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US20070163385A1 - Process for producing microparticles and apparatus therefor - Google Patents

Process for producing microparticles and apparatus therefor Download PDF

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US20070163385A1
US20070163385A1 US10/584,069 US58406904A US2007163385A1 US 20070163385 A1 US20070163385 A1 US 20070163385A1 US 58406904 A US58406904 A US 58406904A US 2007163385 A1 US2007163385 A1 US 2007163385A1
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microparticles
liquid
gas
fluid
powder
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Seiichiro Takahashi
Hiroshi Watanabe
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Mitsui Kinzoku Co Ltd
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Assigned to MITSUI MINING & SMELTING CO., LTD. reassignment MITSUI MINING & SMELTING CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: TAKAHASHI, SEIICHIRO, WATANABE, HIROSHI
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    • 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
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    • 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
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    • 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 process for producing microparticles of a material such as indium oxide-tin oxide powder, and to an apparatus for producing the microparticles.
  • Sputtering is a generally known technique for forming thin film.
  • a thin film is formed by sputtering a sputtering target.
  • the sputtering technique is employed in industrial processes, since a thin film of large surface area can be readily formed, and a high-performance film can be formed at high efficiency.
  • various sputtering techniques have been known, such as reactive sputtering; i.e., sputtering in a reactive gas, and magnetron sputtering, which realizes high-speed thin film formation by placing a magnet on the backside of a target.
  • ITO film is a transparent conductive film which has high optical transparency with respect to visible light and high conductivity and which, therefore, finds a wide variety of uses such as for a liquid crystal display, a heat-generating film for defogging a glass panel, and an IR-reflecting film.
  • the aforementioned sputtering target for forming an ITO film is produced through mixing indium oxide powder and tin oxide powder at a predetermined ratio, molding under dry or wet conditions, and sintering the molded product (Patent Document 1).
  • Patent Document 1 highly-dispersible indium oxide powder has been proposed for producing high-density sintered ITO (see, for example, Patent Documents 2, 3, and 4).
  • Another known method includes sintering an ITO powder synthesized through the co-precipitation method under wet conditions (see, for example Patent Document 5).
  • sintering an ITO powder synthesized through the co-precipitation method under wet conditions see, for example Patent Document 5
  • wet-synthesis methods for producing ITO powder have been proposed for producing high-density sintered ITO (see, for example, Patent Documents 6 to 9).
  • an object of the present invention is to provide a process for producing microparticles, which process enables production of microparticles such as oxide microparticles by means of a simple apparatus at low cost and which is suitable for producing ITO powder.
  • Another object of the invention is to provide an apparatus for producing the microparticles.
  • a process for producing microparticles characterized in that the process comprises feeding into a heat source a raw material in the form of a liquid stream, liquid droplets, or powder; capturing the formed product in the form of microparticles by means of a fluid of atomized liquid (hereinafter referred to as atomized liquid fluid); and collecting the microparticles in the form of slurry through gas-liquid separation.
  • a fluid of atomized liquid hereinafter referred to as atomized liquid fluid
  • the product obtained through feeding the raw material into the heat source is effectively captured in the form of microparticles by means of the atomized liquid fluid, and the microparticles are effectively collected in the form of slurry through gas-liquid separation.
  • a second mode of the present invention is drawn to a specific embodiment of the process of the first mode, wherein the raw material to be fed into the heat source is provided through forming a molten material into a liquid stream or liquid droplets.
  • the raw material in the form of a liquid stream or liquid droplets formed from a molten material such as a metal or an alloy may be converted to an oxide thereof in the heat source, and the oxide can be captured in the form of microparticles by means of the atomized liquid fluid.
  • a third mode of the present invention is drawn to a specific embodiment of the process of the first mode, wherein the raw material to be fed into the heat source is in the form of atomized powder.
  • the raw material in the form of atomized powder formed from a raw material such as a metal or an alloy is fed into the heat source, whereby the microparticles thereof are formed.
  • a fourth mode of the present invention is drawn to a specific embodiment of the process of any of the first to third modes, wherein the gas-liquid separation is performed by means of a cyclone separator.
  • the microparticles are effectively collected with the liquid fluid in the form of slurry through gas-liquid separation performed by means of a cyclone separator.
  • a fifth mode of the present invention is drawn to a specific embodiment of the process of any of the first to fourth modes, wherein the heat source is acetylene flame or DC plasma flame.
  • the raw material is formed into microparticles thereof by acetylene flame or DC plasma flame.
  • a sixth mode of the present invention is drawn to a specific embodiment of the process of any of the first to fifth modes, wherein the liquid fluid is water.
  • the product is captured by water, and the product-water slurry is collected.
  • a seventh mode of the present invention is drawn to a specific embodiment of the process of any of the first to sixth modes, wherein the raw material is at least one member selected from among metals, alloys, oxides, nitrides, and oxide nitrides.
  • the raw material such as metal, alloy, oxide, nitride, or oxide nitride is formed into microparticles thereof.
  • An eighth mode of the present invention is drawn to a specific embodiment of the process of any of the first to seventh modes, wherein the heat source is an oxidizing atmosphere or a nitrifying atmosphere, whereby oxide microparticles, nitride microparticles, or oxide nitride microparticles are produced.
  • the heat source is an oxidizing atmosphere or a nitrifying atmosphere, whereby oxide microparticles, nitride microparticles, or oxide nitride microparticles are produced.
  • the raw material is converted to oxide microparticles, nitride microparticles, or oxide nitride microparticles in an oxidizing atmosphere or a nitrifying atmosphere serving as a heat source.
  • a ninth mode of the present invention is drawn to a specific embodiment of the process of any of the first to seventh modes, wherein the raw material is an In—Sn alloy or ITO powder, from which indium oxide-tin oxide powder is produced.
  • a slurry of ITO powder is produced from an In—Sn alloy or ITO powder.
  • a tenth mode of the present invention is drawn to a specific embodiment of the process of the ninth mode, which process produces indium oxide-tin oxide powder having a tin content of 2.3 to 45 mass % as calculated on the basis of SnO 2 .
  • the produced ITO maintains conductivity by virtue of a predetermined amount of tin oxide.
  • An eleventh mode of the present invention is drawn to a specific embodiment of the process of any of the first to tenth modes, wherein the product flows at a maximum speed of 150 m/sec or less, when the product is captured by means of the liquid fluid.
  • microparticles can be produced at a relatively slow flow speed of the product.
  • an apparatus for producing microparticles characterized in that the apparatus comprises an inlet for introducing, into the inside of the apparatus, a gas fluid and a product obtained through feeding a raw material in the form of a liquid flow, liquid droplets, or powder into a heat source;
  • a fluid jetting means for jetting an atomized liquid fluid to the introduced product
  • a first gas-liquid separation means for subjecting, to gas-liquid separation, microparticles captured by the liquid fluid, to thereby form a slurry of the microparticles
  • a first circulating means for returning a part of an atmosphere fluid containing microparticles that have not been captured by the liquid fluid to a position where the fluid jetting means is disposed.
  • the product obtained through feeding a raw material into a heat source is captured in the form of microparticles by means of an atomized liquid fluid, followed by gas-liquid separation, and at least a part of the atmosphere fluid is circulated through the circulating means, followed by another gas-liquid separation.
  • the microparticles can be effectively collected.
  • a thirteenth mode of the present invention is drawn to a specific embodiment of the apparatus of the twelfth mode, which apparatus further comprises, on the downstream side of the first gas-liquid separation means, a second gas-liquid separation means, the second gas-liquid separation means being provided for introducing a part of an atmosphere fluid containing microparticles that have not been captured by the liquid fluid, for jetting an atomized liquid fluid to the atmosphere fluid, and for performing gas-liquid separation, to thereby obtain a slurry of the microparticles.
  • the microparticles that have not been collected can be effectively collected through the second gas-liquid separation means.
  • a fourteenth mode of the present invention is drawn to a specific embodiment of the apparatus of the thirteenth mode, which apparatus further comprises, on the downstream side of the second gas-liquid separation means, a second circulating means for returning a part of an atmosphere fluid containing microparticles that have not been captured by the liquid fluid to the inlet of the second gas-liquid separation means.
  • the atmosphere gas which has not provided a slurry through the second gas-liquid separation means is further subjected to gas-liquid separation, whereby microparticles are effectively collected.
  • a fifteenth mode of the present invention is drawn to a specific embodiment of the apparatus of any of the twelfth to fourteenth modes, wherein the first or second gas-liquid separation is a cyclone separator.
  • gas-liquid separation can be performed continuously and effectively by means of a cyclone separator.
  • a sixteenth mode of the present invention is drawn to a specific embodiment of the apparatus of any of the twelfth to fifteenth modes, wherein the particles flow at a maximum speed of 150 m/sec or less, when the microparticles are captured by the liquid fluid jetted by means of the fluid jetting means.
  • microparticles can be produced at a relatively slow flow speed.
  • a raw material metal or alloy in the form of a liquid stream, liquid droplets, or powder is fed into a heat source, and the formed product in the form of microparticles is captured by means of an atomized liquid fluid.
  • microparticles can be effectively produced in a simple manner.
  • FIG. 1 Schematic configuration of an embodiment of the apparatus of the present invention for producing microparticles.
  • FIG. 2 An X-ray diffraction chart of ITO powder produced in Example 1 of the present invention.
  • FIG. 3 An X-ray diffraction chart of ITO powder produced in Example 2 of the present invention.
  • FIG. 4 An X-ray diffraction chart of ITO powder produced in Comparative Example 1 of the present invention.
  • FIG. 5 An X-ray diffraction chart of ITO powder produced in Comparative Example 2 of the present invention.
  • FIG. 6 An X-ray diffraction chart of ITO powder produced in Comparative Example 3 of the present invention.
  • FIG. 7 An X-ray diffraction chart of ITO powder produced in Example 3 of the present invention.
  • FIG. 8 An X-ray diffraction chart of ITO powder produced in Comparative Example 4 of the present invention.
  • a raw material in the form of a liquid stream, liquid droplets, or powder is fed into a heat source.
  • the raw material is, for example, metal or alloy, and specific examples include metals such as Mg, Al, Zr, Fe, Si, In, and Sn, and alloys thereof.
  • the raw material may be any of the aforementioned oxides, nitrides, and oxide nitrides of the metal or alloy.
  • the “oxides” include compound oxides, and the “nitrides” include complex nitrides.
  • the raw material to be fed may be melted to form a liquid stream or liquid droplets, or may be powder.
  • a molten metal may be continuously poured from a tank in the form of a liquid stream or liquid droplets.
  • the raw material to be fed may be formed into atomized powder.
  • an ITO powder can be produced. Furthermore, when an ITO powder is employed as a raw material, a different type of ITO material can be produced.
  • the heat source may be an oxidizing atmosphere or a nitrifying atmosphere, and specific examples include acetylene flame and DC plasma flame.
  • acetylene flame and DC plasma flame No particular limitation is imposed on the temperature of the heat source, so long as the heat source can melt metal, alloy, oxide, nitride, or oxide nitride and can sufficiently oxidize or nitrify the raw material.
  • the temperature is at least some thousands of degrees Celsius in the case of acetylene flame, and at least some ten-thousands of degrees Celsius in the case of DC plasma flame.
  • a gas flow of a raw material itself, of the corresponding oxide, of the corresponding nitride, or of the corresponding oxide nitride is yielded as a product.
  • the product may be a raw material itself (i.e., metal or alloy) or the corresponding oxide, nitride, or oxide nitride, depending on the flame conditions.
  • the formed product is captured by means of an atomized liquid fluid.
  • an atomized liquid fluid preferably atomized water
  • atomized liquid fluid is jetted to the product carried by a jet generated from the acetylene flame or DC plasma flame.
  • the product is quenched to form microparticles, and a slurry containing the microparticles in the jetted liquid is produced.
  • the product flows at a maximum speed of, for example, 150 m/sec or less, preferably about 100 m/sec or less, when the product is captured in the form of microparticles.
  • the liquid fluid containing the microparticles captured by means of the jetted liquid fluid is subjected to gas-liquid separation, whereby the microparticles are collected in the form of slurry.
  • gas-liquid separation No particular limitation is imposed on the method of collecting the slurry, and a cyclone separator is preferably employed.
  • an indium oxide-tin oxide (ITO) powder when employed as a raw material, an indium oxide-tin oxide (ITO) powder can be produced.
  • the thus-produced ITO powder contains a large amount of a SnO 2 solid solution component dissolved in In 2 O 3 . Therefore, the ITO exhibits high sinterability and readily provides high-density sintered ITO. As a result, a long-life sputtering target can be produced.
  • the above ITO powder may be employed as a material for an ITO sputtering target.
  • the ITO sputtering target material preferably has a tin content, as calculated on the basis of SnO 2 , of 2.3 to 45 mass %.
  • FIG. 1 An embodiment of the apparatus for producing microparticles of the present invention will next be described with reference to FIG. 1 .
  • the apparatus has an inlet 10 for introducing, into the inside of the apparatus, a gas fluid and a product 3 obtained through feeding of a raw material 2 (e.g., metal or alloy) in the form of a liquid flow, liquid droplets, or powder into a flame 1 (acetylene flame or DC plasma flame) serving as a heat source that can provide an oxidizing atmosphere or a nitrifying atmosphere; fluid jetting means 20 for jetting an atomized liquid fluid to the introduced microparticles; a cyclone separator 30 serving as gas-liquid separation means for subjecting, to gas-liquid separation, the microparticles captured by the liquid fluid, to thereby form a slurry of the microparticles; and circulating means 40 for returning a part of an atmosphere fluid containing microparticles that have not been captured by the liquid fluid to a position where the fluid jetting means is disposed.
  • a raw material 2 e.g., metal or alloy
  • acetylene flame or DC plasma flame acetylene flame or DC
  • the inlet 10 may be gas-suction means.
  • the fluid jetting means 20 is provided in a conduit 11 on the downstream side of the inlet 10 .
  • the fluid jetting means 20 includes, for example, a plurality of jet nozzles 21 for jetting water, a pump 22 for feeding fluid to the jet nozzles 21 , and a fluid tank 23 for storing fluid.
  • No particular limitation is imposed on the jetting direction of the fluid jetted through the jet nozzles 21 .
  • the jetting direction is preferably such that the jetted fluid is merged with a gas flow introduced through the inlet 10 .
  • the product 3 contained in the gas fluid introduced through the inlet 10 is cooled by means of the atomized liquid fluid (e.g., water) to form microparticles, and the microparticles are captured.
  • the atomized liquid fluid e.g., water
  • a venturi section 12 where the flow path is narrowed, is provided on the downstream side of the jet nozzles 21 , so as to prevent reduction in flow rate of a gas-liquid mixture. Provision of the venturi section 12 is not obligatory.
  • the jet nozzles 21 and the pump 22 are not necessarily provided, and instead, the liquid may be jetted on the basis of suction power generated by flow of gas.
  • the conduit 11 provided with the inlet 10 is in communication with an inlet 31 of the cyclone separator 30 serving as gas-liquid separation means.
  • a gas-liquid mixture which has been introduced through the inlet 31 into the cyclone separator 30 forms a vortex 33 proceeding around the inner wall of a cyclone body 32 , whereby a liquid component is separated from the gas.
  • the liquid component i.e., a slurry containing the microparticles, falls down in the cyclone separator 30 , and a gas component is discharged through a gas-discharge outlet 34 .
  • the circulating means 40 is provided so as to communicate with the gas-discharge outlet 34 .
  • circulation piping 41 is connected to the outlet 34 , the circulation piping 41 being in communication with a position near the inlet 10 of the conduit 11 .
  • a blower 42 intervenes in the circulation piping 41 .
  • the circulation means 40 consists of the members 41 and 42 . Through the circulation means 40 , the powder which has not been captured is returned to the upstream side of the jet nozzles 21 , thereby enhancing capturing efficiency.
  • the liquid component which has been separated from the gas by means of the cyclone separator 30 is discharged through a water-discharge outlet 36 and stored in the fluid tank 23 .
  • the supernatant water of the slurry stored in the tank 23 is circulated by means of the circulation means 40 , whereby the concentration of the slurry containing the microparticles gradually increases.
  • Most of the discharged gas produced by means of the cyclone separator 30 is circulated through the gas-discharge outlet 34 to the circulation piping 41 .
  • a second cyclone separator 50 serving as second gas-liquid separation means is connected to the second gas-discharge outlet 35 via discharge piping 43 .
  • the second cyclone separator 50 has virtually the same structure as the cyclone separator 30 and serves as gas-liquid separation means. Specifically, a gas-liquid mixture which has been introduced through an inlet 51 connected to the discharge piping 43 into the second cyclone separator 50 forms a vortex 53 proceeding around the inner wall of a cyclone body 52 , whereby a liquid component is separated from the gas.
  • the liquid component i.e., a slurry containing the microparticles
  • falls down in the cyclone separator 50 and is discharged through a water-discharge outlet 54 and stored in a fluid tank 61 .
  • a venturi section 44 where the flow path is narrowed, intervenes in the discharge piping 43 , and water circulating piping 62 is provided so as to maintain communication between the venturi section 44 and the fluid tank 61 .
  • water contained in the fluid tank 61 is drawn and jetted into the venturi section 44 , whereby microparticles remaining in the gas phase are captured by water (liquid).
  • Gas-discharge piping 71 is connected to a gas-discharge outlet 55 , and a second blower 72 is provided in the gas-discharge piping 71 , such that the gas is discharged through the gas-discharge outlet 55 by the mediation of the second blower 72 .
  • Water contained in the water tank 61 may be jetted into the gas-discharge piping 43 by means of a pump and jet nozzles as mentioned in relation to the cyclone separator 30 .
  • the fluid tank 61 may be provided with a filter and a settling tank for separating microparticles from the liquid through neutralization.
  • a portion of the gas discharged through the gas-discharge outlet 55 may be circulated to the upstream side of the venturi section 44 of the gas-discharge piping 43 , to thereby enhance capturing efficiency.
  • the second cyclone separator 50 is not necessarily provided.
  • a plurality of cyclone separators may be linked together.
  • the powder was collected by means of a bag filter under dry conditions, to thereby yield an ITO powder of Example 1.
  • Example 2 In a manner similar to that of Example 1, an ITO powder was synthesized by means of acetylene flame under dry conditions. The powder was collected by jetting water to the powder under wet conditions, to thereby yield an ITO powder of Example 2.
  • ITO powders of Examples 1 and 2 and Comparative Examples 1 to 3 were analyzed in terms of SnO 2 solid solution content. The determination procedure was as follows. Prior to the test, ITO powders of Examples 1 and 2 and Comparative Examples 2 and 3 were calcined at 1,000° C. for three hours in air so as to grow precipitated SnO 2 microparticles to SnO 2 large particles, which are readily detectable.
  • ICP spectroscopic analysis Inductively coupled high-frequency plasma spectroscopic analysis (ICP spectroscopic analysis) was performed. For calculation, it was assumed that each ITO powder exclusively consists of In, Sn, and oxygen (O), and that a certain amount of oxygen may be deficient. The ratio of In to Sn was calculated from the analytical values, and the ratio by weight of In 2 O 3 to SnO 2 was calculated, under the condition that all elemental In and Sn were converted to In 2 O 3 and SnO 2 , respectively. 2. ITO powders of Examples 1 and 2 and Comparative Examples 1 to 3 were subjected to powder X-ray diffractometry (XRD: by means of MXP 18II, product of Mac Science), whereby the precipitated SnO 2 content of each powder was determined.
  • XRD powder X-ray diffractometry
  • the precipitated SnO2 content (mass %) of the ITO powder was determined from the ratio between integral diffraction intensity attributed to In 2 O 3 (222) and integral diffraction intensity attributed to SnO 2 (110), with respect to Standard Product 1 of Comparative Example 1.
  • the precipitated SnO 2 content (mass %) is a SnO 2 content obtained from an integral intensity of X-ray diffraction attributed to SnO 2 , assuming that the SnO 2 component which has not been dissolved in In 2 O 3 and has been grown through calcination at about 1,000° C. exhibits an X-ray diffraction peak attributed to SnO 2 (110).
  • FIGS. 2 to 6 show the results of X-ray diffraction analysis.
  • the ITO powders of Examples 1 and 2 were found to have a SnO 2 solid solution content of 2.35 wt. % and 2.42 wt. %, which are higher than the SnO 2 solid solution content of 2.26 wt. % of the ITO powder of Comparative Example 2 obtained through wet synthesis.
  • the ITO powder of Comparative Example 3 which had been produced through pulverizing the sintered product thereof, was found to form a compound oxide. Therefore, the SnO 2 solid solution content of the ITO powder of Comparative Example 3 could not be determined.
  • TABLE 1 SnO 2 XRD analysis solid ICP analysis Precipitated solution Sample In Sn In 2 O 3 SnO 2 Compound InO 3 SnO 2 SnO 2 content content No. (wt.
  • the powder was collected by jetting water to the powder under wet conditions, to thereby yield an ITO powder of Example 3.
  • Example 3 Similar to Test Example 1, each of the ITO powders of Example 3 and Comparative Example 4 was analyzed in terms of SnO 2 solid solution content. Powder X-ray diffractometry (XRD) was performed by means of X'PertPRO MPD (product of Spectris Co., Ltd.). The results are shown in Table 2. FIGS. 7 and 8 show the results of X-ray diffraction analysis.
  • the ITO powder of Example 3 was found to have a SnO 2 solid solution content of 3.00 wt. %, which is remarkably higher than the SnO 2 solid solution content of the ITO powder of Example 2 obtained by means of acetylene flame instead of DC plasma flame.
  • SnO 2 XRD analysis solid ICP analysis Precipitated solution Sample In Sn In 2 O 3 SnO 2 Compound InO 3 SnO 2 SnO 2 content content No. (wt. %) (wt. %) (Wt. %) (Wt. %) oxide (222) (110) (wt. %) (wt. %) Ex. 3 73.8 7.46 90.40 9.60 no 691582 31090 6.60 3.00 Comp. 75.1 7.86 90.10 9.90 no 892303 62325 9.90 0.00

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