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CN100522800C - Method and apparatus for producing fine particles - Google Patents

Method and apparatus for producing fine particles Download PDF

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CN100522800C
CN100522800C CNB200480041059XA CN200480041059A CN100522800C CN 100522800 C CN100522800 C CN 100522800C CN B200480041059X A CNB200480041059X A CN B200480041059XA CN 200480041059 A CN200480041059 A CN 200480041059A CN 100522800 C CN100522800 C CN 100522800C
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CN1906125A (en
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高桥诚一郎
渡边弘
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Mitsui Kinzoku Co Ltd
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Mitsui Mining and Smelting Co Ltd
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Abstract

The present invention provides a method for producing fine particles, which is capable of producing fine particles such as oxide fine particles at low cost by a simple apparatus and which is suitable for producing an ITO powder, and a production apparatus. In a method for producing microparticles, a raw material in the form of a liquid stream, droplets, or powder is fed to a heat source, a product is captured in the form of microparticles by a mist-like liquid fluid, and microparticles are collected in the form of a slurry by gas-liquid separation.

Description

微粒的制造方法及制造设备 Microparticle manufacturing method and manufacturing equipment

技术领域 technical field

本发明涉及诸如氧化铟-氧化锡粉体微粒的制造方法和制造设备。The present invention relates to a manufacturing method and manufacturing equipment such as indium oxide-tin oxide powder particles.

背景技术 Background technique

溅射是用于形成薄膜的众所周知的技术。在溅射技术中，通过对溅射靶进行溅射而形成薄膜。溅射技术被用于工业加工，因为可以方便地形成大表面积的薄膜，并且能够以高效率形成高性能的膜。近年来，各种溅射技术已为人所知，例如反应溅射；即在反应性气体中的溅射，和磁控溅射，它通过将磁体置于靶的背面实现了高速率的薄膜形成。Sputtering is a well known technique for forming thin films. In sputtering technology, a thin film is formed by sputtering a sputtering target. Sputtering technology is used in industrial processing because it can easily form thin films with large surface area and can form high-performance films with high efficiency. In recent years, various sputtering techniques have been known, such as reactive sputtering; that is, sputtering in a reactive gas, and magnetron sputtering, which achieves a high rate of film formation by placing a magnet on the back side of a target .

在通过溅射得到的薄膜产品之中，氧化铟-氧化锡(In2O3-SnO2复合氧化物，下文中简称为ITO)薄膜，由于对于可见光具有高的光学透明度并具有高的导电性，因此它作为透明导电膜得到了广泛的应用，例如用于液晶显示，用于玻璃的除雾的生热薄膜，和IR反射薄膜。Among the thin film products obtained by sputtering, indium oxide-tin oxide (In 2 O 3 -SnO 2 composite oxide, hereinafter referred to as ITO) thin film, due to its high optical transparency to visible light and high electrical conductivity , so it has been widely used as a transparent conductive film, such as for liquid crystal display, heat generating film for defogging of glass, and IR reflective film.

因此，为了更高效率和更低成本的生产薄膜，需要对溅射条件和溅射设备进行改进和改善，现在仍在进行当中，而且溅射设备的有效操作是必需的。在通过溅射生产ITO薄膜中，从安装新溅射靶到初始电弧(异常放电)结束的时期，即引发薄膜形成所需要的时期，优选尽可能短，并且评价从靶的安装开始的可溅射时期(累计溅射时间：靶寿命)是一个关键问题。Therefore, in order to produce thin films with higher efficiency and lower cost, improvement and improvement of sputtering conditions and sputtering equipment are required, and are still in progress, and efficient operation of sputtering equipment is required. In the production of ITO thin films by sputtering, the period from the installation of a new sputtering target to the end of the initial arc (abnormal discharge), that is, the period required to initiate film formation, is preferably as short as possible, and the sputterability from the installation of the target is evaluated Sputtering period (cumulative sputtering time: target life) is a key issue.

前述用于形成ITO薄膜的溅射靶是通过如下方法制成：以预定比例混合氧化铟粉和氧化锡粉，在干态或湿态下进行成形，然后烧结成形产物(专利文献1)。在这方面，已提出可高度分散的氧化铟粉以生产高密度ITO烧结体(例如参见专利文献2、3和4)。The aforementioned sputtering target for forming an ITO thin film is made by mixing indium oxide powder and tin oxide powder in a predetermined ratio, forming in a dry or wet state, and then sintering the shaped product (Patent Document 1). In this regard, highly dispersible indium oxide powders have been proposed to produce high-density ITO sintered bodies (see, for example, Patent Documents 2, 3 and 4).

另一种已知方法包括，烧结在湿态下通过共沉淀方法合成的ITO粉体(例如参见专利文献5)。类似地，已提出多种用于生产ITO粉体的湿合成方法用来生产高密度的烧结ITO(例如参见专利文献6-9)。Another known method includes sintering ITO powder synthesized by a co-precipitation method in a wet state (for example, see Patent Document 5). Similarly, various wet synthesis methods for producing ITO powders have been proposed to produce high-density sintered ITO (see, for example, patent documents 6-9).

提出了生产ITO粉体的又一种方法，其中使铟-锡合金在等离子弧中与氧反应，随后通过马赫数≥1的气流以预定或更快的冷却速率冷却反应产物(参见专利文献10)。然而，马赫数≥1的高速气流的使用需要大的设备，这会妨碍ITO粉体的低成本和高效率生产。Yet another method for producing ITO powder has been proposed, in which an indium-tin alloy is reacted with oxygen in a plasma arc, and then the reaction product is cooled at a predetermined or faster cooling rate by a gas flow with a Mach number ≥ 1 (see Patent Document 10 ). However, the use of a high-speed gas flow with a Mach number ≥ 1 requires large equipment, which hinders low-cost and high-efficiency production of ITO powder.

除ITO粉体生产方法以外，提出了生产金属氧化物微粒的下列方法。例如提出了多种方法，包括将金属粉体送入燃烧器火焰，以由此产生氧化物超细微粒，随后进行固-气分离(例如参见专利文献11-16)。还提出了下面的方法，包括将气体喷射于熔融金属，由此形成金属粉体；通过气体输送该粉体；并将该粉体送入进行反应如化学反应或浓缩的液体中，由此形成微粉(参见专利文献17)。此外，提出了形成超微粒的方法，包括向诸如块状金属或金属氧化物棒的源施加等离子弧，由此熔化和蒸发该源，并向蒸发的气体喷射反应/冷却气体(参见专利文献18-20)。In addition to the ITO powder production method, the following methods for producing metal oxide fine particles have been proposed. For example, various methods have been proposed, including feeding metal powder into a burner flame to thereby generate oxide ultrafine particles, followed by solid-gas separation (see, for example, Patent Documents 11-16). Also proposed is a method comprising injecting a gas onto molten metal, thereby forming a metal powder; transporting the powder by the gas; and feeding the powder into a liquid undergoing a reaction such as a chemical reaction or concentration, thereby forming Micropowder (see Patent Document 17). Furthermore, a method of forming ultrafine particles has been proposed, which involves applying a plasma arc to a source such as a bulk metal or metal oxide rod, thereby melting and evaporating the source, and spraying a reaction/cooling gas to the evaporated gas (see Patent Document 18 -20).

然而，上述的干合成方法可能不适合于生产ITO粉体。因此，目前，工业规模上不进行ITO粉体的干法合成。However, the above-mentioned dry synthesis method may not be suitable for producing ITO powder. Therefore, at present, the dry synthesis of ITO powder is not carried out on an industrial scale.

专利文献1：日本专利申请公开No.62-21751Patent Document 1: Japanese Patent Application Laid-Open No. 62-21751

专利文献2：日本专利申请公开No.5-193939Patent Document 2: Japanese Patent Application Laid-Open No. 5-193939

专利文献3：日本专利申请公开No.6-191846Patent Document 3: Japanese Patent Application Laid-Open No. 6-191846

专利文献4：日本专利申请公开No.2001-261336Patent Document 4: Japanese Patent Application Laid-Open No. 2001-261336

专利文献5：日本专利申请公开No.62-21751Patent Document 5: Japanese Patent Application Laid-Open No. 62-21751

专利文献6：日本专利申请公开No.9-221322Patent Document 6: Japanese Patent Application Laid-Open No. 9-221322

专利文献7：日本专利申请公开No.2000-281337Patent Document 7: Japanese Patent Application Laid-Open No. 2000-281337

专利文献8：日本专利申请公开No.2001-172018Patent Document 8: Japanese Patent Application Publication No. 2001-172018

专利文献9：日本专利申请公开No.2002-68744Patent Document 9: Japanese Patent Application Laid-Open No. 2002-68744

专利文献10：日本专利申请公开No.11-11946Patent Document 10: Japanese Patent Application Laid-Open No. 11-11946

专利文献11：日本专利公告No.1-55201Patent Document 11: Japanese Patent Publication No. 1-55201

专利文献12：日本专利公告No.5-77601Patent Document 12: Japanese Patent Publication No. 5-77601

专利文献13：日本专利No.3253338Patent Document 13: Japanese Patent No. 3253338

专利文献14：日本专利No.3253339Patent Document 14: Japanese Patent No. 3253339

专利文献15：日本专利No.3229353Patent Document 15: Japanese Patent No. 3229353

专利文献16：日本专利No.3225073Patent Document 16: Japanese Patent No. 3225073

专利文献17：日本专利申请公开No.60-71037Patent Document 17: Japanese Patent Application Laid-Open No. 60-71037

专利文献18：日本专利申请公开No.2002-253953Patent Document 18: Japanese Patent Application Laid-Open No. 2002-253953

专利文献19：日本专利申请公开No.2002-253954Patent Document 19: Japanese Patent Application Laid-Open No. 2002-253954

专利文献20：日本专利申请公开No.2002-263474Patent Document 20: Japanese Patent Application Laid-Open No. 2002-263474

发明内容 Contents of the invention

本发明待解决的问题Problems to be solved by the present invention

在这样的情形下，本发明的目的是提供生产微粒的方法，该方法能够通过简单设备以低成本生产例如氧化物微粒的微粒，并且该方法适合于生产ITO粉体。本发明的另一个目的是提供生产该微粒的设备。Under such circumstances, an object of the present invention is to provide a method of producing microparticles, which can produce microparticles such as oxide microparticles at low cost by simple equipment, and which is suitable for producing ITO powder. Another object of the present invention is to provide an apparatus for producing the microparticles.

解决问题的方式way to solve the problem

在用于达到上述目的本发明的第一种模式中，提供了生产微粒的方法，其特征在于该方法包括将液流、液滴或粉体形式的原料供入热源；通过雾状液体的流体捕集形成的微粒形式的产物；并通过气-液分离以浆料形式收集微粒，其中所述热源为有火焰的热源。In a first mode of the present invention for achieving the above objects, there is provided a method of producing microparticles, characterized in that the method comprises feeding a material in the form of a liquid stream, liquid droplets or powder to a heat source; trapping the product formed as particulates; and collecting the particulates as a slurry by gas-liquid separation, wherein the heat source is a flamed heat source.

依照第一种模式，通过雾状液体流体可以有效的以微粒形式捕集将原料供入热源而得到的产物，并且通过气-液分离有效的以浆料形式收集的微粒。According to the first mode, the product obtained by supplying the raw material to the heat source can be effectively trapped in the form of fine particles by the mist liquid fluid, and the fine particles collected in the form of slurry can be effectively collected by the gas-liquid separation.

本发明的第二种模式可以被描绘成第一种模式的方法的特定实施方案，其中通过将熔融材料形成液流或液滴来提供待供入热源的原料。The second mode of the invention can be described as a specific embodiment of the method of the first mode, wherein the feedstock to be fed to the heat source is provided by forming molten material into streams or droplets.

依照第二种模式，可以在热源中将由例如金属或合金的熔融材料形成的液流或液滴形式的原料转变成它的氧化物，并且可以通过雾状液体流体以微粒形式捕集氧化物。According to a second mode, the feedstock in the form of a stream or droplets formed from molten material such as a metal or alloy can be converted to its oxide in a heat source and the oxide can be trapped in particulate form by the sprayed liquid flow.

本发明的第三种模式可以被描绘成第一种模式的方法的特定实施方案，其中待供入热源的原料是雾化粉体的形式。A third mode of the invention can be described as a specific implementation of the method of the first mode, wherein the raw material to be fed to the heat source is in the form of an atomized powder.

依照第三种模式，将由例如金属或合金的原料形成的雾化粉体形式的原料供入热源，由此形成其微粒。According to a third mode, a raw material in the form of an atomized powder formed of a raw material such as a metal or an alloy is supplied to a heat source, thereby forming particles thereof.

本发明的第四种模式可以被描绘成第一至第三种模式任何一个的方法的特定实施方案，其中通过旋风分离器进行气-液分离。The fourth mode of the present invention can be described as a specific embodiment of the method of any one of the first to third modes, wherein the gas-liquid separation is performed by a cyclone separator.

依照第四种模式，可以通过利用旋风分离器进行的气-液分离将微粒作为液体流体的浆料收集。According to a fourth mode, the particles can be collected as a slurry of liquid fluid by gas-liquid separation using a cyclone.

本发明的第五种模式可以被描绘成第一至第四种模式任何一个的方法的特定实施方案，其中该热源是乙炔焰或DC等离子焰。A fifth mode of the present invention can be described as a specific embodiment of the method of any one of the first to fourth modes, wherein the heat source is an acetylene flame or a DC plasma flame.

依照第五种模式，通过乙炔焰或DC等离子焰使原料形成为其微粒。According to a fifth mode, the raw material is formed into its particles by means of an acetylene flame or a DC plasma flame.

本发明的第六种模式可以被描绘成第一至第五种模式任何一个的方法的特定实施方案，其中该液体流体是水。A sixth mode of the invention can be described as a specific embodiment of the method of any one of the first to fifth modes, wherein the liquid fluid is water.

依照第六种模式，用水捕集产物，并收集产物-水的浆料。According to a sixth mode, the product is captured with water and a product-water slurry is collected.

本发明的第七种模式可以被描绘成第一至第六种模式任何一个的方法的特定实施方案，其中该原料是选自金属、合金、氧化物、氮化物和氮氧化物中的至少一种。A seventh mode of the present invention can be described as a specific embodiment of the method of any one of the first to sixth modes, wherein the raw material is at least one selected from the group consisting of metals, alloys, oxides, nitrides, and oxynitrides. kind.

依照第七种模式，将例如金属、合金、氧化物、氮化物和氮氧化物的原料形成为其微粒。According to the seventh mode, raw materials such as metals, alloys, oxides, nitrides, and oxynitrides are formed into their fine particles.

本发明的第八种模式可以被描绘成第一至第七种模式任何一个的方法的特定实施方案，其中该热源是氧化气氛或氮化气氛，由此产生氧化物微粒、氮化物微粒和氮氧化物微粒。An eighth mode of the present invention can be described as a specific embodiment of the method of any one of the first to seventh modes, wherein the heat source is an oxidizing atmosphere or a nitriding atmosphere, thereby producing oxide particles, nitride particles and nitrogen oxide particles.

依照第八种模式，在作为热源的氧化气氛或氮化气氛中将原料转变成氧化物微粒、氮化物微粒或氮氧化物微粒。According to the eighth mode, the raw material is converted into oxide fine particles, nitride fine particles or nitrogen oxide fine particles in an oxidizing atmosphere or a nitriding atmosphere as a heat source.

本发明的第九种模式可以被描绘成第一至第七种模式任何一个的方法的特定实施方案，其中原料是In-Sn合金或ITO粉体，由该原料生产氧化铟-氧化锡粉体。The ninth mode of the present invention can be described as a specific embodiment of the method of any one of the first to seventh modes, wherein the raw material is In-Sn alloy or ITO powder, and the indium oxide-tin oxide powder is produced from the raw material .

依照第九种模式，由In-Sn合金或ITO粉体生产ITO粉体的浆料。According to the ninth mode, a slurry of ITO powder is produced from In-Sn alloy or ITO powder.

本发明的第十种模式可以被描绘成第九种模式的方法的特定实施方案，该实施方案生产氧化铟-氧化锡粉体，该粉体的锡含量是2.3-45质量百分比，基于SnO2计算。A tenth mode of the present invention can be described as a specific embodiment of the method of the ninth mode, which produces an indium oxide-tin oxide powder having a tin content of 2.3-45 mass percent based on SnO2 calculate.

依照第十种模式，ITO通过预定量的氧化锡保持了导电性。According to the tenth mode, ITO maintains conductivity by a predetermined amount of tin oxide.

本发明的第十一种模式可以被描绘成第一至第十种模式任何一个的方法的特定实施方案，其中当通过液体流体捕集产物时，产物以150m/s或更小的最大速率流动。The eleventh mode of the present invention can be described as a specific embodiment of the method of any one of the first to tenth modes, wherein when the product is captured by the liquid flow, the product flows at a maximum velocity of 150 m/s or less .

依照第十一种模式，可以在相对低的产物流速下产生微粒。According to the eleventh mode, particles can be generated at relatively low product flow rates.

本发明的第十二种模式中，提供了生产微粒的设备，其特征在于该设备包含：In a twelfth mode of the present invention, an apparatus for producing microparticles is provided, characterized in that the apparatus comprises:

用于将气体流体和产物引入设备内部的进口，该产物是通过将液流、液滴或粉体形式的原料供入热源得到的；Inlets for the introduction of gaseous fluids and products into the interior of the apparatus obtained by feeding raw materials in the form of liquid streams, droplets or powders to the heat source;

用于向引入的产物喷射雾状液体流体的流体喷射装置；a fluid injection device for spraying an atomized liquid fluid on the incoming product;

用于对由液体流体捕集的微粒进行气-液分离以便由此形成微粒浆料的第一气-液分离装置；和a first gas-liquid separation means for gas-liquid separation of particles trapped by the liquid fluid to thereby form a particle slurry; and

用于将包含未被液体流体捕集的微粒的气氛流体的一部分返回到流体喷射装置所在位置的第一循环装置。First circulation means for returning a portion of the atmospheric fluid containing particles not trapped by the liquid fluid to the location of the fluid ejection means.

依照第十二种模式，利用雾状液体以流体微粒形式捕集将原料供入热源得到的产物，随后进行气-液分离，并将至少一部分气氛流体通过循环装置循环，随后进行另一次气-液分离。由此，可以有效收集微粒。According to the twelfth mode, the product obtained by supplying the raw material to the heat source is captured in the form of fluid particles by means of mist liquid, followed by gas-liquid separation, and at least a part of the atmospheric fluid is circulated through the circulation device, followed by another gas-liquid separation. liquid separation. Thereby, fine particles can be efficiently collected.

本发明的第十三种模式可以被描绘成第十二种模式的设备的特定实施方案，该设备在第一气-液分离装置下游侧进一步包含第二气-液分离装置，提供第二气-液分离装置用于引入包含未被液体流体捕集的微粒的气氛流体的一部分，用于向气氛流体喷射雾状液体流体，并用于进行气-液分离，由此获得微粒的浆料。The thirteenth mode of the present invention can be described as a specific embodiment of the apparatus of the twelfth mode, which further comprises a second gas-liquid separation device on the downstream side of the first gas-liquid separation device, providing a second gas-liquid separation device. - Liquid separation means for introducing a portion of the atmospheric fluid containing particles not trapped by the liquid fluid, for spraying the atmospheric fluid with a mist of the liquid fluid, and for performing gas-liquid separation, thereby obtaining a slurry of particles.

依照第十三种模式，可以通过第二气-液分离装置有效收集未被收集的微粒。According to the thirteenth mode, uncollected fine particles can be efficiently collected by the second gas-liquid separation device.

本发明的第十四种模式可以被描绘成第十三种模式的设备的特定实施方案，该设备在第二气-液分离装置的下游侧进一步包含第二循环装置，该循环装置用于将包含未被液体流体捕集到的颗粒的气氛流体的一部分返回到第二气-液分离装置的入口。The fourteenth mode of the present invention can be described as a specific embodiment of the apparatus of the thirteenth mode, which further comprises a second circulation device on the downstream side of the second gas-liquid separation device, and the circulation device is used to convert A portion of the atmospheric fluid containing particles not trapped by the liquid fluid is returned to the inlet of the second gas-liquid separation device.

依照第十四种模式，对未通过第二气-液分离装置提供浆料的气氛气体进一步进行气-液分离，由此有效收集微粒。According to the fourteenth mode, gas-liquid separation is further performed on the atmospheric gas not supplied with the slurry through the second gas-liquid separation device, thereby effectively collecting fine particles.

本发明的第十五种模式可以被描绘成第十二至十四种模式任何一个的设备的特定实施方案，其中第一气-液分离装置是旋风分离器。A fifteenth mode of the invention can be characterized as a specific embodiment of the apparatus of any one of the twelfth to fourteenth modes, wherein the first gas-liquid separation means is a cyclone separator.

依照第十五种模式，可以通过旋风分离器连续且有效地进行气-液分离。According to the fifteenth mode, gas-liquid separation can be continuously and efficiently performed by the cyclone separator.

本发明的第十六种模式可以被描绘成第十二至十五种模式任何一个的设备的特定实施方案，其中当通过流体喷射装置喷射的液体流体捕集微粒时，流体以150m/s或更小的最大速率流动。A sixteenth mode of the present invention can be described as a particular embodiment of the apparatus of any one of the twelfth to fifteenth modes, wherein when the liquid fluid jetted by the fluid jetting means traps particles, the fluid travels at 150 m/s or Smaller maximum rate flow.

依照第十六种模式，能够以相对低的流速生产微粒。According to the sixteenth mode, particles can be produced at a relatively low flow rate.

发明效果Invention effect

如上文所述，依照本发明，将液流、液滴或粉体形式的原料金属或合金供入热源，并通过雾状液体流体捕集形成的微粒形式的产物。由此，能够以简单的方式有效生产微粒。As stated above, in accordance with the present invention, the feedstock metal or alloy in the form of a liquid stream, liquid droplets or powder is supplied to the heat source and the resulting product is captured in the form of particulates by a mist of the liquid flow. Microparticles can thus be efficiently produced in a simple manner.

附图简述Brief description of the drawings

图1：本发明的微粒生产设备的一个实施方案的示意布局。Figure 1: Schematic layout of one embodiment of the microparticle production apparatus of the present invention.

图2：本发明实施例1中生产的ITO粉体的X射线衍射图。Figure 2: X-ray diffraction pattern of the ITO powder produced in Example 1 of the present invention.

图3：本发明实施例2中生产的ITO粉体的X射线衍射图。Figure 3: X-ray diffraction pattern of the ITO powder produced in Example 2 of the present invention.

图4：本发明比较例1中生产的ITO粉体的X射线衍射图。Figure 4: X-ray diffraction pattern of the ITO powder produced in Comparative Example 1 of the present invention.

图5：本发明比较例2中生产的ITO粉体的X射线衍射图。Figure 5: X-ray diffraction pattern of the ITO powder produced in Comparative Example 2 of the present invention.

图6：本发明比较例3中生产的ITO粉体的X射线衍射图。Figure 6: X-ray diffraction pattern of the ITO powder produced in Comparative Example 3 of the present invention.

图7：本发明实施例3中生产的ITO粉体的X射线衍射图。Figure 7: X-ray diffraction pattern of the ITO powder produced in Example 3 of the present invention.

图8：本发明比较例4中生产的ITO粉体的X射线衍射图。Figure 8: X-ray diffraction pattern of the ITO powder produced in Comparative Example 4 of the present invention.

实施本发明的最佳方式Best Mode for Carrying Out the Invention

依照本发明的生产微粒的方法，将液流、液滴或粉体形式的原料供入热源。According to the method of producing microparticles of the present invention, the raw material in the form of a liquid stream, liquid droplets or powder is supplied to a heat source.

该原料可以是例如金属或合金，且具体的实例包括诸如Mg、Al、Zr、Fe、Si、In和Sn的金属，以及它们的合金。该原料可以是任何的该金属或合金的上述氧化物、氮化物和氧氮化物。这里所用的“氧化物”包括复合氧化物，且“氮化物”包括复合氮化物。The raw material may be, for example, a metal or an alloy, and specific examples include metals such as Mg, Al, Zr, Fe, Si, In, and Sn, and alloys thereof. The starting material may be any of the aforementioned oxides, nitrides and oxynitrides of the metal or alloy. As used herein, "oxide" includes composite oxides, and "nitride" includes composite nitrides.

可以将待供入的原料熔化形成液流或液滴，或者待供入的原料可以是粉体。换言之，可以将熔融金属从容器中以液流或液滴形式连续倒出。或者，可以将待供入的原料形成雾化粉体。The raw material to be fed may be melted to form a liquid stream or droplets, or the raw material to be fed may be a powder. In other words, the molten metal can be poured continuously from the container in a stream or in droplets. Alternatively, the raw material to be fed may be formed into an atomized powder.

在使用In-Sn合金作为原料的情形中，可以生产ITO粉体。此外，当使用ITO粉体作为原料时，可以生产不同类型的ITO材料。In the case of using an In-Sn alloy as a raw material, ITO powder can be produced. In addition, when using ITO powder as a raw material, different types of ITO materials can be produced.

该热源可以是氧化气氛或氮化气氛，且具体的实例包括乙炔焰和DC等离子焰。对热源的温度没有具体的限制，只要该热源能够熔化金属、合金、氧化物、氮化物或氮氧化物，并能够充分氧化或氮化原料。可以想到的是，在乙炔焰情形中该温度至少为数千摄氏度，而在DC等离子焰中温度至少为数万摄氏度。The heat source may be an oxidizing atmosphere or a nitriding atmosphere, and specific examples include an acetylene flame and a DC plasma flame. There is no specific limit to the temperature of the heat source, as long as the heat source can melt the metal, alloy, oxide, nitride or oxynitride, and can sufficiently oxidize or nitride the raw material. It is conceivable that this temperature is at least several thousand degrees Celsius in the case of an acetylene flame, and at least tens of thousands of degrees Celsius in a DC plasma flame.

将液流、液滴或粉体形式的原料供入上述乙炔焰或DC等离子焰中时，作为产物产生原料本身的、对应氧化物的、对应氮化物的或对应氮氧化物的气流。根据火焰的状态，该产物可以是原料自身(即金属或合金)或对应的氧化物、氮化物或氮氧化物。换言之，当该火焰是氧化气氛时，形成金属或合金的氧化物或氮氧化物，然而当该火焰是氮化气氛时，形成金属或合金的氮化物或氮氧化物。或者，当使用氧化物、氮化物或氮氧化物作为原料时，可以形成不同类型的氧化物、氮化物或氮氧化物。When the feedstock in the form of liquid streams, droplets or powder is fed into the aforementioned acetylene flame or DC plasma flame, a gas stream of the feedstock itself, corresponding to oxides, corresponding to nitrides or corresponding to nitrogen oxides is produced as a product. Depending on the state of the flame, this product can be the starting material itself (ie metal or alloy) or the corresponding oxide, nitride or oxynitride. In other words, when the flame is an oxidizing atmosphere, oxides or oxynitrides of metals or alloys are formed, whereas when the flame is a nitriding atmosphere, nitrides or oxynitrides of metals or alloys are formed. Alternatively, when oxides, nitrides or oxynitrides are used as raw materials, different types of oxides, nitrides or oxynitrides may be formed.

依照本发明，通过雾状液体流体捕集形成的产物。具体而言，将雾状液体流体，优选雾状水，喷射到乙炔焰或DC等离子焰产生的射流所运载的产物上。通过雾状液体流体的作用，产物被急冷形成微粒，并产生包含喷射液体中的微粒的浆料。According to the present invention, the product formed is captured by the mist-like liquid fluid. Specifically, an atomized liquid fluid, preferably water, is sprayed onto the product carried by the jets produced by the acetylene flame or DC plasma flame. The product is quenched into particles by the action of the sprayed liquid fluid, and a slurry containing the particles in the sprayed liquid is produced.

对待供入的雾状液体流体的类型没有具体的限制，只要该流体能捕集并冷却产物。例如，当使用水时，使用环境温度下的水(优选纯净水)。或者，也可以使用冷水。There is no particular restriction on the type of mist liquid fluid to be fed, as long as the fluid captures and cools the product. For example, when water is used, water (preferably purified water) at ambient temperature is used. Alternatively, cold water can also be used.

当捕集微粒形式的产物时，该产物以例如150m/s或更小，优选以大约100m/s或更小的最大速度流动。When trapping product in particulate form, the product flows at a maximum velocity of eg 150 m/s or less, preferably about 100 m/s or less.

依照本发明，对包含通过喷射液体流体捕集到的微粒的液体流体进行气-液分离，由此以浆料的形式收集微粒。对收集浆料的方法没有具体的限制，并优选使用旋风分离器。According to the present invention, a liquid fluid containing particles trapped by spraying the liquid fluid is subjected to gas-liquid separation, whereby the particles are collected in the form of a slurry. There is no specific limitation on the method of collecting the slurry, and it is preferable to use a cyclone separator.

依照本发明的方法，当使用In-Sn合金或ITO粉体作为原料时，可以产生氧化铟-氧化锡(ITO)的粉体。如此产生的ITO粉体包含大量溶解在In2O3中的SnO2固溶体组分。因此，该ITO表现出高的可烧结性并容易提供高密度的烧结ITO。结果，可以生产出长寿命的溅射靶。当使用通过各种生产方法生产的ITO粉体或通过粉碎烧结ITO产生的ITO粉体作为原料时，可以生产出特性与原料粉体不同并且包含大量溶解在In2O3中的SnO2固溶体组分的不同类型的ITO粉体。According to the method of the present invention, when In-Sn alloy or ITO powder is used as a raw material, indium oxide-tin oxide (ITO) powder can be produced. The ITO powder thus produced contains a large amount of SnO 2 solid solution components dissolved in In 2 O 3 . Therefore, the ITO exhibits high sinterability and easily provides high-density sintered ITO. As a result, long-life sputtering targets can be produced. When using ITO powder produced by various production methods or ITO powder produced by pulverizing and sintering ITO as a raw material, it is possible to produce a solid solution group of SnO 2 that has characteristics different from the raw material powder and contains a large amount of SnO 2 dissolved in In 2 O 3 Different types of ITO powders.

可以使用上述的ITO粉体作为ITO溅射靶的材料。ITO溅射靶材料优选具有2.3至45质量百分比的锡含量，基于SnO2计算。The above-mentioned ITO powder can be used as the material of the ITO sputtering target. The ITO sputtering target material preferably has a tin content of 2.3 to 45 mass percent, calculated on the basis of SnO2 .

实施例 Example

下面将参照图1描述本发明的微粒生产设备的一个实施方案。An embodiment of the microparticle production apparatus of the present invention will be described below with reference to FIG. 1 .

该设备具有用于向设备内部引入气体流体和产物3的入口10，通过将液流、液滴或粉体形式的原料2(例如金属和合金)供入作为热源并且可提供氧化气氛或氮化气氛的火焰1(乙炔焰或DC等离子焰)中得到产物3；用于向引入的微粒喷射雾状液体流体的流体喷射装置20；作为气-液分离装置的旋风分离器30，以便对被液体流体捕集的微粒进行气-液分离，从而形成微粒的浆料；和用于将一部分包含未被液体流体捕集的微粒的气氛流体返回到流体喷射装置所在位置的循环装置40。The apparatus has an inlet 10 for introducing gaseous fluids and products 3 into the interior of the apparatus by feeding raw materials 2 such as metals and alloys in the form of liquid streams, droplets or powders as heat sources and can provide an oxidizing atmosphere or nitriding Obtain product 3 in the flame 1 (acetylene flame or DC plasma flame) of atmosphere; Be used for spraying the fluid injection device 20 of atomized liquid fluid to the particle that introduces; As the cyclone separator 30 of gas-liquid separation device, so that the liquid fluid trapped particles undergoing gas-liquid separation to form a slurry of particles; and circulation means 40 for returning a portion of the atmospheric fluid containing particles not trapped by the liquid fluid to the location of the fluid ejection device.

对入口10的类型没有具体的限制，只要该入口容许包含产物的气流供入设备内部。该入口可以是吸气装置。There is no particular restriction on the type of inlet 10, as long as it allows a gas stream containing product to be fed into the interior of the device. The inlet may be a suction device.

在导管11中于入口10的下游侧提供流体喷射装置20。该流体喷射装置20包括，例如多个用于喷水的喷射喷嘴21，将流体供向喷射喷嘴21的泵22，和存储流体的流体容器23。对通过喷射喷嘴21喷出的流体的喷射方向没有具体的限制。然而，该喷射方向优选为，使喷射流体与通过入口10引入的气流合并。通过雾状液体流体(例如水)将包含在通过入口10引入的气体流体中的产物3冷却以便形成微粒，并捕集该微粒。在导管11中，在喷射喷嘴21的下游侧提供流路变窄的文氏管段12，以便防止液-气混合物的流速降低。文氏管段12的提供并不是必须的。并非必须提供喷射喷嘴21和泵22，相反，可以基于气体流动产生的吸力喷射液体。A fluid ejection device 20 is provided in the conduit 11 on the downstream side of the inlet 10 . The fluid ejection device 20 includes, for example, a plurality of ejection nozzles 21 for ejecting water, a pump 22 for supplying fluid to the ejection nozzles 21, and a fluid container 23 for storing the fluid. There is no specific limitation on the spray direction of the fluid sprayed through the spray nozzle 21 . However, the injection direction is preferably such that the injection fluid merges with the gas flow introduced through the inlet 10 . The product 3 contained in the gaseous fluid introduced through the inlet 10 is cooled by the mist liquid fluid (eg water) to form particles and the particles are trapped. In the conduit 11, a venturi section 12 in which the flow path is narrowed is provided on the downstream side of the injection nozzle 21 in order to prevent a decrease in the flow velocity of the liquid-gas mixture. The provision of the venturi section 12 is not mandatory. It is not necessary to provide the spray nozzle 21 and the pump 22, but instead, the liquid may be sprayed based on the suction generated by the gas flow.

提供有入口10的导管11与作为气-液分离装置的旋风分离器30的入口31相连。通过入口31引入到旋风分离器30中的气-液混合物形成绕旋风分离器体32内壁前进的涡流33，由此将液体组分与气体分离。液体组分，即包含微粒的浆料，在旋风分离器30中下降，而通过排气出口34将气体组分排出。A conduit 11 provided with an inlet 10 is connected to an inlet 31 of a cyclone 30 as gas-liquid separating means. The gas-liquid mixture introduced into the cyclone separator 30 through the inlet 31 forms a vortex 33 which advances around the inner wall of the cyclone body 32, thereby separating the liquid components from the gas. The liquid component, ie the slurry containing particles, descends in the cyclone 30 , while the gaseous component is discharged through the exhaust outlet 34 .

在该实施方案的设备中，提供循环装置40以便与排气出口34相连。换言之，循环管道41与出口34相连，并且循环管道41与导管11的入口10附近的位置相连。鼓风机42介于循环管41之中。循环装置40由部件41和42组成。通过循环装置40，将未被捕集的粉体返回到喷射喷嘴21的上游侧，从而提高捕集效率。In the apparatus of this embodiment, a circulation device 40 is provided so as to be connected to the exhaust outlet 34 . In other words, the circulation pipe 41 is connected to the outlet 34 , and the circulation pipe 41 is connected to a position near the inlet 10 of the conduit 11 . The blower 42 is interposed in the circulation pipe 41 . The circulation device 40 consists of components 41 and 42 . By the circulation device 40, the uncollected powder is returned to the upstream side of the injection nozzle 21, thereby improving the collection efficiency.

将通过旋风分离器30与气体分离的液体组分通过排水出口36排出并存储在流体容器23中。通过循环装置40将容器23中浆料的上层清水循环，由此包含微粒的浆料的浓度逐渐增加。The liquid components separated from the gas by the cyclone separator 30 are discharged through the drain outlet 36 and stored in the fluid container 23 . The clear water in the upper layer of the slurry in the container 23 is circulated by the circulation device 40, whereby the concentration of the slurry containing fine particles gradually increases.

通过排气出口34将旋风分离器30产生的排出气中的大部分循环至循环管道41。将一部分排出气，例如排出气体量的约1/10，通过第二排气出口35排出。Most of the exhaust gas produced by the cyclone separator 30 is circulated to the circulation pipe 41 through the exhaust outlet 34 . A part of the exhaust gas, for example about 1/10 of the exhaust gas volume, is discharged through the second exhaust outlet 35 .

在本实施方案的设备中，作为第二气-液分离装置的第二旋风分离器50通过排气管道43与第二排气出口35相连。第二旋风分离器50基本上具有与旋风分离器30相同的结构，并用作气-液分离装置。具体地，通过与排气管道43相连的入口51引入到第二旋风分离器50中的气-液混合物形成绕旋风分离器体52内壁前进的涡流53，由此将液体组分与气体分离。液体组分，即包含微粒的浆料，在旋风分离器50中下降，并通过排水出口54被排出并存储在流体容器61中。更具体地，流路变窄的文氏管段44介于排气管道43中，并提供水循环管道62以便保持文氏管段44与流体容器61的连通。当在文氏管段44中提供高速气流时，容纳在流体容器中61的水会被抽出并喷入文氏管段44，由此可以用水(液体)捕集残留在气相中的微粒。排气管道71与排气出口55相连，并在排气管道71中提供第二鼓风机72，以便通过第二鼓风机72的帮助将气体通过排气出口55排出。可以通过关于旋风分离器30所提到的泵和喷射喷嘴将容纳在水容器61中的水喷入排气管道43中。同样如上文所提到的，可以为流体容器61配备过滤器和沉淀容器以便通过中和作用从液体中分离微粒。另外，可以将通过排气出口55排出的一部分气体循环到排气管道43的文氏管段44的上游侧，以便由此提高捕集效率。In the apparatus of this embodiment, the second cyclone separator 50 as the second gas-liquid separation device is connected to the second exhaust outlet 35 through the exhaust pipe 43 . The second cyclone separator 50 basically has the same structure as the cyclone separator 30, and serves as a gas-liquid separation device. Specifically, the gas-liquid mixture introduced into the second cyclone 50 through the inlet 51 connected to the exhaust duct 43 forms a vortex 53 advancing around the inner wall of the cyclone body 52, thereby separating the liquid components from the gas. The liquid component, ie the slurry containing particles, descends in the cyclone separator 50 and is drained through the drain outlet 54 and stored in the fluid container 61 . More specifically, a venturi section 44 with a narrowed flow path is interposed in the exhaust duct 43 , and a water circulation duct 62 is provided to maintain communication between the venturi section 44 and the fluid container 61 . When a high-speed gas flow is provided in the venturi section 44, the water contained in the fluid container 61 is drawn out and sprayed into the venturi section 44, whereby particles remaining in the gas phase can be trapped with water (liquid). An exhaust duct 71 is connected to the exhaust outlet 55 , and a second blower 72 is provided in the exhaust duct 71 so as to exhaust gas through the exhaust outlet 55 with the help of the second blower 72 . The water contained in the water container 61 can be sprayed into the exhaust duct 43 by means of the pump and spray nozzles mentioned for the cyclone separator 30 . Also as mentioned above, the fluid container 61 can be equipped with a filter and a settling container to separate particles from the liquid by neutralization. In addition, a part of the gas exhausted through the exhaust outlet 55 may be circulated to the upstream side of the venturi section 44 of the exhaust duct 43 to thereby increase the trapping efficiency.

当旋风分离器30提供足够的微粒捕集效率时，不必提供第二旋风分离器50。为了进一步提高捕集效率，可以将多个旋风分离器连接在一起。When the cyclone 30 provides sufficient particle trapping efficiency, it is not necessary to provide the second cyclone 50 . To further increase collection efficiency, multiple cyclones can be connected together.

下面将描述使用上述实施方案的设备的微粒生产实施例。An example of microparticle production using the apparatus of the above-described embodiment will be described below.

实施例1Example 1

将In-Sn合金(Sn：9.6wt％)的雾化粉体(平均颗粒尺寸：45μm)引入乙炔焰，由此在干态下合成ITO(In2O3:SnO2＝90:10wt％)粉体。通过袋滤器在干态下收集该粉体，由此产生实施例1的ITO粉体。Atomized powder (average particle size: 45 μm) of In—Sn alloy (Sn: 9.6 wt%) was introduced into an acetylene flame, thereby synthesizing ITO in a dry state (In 2 O 3 :SnO 2 =90:10 wt%) Powder. The powder was collected in a dry state by a bag filter, thereby yielding the ITO powder of Example 1.

实施例2Example 2

以类似于实施例1的方式，在干态下通过乙炔焰合成ITO粉体。通过向粉体喷水在湿态下收集该粉体，由此产生实施例2的ITO粉体。In a manner similar to Example 1, ITO powder was synthesized by acetylene flame in a dry state. The powder was collected in a wet state by spraying water on the powder, whereby the ITO powder of Example 2 was produced.

比较例1Comparative example 1

在1000℃下煅烧湿态下合成的氧化铟粉体。类似地，在1000℃下煅烧湿态下合成的氧化锡粉体。通过研钵混合如此煅烧的氧化铟粉体(90质量％)和氧化锡粉体(10质量％)，由此产生比较例1的氧化物粉体(标准产物1)。The indium oxide powder synthesized in the wet state was calcined at 1000°C. Similarly, the wet synthesized tin oxide powder was calcined at 1000 °C. The thus-calcined indium oxide powder (90% by mass) and tin oxide powder (10% by mass) were mixed by a mortar, thereby producing the oxide powder of Comparative Example 1 (Standard Product 1).

比较例2Comparative example 2

在湿态下通过共沉淀合成ITO粉体，由此产生比较例2的ITO粉体。The ITO powder was synthesized by co-precipitation in a wet state, whereby the ITO powder of Comparative Example 2 was produced.

通过如下程序进行共沉淀湿法合成。首先，在环境温度下将In(4N)(20g)溶解在硝酸(特级试剂，浓度：60-61％)(133cc)中，由此产生溶液(pH＝-1.5)。类似地，在环境温度下将Sn(4N)(2.12g)溶解在盐酸(特级试剂，浓度：35-36％)(100cc)中，由此产生溶液(pH＝-1.9)。将两种溶液混合，从而得到混合酸溶液。混合过程中没有观察到沉淀，并且发现混合溶液的pH为-1.5。随后，向该酸性溶液中加入25％的氨水(特级试剂)进行中和，由此将pH调节至6.5，并析出白色物质。几小时之后，去除上层清液，并用纯净水清洗沉淀物(2L×3)，随后在80℃下干燥，在600℃下烘烤三小时，并脱水，由此通过湿法合成产生ITO粉体。Co-precipitation wet synthesis was performed by the following procedure. First, In(4N) (20 g) was dissolved in nitric acid (special grade reagent, concentration: 60-61%) (133 cc) at ambient temperature, thereby producing a solution (pH=-1.5). Similarly, Sn(4N) (2.12 g) was dissolved in hydrochloric acid (special grade reagent, concentration: 35-36%) (100 cc) at ambient temperature, thereby producing a solution (pH=-1.9). The two solutions are mixed to obtain a mixed acid solution. No precipitation was observed during mixing, and the pH of the mixed solution was found to be -1.5. Subsequently, 25% ammonia water (special grade reagent) was added to the acidic solution for neutralization, whereby the pH was adjusted to 6.5, and a white substance was precipitated. After several hours, the supernatant was removed, and the precipitate (2L×3) was washed with purified water, then dried at 80°C, baked at 600°C for three hours, and dehydrated, thereby producing ITO powder by wet synthesis .

比较例3Comparative example 3

在1550℃或更高温度下，烧结湿态下合成的氧化铟粉体和氧化锡粉体的混合物(氧化锡含量：10wt％)。将烧结ITO磨碎，由此产生比较例3的ITO粉体。A mixture of indium oxide powder and tin oxide powder synthesized in a wet state (tin oxide content: 10 wt %) was sintered at 1550° C. or higher. The sintered ITO was pulverized, whereby the ITO powder of Comparative Example 3 was produced.

测试实施例1Test Example 1

分析实施例1和2与比较例1-3的每个ITO粉体的SnO2固溶体含量。检测程序如下。测试之前，在空气中将实施例1和2以及比较例2和3的ITO粉体在1000℃下煅烧三小时以便使析出的SnO2微粒生长成易于检测的SnO2大颗粒，The SnO 2 solid solution content of each ITO powder of Examples 1 and 2 and Comparative Examples 1-3 was analyzed. The detection procedure is as follows. Before the test, the ITO powders of Examples 1 and 2 and Comparative Examples 2 and 3 were calcined at 1000° C. for three hours in air in order to make the precipitated SnO 2 particles grow into easily detectable SnO 2 large particles,

1.进行感应耦合高频等离子分光分析(ICP分光分析)。为了计算，假定各ITO粉体只是由In、Sn和氧(O)组成，并且可以具有一定量的氧不足。根据分析值计算In与Sn的比值，并计算在所有In和Sn元素分别转变成In2O3和SnO2条件下的In2O3与SnO2的重量比。1. Perform inductively coupled high-frequency plasma spectroscopic analysis (ICP spectroscopic analysis). For calculation, it is assumed that each ITO powder is composed of only In, Sn, and oxygen (O), and may have a certain amount of oxygen deficiency. Calculate the ratio of In to Sn from the analytical values, and calculate the weight ratio of In 2 O 3 to SnO 2 under the condition that all In and Sn elements are transformed into In 2 O 3 and SnO 2 , respectively.

2.对实施例1和2以及比较例1-3的ITO粉体进行粉末X射线衍射分析(XRD：利用MXP 18II，Mac Science的产品)，由此测定各粉体的析出SnO2含量。在各情形中，从对应的衍射图检查复合氧化物(In4Sn3O12)的存在。未检测出该复合氧化物时，根据In2O3(222)的积分衍射强度与SnO2(110)的积分衍射强度的比值，相对于比较例1的标准产物1，确定ITO粉体的析出SnO2含量(质量百分比)。具体地，析出SnO2含量(质量百分比)是根据SnO2的X射线衍射积分强度得到的SnO2含量，假定未溶解在In2O3中并且通过约1000℃的煅烧生长的SnO2组分可表现出SnO2(110)的X射线衍射峰。图2至图6显示了X射线衍射分析的结果。2. The ITO powders of Examples 1 and 2 and Comparative Examples 1-3 were subjected to powder X-ray diffraction analysis (XRD: using MXP 18II, a product of Mac Science), thereby determining the precipitated SnO content of each powder. In each case, the presence of a composite oxide (In 4 Sn 3 O 12 ) was checked from the corresponding diffractogram. When the composite oxide was not detected, the precipitation of the ITO powder was determined based on the ratio of the integrated diffraction intensity of In 2 O 3 (222) to the integrated diffraction intensity of SnO 2 (110), relative to the standard product 1 of Comparative Example 1. SnO content (mass percent). Specifically, the precipitated SnO2 content (mass percentage) is the SnO2 content obtained according to the X-ray diffraction integrated intensity of SnO2 , assuming that the SnO2 component that is not dissolved in In2O3 and grown by calcination at about 1000 °C can be Exhibits an X-ray diffraction peak of SnO 2 (110). Figures 2 to 6 show the results of X-ray diffraction analysis.

3.基于“1”和“2”的结果，由通过ICP分析检测到但没有通过X射线衍射作为SnO2(110)检测到的SnO2量得到各ITO粉体的SnO2固溶体含量(In2O3中)。3. Based on the results of "1" and "2", the SnO 2 solid solution content (In 2 O 3 ).

结果如表1所示。The results are shown in Table 1.

发现实施例1和2的ITO粉体具有2.35wt％和2.42wt％的SnO2固溶体含量，这高于通过湿法合成所得比较例2的ITO粉体的SnO2固溶体含量2.26wt％。发现通过粉碎烧结产物产生的比较例3的ITO粉体形成复合氧化物。因此，不能测定比较例3的ITO粉体的SnO2固溶体含量。The ITO powders of Examples 1 and 2 were found to have SnO2 solid solution content of 2.35wt% and 2.42wt%, which was higher than the SnO2 solid solution content of 2.26wt% of the ITO powder of Comparative Example 2 obtained by wet synthesis. It was found that the ITO powder of Comparative Example 3 produced by pulverizing the sintered product formed a composite oxide. Therefore, the SnO 2 solid solution content of the ITO powder of Comparative Example 3 could not be measured.

表1Table 1

Figure C200480041059D00161
Figure C200480041059D00161

实施例3Example 3

将In-Sn合金(Sn：9.6wt％)的雾化粉体(平均颗粒尺寸：45μm)引入DC等离子焰，以便由此在干态下合成ITO(In2O3:SnO2＝90:10wt％)粉体。通过向粉体喷射水在湿态下收集该粉体，由此产生实施例3的ITO粉体。Atomized powder (average particle size: 45 μm) of In—Sn alloy (Sn: 9.6 wt %) was introduced into a DC plasma flame to thereby synthesize ITO in a dry state (In 2 O 3 :SnO 2 =90:10 wt %) powder. The powder was collected in a wet state by spraying water on the powder, whereby the ITO powder of Example 3 was produced.

比较例4Comparative example 4

类似于比较例1，在1000℃下煅烧湿态下合成的氧化铟粉体。类似地，在1000℃下煅烧湿态下合成的氧化锡粉体。通过研钵将如此煅烧的氧化铟粉体(90质量百分比)和氧化锡粉体(10质量百分比)混合，由此产生比较例4的氧化物粉体(标准产物2)Similar to Comparative Example 1, the indium oxide powder synthesized in wet state was calcined at 1000°C. Similarly, the wet synthesized tin oxide powder was calcined at 1000 °C. The thus-calcined indium oxide powder (90 mass percent) and tin oxide powder (10 mass percent) were mixed by a mortar, thereby producing the oxide powder of Comparative Example 4 (standard product 2)

测试实施例2Test Example 2

类似于测试实施例1，分析实施例3和比较例4的各ITO粉体的SnO2固溶体含量。通过X’PertPRO MPD(Spectris有限公司的产品)进行粉末X射线衍射分析(XRD)。结果如表2所示。图7和图8显示了X射线衍射分析的结果。Similar to Test Example 1, the SnO 2 solid solution content of each ITO powder of Example 3 and Comparative Example 4 was analyzed. Powder X-ray diffraction analysis (XRD) was performed by X'PertPRO MPD (product of Spectris Co., Ltd.). The results are shown in Table 2. Figures 7 and 8 show the results of X-ray diffraction analysis.

发现实施例3的ITO粉体的SnO2固溶体含量为3.00wt％，这显著高于通过乙炔焰而非DC等离子焰得到的实施例2的ITO粉体的SnO2固溶体含量。It was found that the SnO2 solid solution content of the ITO powder of Example 3 was 3.00 wt%, which was significantly higher than that of the ITO powder of Example 2 obtained by acetylene flame instead of DC plasma flame.

表2Table 2

Claims (16)

1. produce the method for particulate, it is characterized in that this method comprises that the raw material with liquid stream, drop or powder form infeeds thermal source; Capture the product of the particulate form that forms by the fog-like liquid fluid; And separate with slurry form by solution-air and to collect particulate, wherein said thermal source is the thermal source that flame is arranged.
2. according to the method for the production particulate of claim 1, wherein provide the raw material of waiting to infeed thermal source by melting material being formed liquid stream or drop.
3. according to the method for the production particulate of claim 1, the raw material of wherein waiting to infeed thermal source is the form of atomizing powder.
4. according to the method for the production particulate of claim 1, wherein carry out this solution-air and separate by cyclonic separator.
5. according to the method for the production particulate of claim 1, wherein this thermal source is acetylene flame or DC flame passes.
6. according to the method for the production particulate of claim 1, wherein this liquid fluid is a water.
7. according to the method for the production particulate of claim 1, wherein this raw material is to be selected from least a in metal, alloy, oxide compound, nitride and the oxynitride.
8. according to the method for the production particulate of claim 1, wherein this thermal source is oxidizing atmosphere or nitriding atmosphere, produces oxide fine particle, nitride particulate or oxynitride particulate thus.
9. according to the method for the production particulate of claim 1, wherein raw material is In-Sn alloy or ITO powder, by this raw material production indium oxide-tin oxide body.
10. according to the method for the production particulate of claim 9, this method produces tin content and presses SnO 2Be calculated as the indium oxide-tin oxide body of 2.3-45 mass percent.
11. according to the method for any one production particulate of claim 1 to 10, wherein when capturing product by liquid fluid, this product flows with 150m/s or littler maximum rate.
12. produce the equipment of particulate, it is characterized in that this equipment comprises:
Be used for the import with gaseous fluid and product introducing device interior, this product is to infeed thermal source by the raw material with liquid stream, drop or powder form to obtain;
Be used for spraying fog-like liquid fluidic fluid jet device to the product of introducing;
Being used for that the particulate that is captured by liquid fluid is carried out solution-air separates so that form first gas-liquid separation device of particulate slurry thus; With
An atmosphere fluidic part that is used for comprising not the particulate that is captured by liquid fluid turns back to first circulation device of fluid jet device position.
13. equipment according to the production particulate of claim 12, this equipment comprises second gas-liquid separation device in addition in the first gas-liquid separation device downstream side, the atmosphere fluidic part of the particulate that is captured by liquid fluid is provided second gas-liquid separation device to be used to introduce to comprise not, be used for to atmosphere fluid jet fog-like liquid fluid, and be used to carry out the solution-air separation, obtain the slurry of particulate thus.
14. equipment according to the production particulate of claim 13, this equipment comprises second circulation device in addition in the downstream side of second gas-liquid separation device, and the atmosphere fluidic part that this second circulation device is used for comprising not the particulate that is captured by liquid fluid turns back to the inlet of second gas-liquid separation device.
15. according to the equipment of the production particulate of claim 12, wherein first gas-liquid separation device is a cyclonic separator.
16. according to the equipment of any one production particulate of claim 12 to 15, wherein when the liquid fluid trap particles of spraying by fluid jet device, fluid flows with 150m/s or littler maximum rate.
CNB200480041059XA 2003-12-25 2004-12-24 Method and apparatus for producing fine particles Expired - Fee Related CN100522800C (en)

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WO2005066069A1 (en) 2005-07-21
CN1906125A (en) 2007-01-31
JPWO2005066069A1 (en) 2007-07-26
KR20060109505A (en) 2006-10-20
TW200536776A (en) 2005-11-16
KR100907735B1 (en) 2009-07-14

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