B (zh) * 2019-01-19 2023-08-22 广西晶联光电材料有限责任公司 一种制备金属氧化物粉体的装置和方法
CN112774611B (zh) * 2021-01-18 2024-01-30 广西大学 一种超重力微界面传质强化反应-结晶干燥耦合一体机

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5131754A (ja) * 1974-09-13 1976-03-18 Kansai Paint Co Ltd Kyujogoseijushifunmatsu no seizoho
JPH0699057A (ja) * 1992-06-12 1994-04-12 Stork Protecon Bv 粒状物質と液体の接触装置

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5131751A (ja) 1974-09-12 1976-03-18 Mitsubishi Monsanto Chem Shinkuseikeiyonanshitsuhorienkabiniruenbosushiito no seizoho
US4787935A (en) * 1987-04-24 1988-11-29 United States Of America As Represented By The Secretary Of The Air Force Method for making centrifugally cooled powders
JP2788919B2 (ja) * 1988-02-10 1998-08-20 ノルスク・ヒドロ・アーエスアー 金属粉の製造方法及び装置
JPH03247709A (ja) * 1990-02-23 1991-11-05 Kawasaki Steel Corp 金属粉末製造装置
JP3305357B2 (ja) * 1992-05-21 2002-07-22 東芝機械株式会社 耐食・耐摩耗性に優れた合金およびその製造方法ならびにその合金製造用材料
US5935461A (en) * 1996-07-25 1999-08-10 Utron Inc. Pulsed high energy synthesis of fine metal powders
JP4488651B2 (ja) * 2001-05-23 2010-06-23 高周波熱錬株式会社 熱プラズマによるセラミック又は金属の球状粉末の製造方法および装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5131754A (ja) * 1974-09-13 1976-03-18 Kansai Paint Co Ltd Kyujogoseijushifunmatsu no seizoho
JPH0699057A (ja) * 1992-06-12 1994-04-12 Stork Protecon Bv 粒状物質と液体の接触装置

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2009095685A (ja) * 2007-10-12 2009-05-07 Tokyo Electron Ltd 粉体製造装置および方法
JP2015515361A (ja) * 2012-02-28 2015-05-28 ユニバーシティ オブ レスターＵｎｉｖｅｒｓｉｔｙ Ｏｆ Ｌｅｉｃｅｓｔｅｒ 気相法と湿式化学法との組合せによる化学反応
US9931607B2 (en) 2012-02-28 2018-04-03 Gediminas Gallinis Chemical reaction by combination of gas-phase and wet-chemical methods
JPWO2018030106A1 (ja) * 2016-08-10 2019-01-24 国立大学法人 熊本大学 ナノ粒子集合体、及びナノ粒子集合体の製造方法

Also Published As

Publication number Publication date
US20070163385A1 (en) 2007-07-19
TW200536776A (en) 2005-11-16
JPWO2005066069A1 (ja) 2007-07-26
JP4864459B2 (ja) 2012-02-01
KR20060109505A (ko) 2006-10-20
KR100907735B1 (ko) 2009-07-14
CN100522800C (zh) 2009-08-05
CN1906125A (zh) 2007-01-31

Similar Documents

Publication Publication Date Title
WO2005066069A1 (fr) Procede de production de microparticules et appareil associe
US7611649B2 (en) Nanopowders synthesis apparatus and method
CA2579539C (fr) Procede et appareil de fabrication de fines particules
CN103785860B (zh) 3d打印机用的金属粉末及其制备方法
US20040065170A1 (en) Method for producing nano-structured materials
CN111819018B (zh) 微粒子的制造方法及微粒子
JP4296269B2 (ja) 高輝度発光材料の製造方法及びそれに用いる製造装置
JP2009513476A (ja) 二酸化チタンの製造方法
KR100844446B1 (ko) 산화인듐-산화주석 분말 및 그것을 사용한 스퍼터링 타겟및 산화인듐-산화주석 분말의 제조방법
US20030102207A1 (en) Method for producing nano powder
US5278384A (en) Apparatus and process for the treatment of powder particles for modifying the surface properties of the individual particles
TW202128315A (zh) 微粒子之製造裝置及微粒子之製造方法
JP4721901B2 (ja) 酸化インジウム−酸化錫粉末及びそれを用いたスパッタリングターゲット
US7097691B2 (en) Method for producing pigment nano-particles
CN1380255A (zh) 氨络合液喷雾热解制备碱式碳酸盐纳米粒子的方法与设备
CN107998995B (zh) 一种气液混合高压雾化制备化合物粉末材料的装置及方法
RU2434716C2 (ru) Способ получения нанопорошков нитрида титана
KR100529054B1 (ko) 고온 다습한 캐리어 가스에 의하여 운반되는미세분체로부터 수분을 제거하는 장치 및 방법
WO2001040402A1 (fr) Procede de production de phosphore
US7611650B2 (en) Nanopowders synthesis apparatus
CN114728333A (zh) 微粒子
CN1295152C (zh) 制备纳米氧化铝粉的电弧喷涂反应合成设备及方法
KR100734608B1 (ko) 고온 다습한 캐리어 가스에 의해 이송되는 분체의 제조장치
CN1275863C (zh) 球形Zr(OH) 4微颗粒的真空反应负压输送连续化制备装置
CN1465461A (zh) 一种表面经良好保护的纳米金属粉的制备方法

Legal Events

Date Code Title Description
WWE Wipo information: entry into national phase

Ref document number: 2005516840

Country of ref document: JP

AK Designated states

Kind code of ref document: A1

Designated state(s): AE AG AL AM AT AU AZ BA BB BG BR BW BY BZ CA CH CN CO CR CU CZ DE DK DM DZ EC EE EG ES FI GB GD GE GH GM HR HU ID IL IN IS JP KE KG KP KR KZ LC LK LR LS LT LU LV MA MD MG MK MN MW MX MZ NA NI NO NZ OM PG PH PL PT RO RU SC SD SE SG SK SL SY TJ TM TN TR TT TZ UA UG US UZ VC VN YU ZA ZM ZW

AL Designated countries for regional patents

Kind code of ref document: A1

Designated state(s): GM KE LS MW MZ NA SD SL SZ TZ UG ZM ZW AM AZ BY KG KZ MD RU TJ TM AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LT LU MC NL PL PT RO SE SI SK TR BF BJ CF CG CI CM GA GN GQ GW ML MR NE SN TD TG

121 Ep: the epo has been informed by wipo that ep was designated in this application
WWE Wipo information: entry into national phase

Ref document number: 2007163385

Country of ref document: US

Ref document number: 10584069

Country of ref document: US

NENP Non-entry into the national phase

Ref country code: DE

WWW Wipo information: withdrawn in national office

Country of ref document: DE

WWE Wipo information: entry into national phase

Ref document number: 1020067013332

Country of ref document: KR

WWE Wipo information: entry into national phase

Ref document number: 200480041059.X

Country of ref document: CN

WWP Wipo information: published in national office

Ref document number: 1020067013332

Country of ref document: KR

122 Ep: pct application non-entry in european phase
WWP Wipo information: published in national office

Ref document number: 10584069

Country of ref document: US