JPWO2005066069A1 - Fine particle production method and production apparatus - Google Patents

Fine particle production method and production apparatus Download PDF

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JPWO2005066069A1
JPWO2005066069A1 JP2005516840A JP2005516840A JPWO2005066069A1 JP WO2005066069 A1 JPWO2005066069 A1 JP WO2005066069A1 JP 2005516840 A JP2005516840 A JP 2005516840A JP 2005516840 A JP2005516840 A JP 2005516840A JP WO2005066069 A1 JPWO2005066069 A1 JP WO2005066069A1
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fine particles
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JP4864459B2 (en
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高橋　誠一郎
誠一郎 高橋
渡辺　弘
渡辺　　弘
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Mitsui Mining and Smelting Co Ltd
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Abstract

酸化物微粒子等の微粒子をより簡便な装置で且つ低コストで製造でき、ＩＴＯ粉末の製造に好適な微粒子の製造方法及び製造装置を提供する。 微粒子を製造する方法において、原料を液流、液滴又は粉末として、熱源中に供給し、生成物を霧状の液状流体により微粒子として捕獲し、気液分離により前記微粒子をスラリーとして回収する。Provided are a fine particle production method and a production apparatus that can produce fine particles such as oxide fine particles with a simpler apparatus and at a lower cost, and are suitable for production of ITO powder. In the method for producing fine particles, the raw material is supplied as a liquid stream, droplets or powder into a heat source, the product is captured as fine particles with a mist-like liquid fluid, and the fine particles are recovered as a slurry by gas-liquid separation.

Description

本発明は、酸化インジウム−酸化錫粉末などの微粒子の製造方法及び製造装置に関する。  The present invention relates to a method and apparatus for producing fine particles such as indium oxide-tin oxide powder.

一般的に、薄膜を成膜する方法の１つとしてスパッタリング法が知られている。スパッタリング法とは、スパッタリングターゲットをスパッタリングすることにより薄膜を得る方法であり、大面積化が容易であり、高性能の膜が効率よく成膜できるため、工業的に利用されている。また、近年、スパッタリングの方式として、反応性ガスの中でスパッタリングを行う反応性スパッタリング法や、ターゲットの裏面に磁石を設置して薄膜形成の高速化を図るマグネトロンスパッタリング法なども知られている。  In general, a sputtering method is known as one of methods for forming a thin film. The sputtering method is a method of obtaining a thin film by sputtering a sputtering target, is easy to increase in area, and can be efficiently formed into a high-performance film, and is used industrially. In recent years, as sputtering methods, there are known a reactive sputtering method in which sputtering is performed in a reactive gas, and a magnetron sputtering method in which a magnet is placed on the back surface of a target to increase the speed of thin film formation.

このようなスパッタリング法で用いられる薄膜のうち、特に、酸化インジウム−酸化錫（Ｉｎ２Ｏ３−ＳｎＯ２の複合酸化物、以下、「ＩＴＯ」という）膜は、可視光透過性が高く、かつ導電性が高いので透明導電膜として液晶表示装置やガラスの結露防止用発熱膜、赤外線反射膜等に幅広く用いられている。Among the thin films used in such a sputtering method, in particular, an indium oxide-tin oxide (In 2 O 3 —SnO 2 composite oxide, hereinafter referred to as “ITO”) film has high visible light transmittance, and Because of its high conductivity, it is widely used as a transparent conductive film for liquid crystal display devices, heat generation films for preventing condensation of glass, infrared reflective films, and the like.

このため、より効率よく低コストで成膜するために、現在においてもスパッタ条件やスパッタ装置などの改良が日々行われており、装置を如何に効率的に稼働させるかが重要となる。また、このようなＩＴＯスパッタリングにおいては、新しいスパッタリングターゲットをセットしてから初期アーク（異常放電）がなくなって製品を製造できるまでの時間が短いことと、一度セットしてからどれくらいの期間使用できるか（積算スパッタリング時間：ターゲットライフ）が問題となる。  For this reason, in order to form a film more efficiently and at a lower cost, improvement of sputtering conditions and a sputtering apparatus are carried out every day, and it is important how to operate the apparatus efficiently. In addition, in such ITO sputtering, the time from when a new sputtering target is set until the initial arc (abnormal discharge) disappears and the product can be manufactured is short, and how long can it be used once set? (Integrated sputtering time: target life) becomes a problem.

このようなＩＴＯスパッタリングターゲットは、酸化インジウム粉末及び酸化錫粉末を所定の割合で混合して乾式又は湿式で成形し、焼結したものであり（特許文献１）、高密度のＩＴＯ焼結体を得るための高分散性の酸化インジウム粉末が提案されている（特許文献２，３，４等参照）。  Such an ITO sputtering target is obtained by mixing indium oxide powder and tin oxide powder at a predetermined ratio, molding them in a dry or wet manner, and sintering them (Patent Document 1). A highly dispersible indium oxide powder to be obtained has been proposed (see Patent Documents 2, 3, 4, etc.).

また、共沈法により湿式合成されたＩＴＯ粉末をＩＴＯ焼結体とすることも知られており（特許文献５等参照）、同様に高密度な焼結体を得るためのＩＴＯ粉末の湿式合成方法が多数提案されている（特許文献６〜９等参照）。  It is also known that ITO powder wet-synthesized by the coprecipitation method is used as an ITO sintered body (see Patent Document 5 etc.), and wet synthesis of ITO powder to obtain a high-density sintered body similarly. Many methods have been proposed (see Patent Documents 6 to 9).

さらに、プラズマアーク中でインジウム−錫合金と酸素とを反応させて、マッハ１以上のガス流で所定の冷却速度以上で冷却することによりＩＴＯ粉末を製造する方法が提案されている（特許文献１０参照）。しかしながら、マッハ１以上の高速ガス流を用いるなど、設備が大がかりになり、安価に効率よくＩＴＯ粉末を製造することができないという問題がある。  Furthermore, a method for producing ITO powder by reacting an indium-tin alloy with oxygen in a plasma arc and cooling at a predetermined cooling rate or higher with a gas flow of Mach 1 or higher is proposed (Patent Document 10). reference). However, there is a problem that the equipment becomes large, such as using a high-speed gas flow of Mach 1 or more, and ITO powder cannot be manufactured efficiently at low cost.

一方、ＩＴＯ粉末の製造方法ではないが、金属酸化物微粒子の製造方法としては、以下の方法が提案されている。例えば、金属粉末をバーナ火炎中に供給し、酸化物超微粒子を製造し、固気相分離する各種方法が提案されている（特許文献１１〜１６等参照）。また、溶融金属に気体を噴射して粉体化し、気体で搬送される粉体を液体中に導入して化学反応および濃縮等の反応を起こさせて微粉体を製造する方法が提案されている（特許文献１７参照）。さらに、金属バルク又は金属酸化物棒などの原料体にプラズマアークをあてて原料体を溶融蒸発させ、この蒸発ガスに反応・冷却ガスを吹き付けて超微粒子を形成する方法が提案されている（特許文献１８〜２０参照）。  On the other hand, although it is not a manufacturing method of ITO powder, the following method is proposed as a manufacturing method of metal oxide fine particles. For example, various methods have been proposed in which metal powder is supplied into a burner flame, ultrafine oxide particles are produced, and solid-phase separation is performed (see Patent Documents 11 to 16 and the like). In addition, a method has been proposed in which a gas is injected into molten metal to form powder, and a powder conveyed by gas is introduced into the liquid to cause a reaction such as a chemical reaction and concentration to produce a fine powder. (See Patent Document 17). Furthermore, a method has been proposed in which a plasma arc is applied to a raw material body such as a metal bulk or a metal oxide rod to melt and evaporate the raw material body, and a reaction / cooling gas is sprayed on the evaporated gas to form ultrafine particles (patent) Reference 18-20).

しかしながら、このような乾式合成は、ＩＴＯ粉末に適さないためか、現在、ＩＴＯ粉末の乾式合成は工業的に行われていない。
特開昭６２−２１７５１号公報 特開平５−１９３９３９号公報 特開平６−１９１８４６号公報 特開２００１−２６１３３６号公報 特開昭６２−２１７５１号公報 特開平９−２２１３２２号公報 特開２０００−２８１３３７号公報 特開２００１−１７２０１８号公報 特開２００２−６８７４４号公報 特開平１１−１１９４６号公報 特公平１−５５２０１号公報 特公平５−７７６０１号公報 特許第３２５３３３８号公報 特許第３２５３３３９号公報 特許第３２２９３５３号公報 特許第３２２５０７３号公報 特開昭６０−７１０３７号公報 特開２００２−２５３９５３号公報 特開２００２−２５３９５４号公報 特開２００２−２６３４７４号公報 However, because such dry synthesis is not suitable for ITO powder, dry synthesis of ITO powder is not industrially performed at present.
JP-A-62-221751 JP-A-5-193939 Japanese Patent Laid-Open No. 6-191846 JP 2001-261336 A JP-A-62-221751 JP-A-9-221322 JP 2000-281337 A JP 2001-172018 A JP 2002-68744 A Japanese Patent Laid-Open No. 11-11946 Japanese Patent Publication No. 1-55201 Japanese Patent Publication No. 5-77601 Japanese Patent No. 3253338 Japanese Patent No. 3253339 Japanese Patent No. 3229353 Japanese Patent No. 3225073 JP 60-71037 A JP 2002-253953 A Japanese Patent Application Laid-Open No. 2002-253954 JP 2002-263474 A

本発明はこのような事情に鑑み、酸化物微粒子等の微粒子をより簡便な装置で且つ低コストで製造でき、ＩＴＯ粉末の製造に好適な微粒子の製造方法及び製造装置を提供することを課題とする。  In view of such circumstances, the present invention has an object to provide a production method and production apparatus for fine particles suitable for production of ITO powder, which can produce fine particles such as oxide fine particles with a simpler apparatus and at lower cost. To do.

前記課題を解決する本発明の第１の態様は、微粒子を製造する方法において、原料を液流、液滴又は粉末として、熱源中に供給し、生成物を霧状の液状流体により微粒子として捕獲し、気液分離により前記微粒子をスラリーとして回収することを特徴とする微粒子の製造方法にある。  According to a first aspect of the present invention for solving the above-described problem, in the method for producing fine particles, the raw material is supplied as a liquid stream, droplets or powder into a heat source, and the product is captured as fine particles by a mist-like liquid fluid. In addition, the present invention provides a method for producing fine particles, wherein the fine particles are recovered as a slurry by gas-liquid separation.

かかる第１の態様では、原料が熱源中に供給されて得られた生成物は、霧状の液状流体により微粒子として捕獲されて気液分離により効率的に回収される。  In the first aspect, the product obtained by supplying the raw material into the heat source is captured as fine particles by the atomized liquid fluid and efficiently recovered by gas-liquid separation.

本発明の第２の態様は、第１の態様において、原料の溶湯から液流又は液滴を形成して前記熱源中に供給することを特徴とする微粒子の製造方法にある。  According to a second aspect of the present invention, there is provided a method for producing fine particles according to the first aspect, wherein a liquid flow or droplets are formed from a molten raw material and supplied into the heat source.

かかる第２の態様では、原料としての金属若しくは合金などの溶湯からの液流又は液滴は熱源中で場合によっては酸化物となり、霧状の液状流体により微粒子として捕獲される。  In the second aspect, a liquid flow or droplets from a molten metal such as a metal or an alloy as a raw material becomes an oxide in some cases in a heat source, and is captured as fine particles by a mist-like liquid fluid.

本発明の第３の態様は、第１の態様において、原料のアトマイズ粉末を形成して前記熱源中に供給することを特徴とする微粒子の製造方法にある。  According to a third aspect of the present invention, there is provided a method for producing fine particles according to the first aspect, wherein a raw material atomized powder is formed and supplied into the heat source.

かかる第３の態様では、原料の金属若しくは合金などはアトマイズ粉末として熱源中に供給され、微粒子とされる。  In the third aspect, the raw material metal or alloy is supplied as atomized powder into the heat source to form fine particles.

本発明の第４の態様は、第１〜３の何れかの態様において、前記気液分離をサイクロンを用いて行うことを特徴とする微粒子の製造方法にある。  According to a fourth aspect of the present invention, in any one of the first to third aspects, the gas-liquid separation is performed using a cyclone.

かかる第４の態様では、サイクロンにより気液分離されて微粒子が液状流体のスラリーとして回収される。  In the fourth aspect, gas-liquid separation is performed by the cyclone, and the fine particles are recovered as a liquid fluid slurry.

本発明の第５の態様は、第１〜４の何れかの態様において、前記熱源が、アセチレン炎又はＤＣプラズマ炎であることを特徴とする微粒子の製造方法にある。  According to a fifth aspect of the present invention, in any one of the first to fourth aspects, the heat source is an acetylene flame or a DC plasma flame.

かかる第５の態様では、原料は、アセチレン炎又はＤＣプラズマ炎により微粒子とされる。  In the fifth aspect, the raw material is made into fine particles by an acetylene flame or a DC plasma flame.

本発明の第６の態様は、第１〜５の何れかの態様において、前記液状流体が、水であることを特徴とする微粒子の製造方法にある。  According to a sixth aspect of the present invention, there is provided the method for producing fine particles according to any one of the first to fifth aspects, wherein the liquid fluid is water.

かかる第６の態様では、生成物は水により捕獲され、スラリーとして回収される。  In such a sixth aspect, the product is captured by water and recovered as a slurry.

本発明の第７の態様は、第１〜６の何れかの態様において、前記原料が、金属、合金、酸化物、窒化物及び酸窒化物から選択される少なくとも一種であることを特徴とする微粒子の製造方法にある。  According to a seventh aspect of the present invention, in any one of the first to sixth aspects, the raw material is at least one selected from metals, alloys, oxides, nitrides, and oxynitrides. It exists in the manufacturing method of microparticles.

かかる第７の態様では、金属、合金、酸化物、窒化物及び酸窒化物などの原料は、微粒子とされる。  In the seventh aspect, raw materials such as metals, alloys, oxides, nitrides, and oxynitrides are fine particles.

本発明の第８の態様は、第１〜７の何れかの態様において、前記熱源が、酸化雰囲気又は窒化雰囲気の何れかであり、酸化物、窒化物及び酸窒化物の何れかの微粒子を得ることを特徴とする微粒子の製造方法にある。  According to an eighth aspect of the present invention, in any one of the first to seventh aspects, the heat source is either an oxidizing atmosphere or a nitriding atmosphere, and fine particles of any of oxide, nitride, and oxynitride are used. It is in the manufacturing method of microparticles | fine-particles characterized by obtaining.

かかる第８の態様では、原料は、酸化雰囲気又は窒化雰囲気下の熱源中で、酸化物、窒化物又は酸窒化物の微粒子とされる。  In the eighth aspect, the raw material is fine particles of oxide, nitride or oxynitride in a heat source in an oxidizing atmosphere or a nitriding atmosphere.

本発明の第９の態様は、第１〜７の何れかの態様において、前記原料が、Ｉｎ−Ｓｎ合金又はＩＴＯ粉末であり、酸化インジウム−酸化錫粉末を製造することを特徴とする微粒子の製造方法にある。  A ninth aspect of the present invention is the fine particle according to any one of the first to seventh aspects, wherein the raw material is an In—Sn alloy or ITO powder, and an indium oxide-tin oxide powder is produced. In the manufacturing method.

かかる第９の態様では、Ｉｎ−Ｓｎ合金又はＩＴＯ粉末からＩＯ粉末がスラリーとして製造される。  In the ninth aspect, IO powder is produced as a slurry from In—Sn alloy or ITO powder.

本発明の第１０の態様は、第９の態様において、錫含有量がＳｎＯ２換算で２．３〜４５質量％である酸化インジウム−酸化錫粉末を製造することを特徴とする微粒子の製造方法にある。A tenth aspect of the present invention is the method for producing fine particles according to the ninth aspect, wherein an indium oxide-tin oxide powder having a tin content of 2.3 to 45% by mass in terms of SnO 2 is produced. It is in.

かかる第１０の態様では、所定量の酸化錫によりＩＴＯの導電性が保持される。  In the tenth aspect, the conductivity of ITO is maintained by a predetermined amount of tin oxide.

本発明の第１１の態様は、第１〜１０の何れかの態様において、前記生成物の前記液状流体により捕獲する際の最大速度が、１５０ｍ／ｓｅｃ以下であることを特徴とする微粒子の製造方法にある。  The eleventh aspect of the present invention is the production of fine particles according to any one of the first to tenth aspects, wherein a maximum speed when the product is captured by the liquid fluid is 150 m / sec or less. Is in the way.

かかる第１１の態様では、比較的低速の流速で微粒子を製造することができる。  In the eleventh aspect, fine particles can be produced at a relatively low flow rate.

本発明の第１２の態様は、熱源中に原料を液流、液滴又は粉末として供給することにより得られる生成物を気体流体と共に導入する導入口と、導入された生成物に対して霧状の液状流体を噴射する流体噴射手段と、液状流体で捕獲された微粒子を気液分離して前記微粒子のスラリーを得る気液分離手段と、液状流体で捕獲できなかった微粒子を含む雰囲気流体の一部を流体滴噴射位置まで戻して循環させる循環手段とを具備することを特徴とする微粒子の製造装置にある。  According to a twelfth aspect of the present invention, there is provided an inlet for introducing a product obtained by supplying a raw material as a liquid stream, droplets or powder into a heat source together with a gas fluid, A fluid ejecting means for ejecting the liquid fluid; a gas-liquid separating means for obtaining a slurry of the fine particles by gas-liquid separation of the fine particles captured by the liquid fluid; and an atmosphere fluid containing the fine particles that could not be captured by the liquid fluid. And a circulating means for circulating the part back to the fluid droplet ejection position.

かかる第１２の態様では、原料が熱源中に供給されて得られた生成物は、霧状の液状流体により微粒子として捕獲されて気液分離され、雰囲気流体の少なくとも一部は循環手段により循環されて再度気液分離されることにより効率的に回収される。  In the twelfth aspect, the product obtained by supplying the raw material into the heat source is captured as fine particles by the atomized liquid fluid and separated into gas and liquid, and at least a part of the atmospheric fluid is circulated by the circulation means. Then, it is efficiently recovered by gas-liquid separation again.

本発明の第１３の態様は、第１２の態様において、前記気液分離手段の下流側にさらに、液状流体で捕獲できなかった微粒子を含む雰囲気流体の一部を導入すると共に霧状の液状流体を噴射し気液分離して前記微粒子のスラリーを得る第２の気液分離手段を具備することを特徴とする微粒子の製造装置にある。  In a thirteenth aspect of the present invention, in the twelfth aspect, a part of the atmospheric fluid containing fine particles that could not be captured by the liquid fluid is further introduced to the downstream side of the gas-liquid separation means, and the atomized liquid fluid And a second gas-liquid separation means for obtaining a slurry of the fine particles by gas-liquid separation.

かかる第１３の態様では、第２の気液分離手段により、回収できなかった微粒子が効率的に回収される。  In the thirteenth aspect, the second gas-liquid separation means efficiently recovers the fine particles that could not be recovered.

本発明の第１４の態様は、第１３の態様において、前記気液分離手段の下流側にさらに、液状流体で捕獲できなかった微粒子を含む雰囲気流体の一部を前記第２の気液分離手段の導入部まで戻す第２の循環手段を具備することを特徴とする微粒子の製造装置にある。  According to a fourteenth aspect of the present invention, in the thirteenth aspect, a part of the atmospheric fluid containing fine particles that could not be captured by the liquid fluid is further disposed downstream of the gas-liquid separation means. In the fine particle production apparatus, the second circulation means for returning to the introduction portion is provided.

かかる第１４の態様では、第２の気液分離手段でスラリーとして回収できなかった雰囲気ガスが再度気液分離され、微粒子が効率的に回収される。  In the fourteenth aspect, the atmospheric gas that could not be recovered as a slurry by the second gas-liquid separation means is again gas-liquid separated, and the fine particles are efficiently recovered.

本発明の第１５の態様は、第１２〜１４の何れかの態様において、前記気液分離手段がサイクロンであることを特徴とする微粒子の製造装置にある。  According to a fifteenth aspect of the present invention, in any one of the twelfth to fourteenth aspects, the gas-liquid separation unit is a cyclone.

かかる第１５の態様では、サイクロンにより気液分離を連続的且つ効率的に行うことができる。  In the fifteenth aspect, gas-liquid separation can be performed continuously and efficiently by the cyclone.

本発明の第１６の態様は、第１２〜１５の何れかの態様において、前記流体噴射手段が噴射した液状流体に微粒子が捕獲される際の最大速度が１５０ｍ／ｓｅｃ以下であることを特徴とする微粒子の製造装置にある。  A sixteenth aspect of the present invention is characterized in that, in any one of the twelfth to fifteenth aspects, a maximum speed when the fine particles are captured in the liquid fluid ejected by the fluid ejecting means is 150 m / sec or less. It is in the production apparatus of fine particles.

かかる第１６の態様では、比較的低速の流速で微粒子を製造することができる。  In the sixteenth aspect, fine particles can be produced at a relatively low flow rate.

以上説明したように、本発明によれば、熱源中に原料金属若しくは合金を液流、液滴又は粉末として導入することにより得られた生成物を霧状の液状流体で捕獲することにより、微粒子を効率よく簡便に製造することができるという効果を奏する。  As described above, according to the present invention, fine particles can be obtained by capturing a product obtained by introducing a raw metal or alloy into a heat source as a liquid stream, droplet or powder with a mist-like liquid fluid. Can be produced efficiently and simply.

［図１］本発明の一実施形態に係る微粒子の製造装置の概略構成図である。本発明の実施例１のＩＴＯ粉末のＸ線回折の結果を示す図である。 本発明の実施例２のＩＴＯ粉末のＸ線回折の結果を示す図である。 本発明の比較例１のＩＴＯ粉末のＸ線回折の結果を示す図である。 本発明の比較例２のＩＴＯ粉末のＸ線回折の結果を示す図である。 本発明の比較例３のＩＴＯ粉末のＸ線回折の結果を示す図である。 本発明の実施例３のＩＴＯ粉末のＸ線回折の結果を示す図である。 本発明の比較例４のＩＴＯ粉末のＸ線回折の結果を示す図である。 FIG. 1 is a schematic configuration diagram of an apparatus for producing fine particles according to an embodiment of the present invention. It is a figure which shows the result of the X-ray diffraction of the ITO powder of Example 1 of this invention. It is a figure which shows the result of the X-ray diffraction of the ITO powder of Example 2 of this invention. It is a figure which shows the result of the X-ray diffraction of the ITO powder of the comparative example 1 of this invention. It is a figure which shows the result of the X-ray diffraction of the ITO powder of the comparative example 2 of this invention. It is a figure which shows the result of the X-ray diffraction of the ITO powder of the comparative example 3 of this invention. It is a figure which shows the result of the X-ray diffraction of the ITO powder of Example 3 of this invention. It is a figure which shows the result of the X-ray diffraction of the ITO powder of the comparative example 4 of this invention.

本発明の微粒子を製造する方法では、原料を、液流、液滴又は粉末として、熱源中に供給する。  In the method for producing fine particles of the present invention, the raw material is supplied into the heat source as a liquid stream, droplets or powder.

ここで、原料は、例えば、金属若しくは合金であり、金属若しくは合金としては、例えば、Ｍｇ、Ａｌ、Ｚｒ、Ｆｅ、Ｓｉ、Ｉｎ、Ｓｎなどの金属、又はこれらの合金である。また、原料として、上述した金属若しくは合金などの酸化物、窒化物及び酸窒化物を用いることができる。なお、ここで、酸化物は、複合酸化物を含むものであり、窒化物は複合窒化物を含むものである。  Here, the raw material is, for example, a metal or an alloy, and the metal or alloy is, for example, a metal such as Mg, Al, Zr, Fe, Si, In, or Sn, or an alloy thereof. In addition, the above-described oxides, nitrides, and oxynitrides such as metals or alloys can be used as raw materials. Here, the oxide includes a composite oxide, and the nitride includes a composite nitride.

かかる原料は、溶融した状態の液流又は液滴として供給してもよいし、粉末状態として供給してもよい。すなわち、溶湯溜などから連続的に液流として若しくは液滴として滴下してもよく、又はアトマイズ粉末を形成してこれを供給するようにしてもよい。  Such a raw material may be supplied as a molten liquid stream or droplet, or may be supplied as a powder. That is, it may be dripped continuously as a liquid flow or as a droplet from a molten metal reservoir or the like, or atomized powder may be formed and supplied.

例えば、Ｉｎ−Ｓｎ合金を原料とすると、ＩＴＯ粉末を得ることができる。また、ＩＴＯ粉末を原料としても、性状の異なるＩＴＯ粉末を得ることができる。  For example, when an In—Sn alloy is used as a raw material, ITO powder can be obtained. Moreover, even if ITO powder is used as a raw material, ITO powder having different properties can be obtained.

また、熱源としては、酸化雰囲気又は窒化雰囲気可能な熱源を挙げることができ、例えば、アセチレン炎、ＤＣプラズマ炎などを挙げることができる。熱源の温度は、金属若しくは合金又は酸化物や窒化物あるいは酸窒化物を溶融し、十分に酸化若しくは窒化できる程度であればよく、特に制限されない。なお、アセチレン炎の場合には、数千℃以上、ＤＣプラズマ炎の場合には、数万℃以上であるといわれている。  Examples of the heat source include a heat source capable of oxidizing atmosphere or nitriding atmosphere, and examples thereof include acetylene flame and DC plasma flame. The temperature of the heat source is not particularly limited as long as it can be sufficiently oxidized or nitrided by melting a metal, an alloy, an oxide, a nitride, or an oxynitride. In the case of acetylene flame, it is said that the temperature is several thousand ° C. or higher, and in the case of DC plasma flame, it is said to be several tens of thousands ° C. or higher.

このようなアセチレン炎又はＤＣプラズマ炎に原料を液流、液滴又は粉末として供給すると、生成物は、そのまま又は酸化物や窒化物あるいは酸窒化物として気体流と共に得られる。原料をそのまま金属若しくは合金の生成物として得るか、又は金属若しくは合金の酸化物や窒化物あるいは酸窒化物とするかは熱源の火炎の状態によって決定され、酸化雰囲気にすると、金属若しくは合金の酸化物あるいは酸窒化物の生成物が得られ、窒化雰囲気とすると、金属若しくは合金の窒化物や酸窒化物が得られる。また、原料として、酸化物や窒化物あるいは酸窒化物を用いても、性状の異なる酸化物や窒化物あるいは酸窒化物を得ることができる。  When the raw material is supplied to such an acetylene flame or DC plasma flame as a liquid stream, droplets or powder, the product is obtained as it is or as an oxide, nitride or oxynitride together with the gas stream. Whether the raw material is directly obtained as a metal or alloy product, or whether it is an oxide or nitride or oxynitride of a metal or alloy is determined by the state of the flame of the heat source. When a nitriding atmosphere is obtained, a metal or alloy nitride or oxynitride is obtained. Further, even when oxides, nitrides, or oxynitrides are used as raw materials, oxides, nitrides, or oxynitrides having different properties can be obtained.

本発明では、得られた生成物を霧状の液状流体により捕獲する。すなわち、アセチレン炎やＤＣプラズマ炎の噴流と共に流れる生成物に霧状の液状流体、好ましくは霧状の水を噴霧する。これにより、生成物は急冷されて微粒子となり、噴霧された液状流体のスラリーとなる。  In the present invention, the obtained product is captured by a mist liquid fluid. That is, a mist-like liquid fluid, preferably mist-like water, is sprayed on the product flowing along with the jet of acetylene flame or DC plasma flame. As a result, the product is rapidly cooled to form fine particles, and becomes a sprayed liquid fluid slurry.

ここで、霧状の液状流体の供給は、得られる生成物を捕獲して冷却できるように行えばよく、特に限定されない。例えば、水を用いる場合には、常温の水、好ましくは、常温の純水を用いればよいが、冷却水を用いてもよい。  Here, the supply of the mist-like liquid fluid may be performed so that the obtained product can be captured and cooled, and is not particularly limited. For example, when water is used, room temperature water, preferably pure water at room temperature, may be used, but cooling water may be used.

生成物を微粒子として捕獲する場合、捕獲する際の最大速度は、例えば、１５０ｍ／ｓｅｃ以下、好ましくは１００ｍ／ｓｅｃ以下程度である。  When capturing the product as fine particles, the maximum speed for capturing is, for example, 150 m / sec or less, and preferably about 100 m / sec or less.

本発明では、噴霧された液状流体に捕獲された微粒子を含む液状流体を気液分離し、微粒子をスラリーとして回収する。ここで、スラリーの回収方法は特に限定されないが、好ましくは、サイクロンを用いて行うことができる。  In the present invention, a liquid fluid containing fine particles trapped in the sprayed liquid fluid is gas-liquid separated, and the fine particles are recovered as a slurry. Here, the method for recovering the slurry is not particularly limited, but it can be preferably performed using a cyclone.

本発明方法を用いると、原料としてＩｎ−Ｓｎ合金若しくはＩＴＯ粉末を用いることにより、酸化インジウム−酸化錫（ＩＴＯ）粉末を製造することができる。このように製造されたＩＴＯ粉末は、このようにＩｎ２Ｏ３中のＳｎＯ２固溶量が高水準なので、焼結性が高く、比較的容易に高密度の焼結体が得られ、この結果、ライフの長いターゲットを得ることができる。なお、各種製造方法により製造されたＩＴＯ粉末、又は焼結されたＩＴＯ焼結体を粉砕したＩＴＯ粉末を原料とした場合、原料とは異なる性状で、Ｉｎ２Ｏ３中のＳｎＯ２固溶量が高水準なＩＴＯ粉末を得ることができる。When the method of the present invention is used, an indium oxide-tin oxide (ITO) powder can be produced by using an In—Sn alloy or ITO powder as a raw material. Since the ITO powder thus produced has a high level of SnO 2 solid solution in In 2 O 3 as described above, the sinterability is high, and a high-density sintered body can be obtained relatively easily. As a result, a target with a long life can be obtained. In addition, when ITO powder manufactured by various manufacturing methods or ITO powder obtained by pulverizing a sintered ITO sintered body is used as a raw material, the amount of SnO 2 solid solution in In 2 O 3 is different from that of the raw material. Can obtain a high level of ITO powder.

なお、かかるＩＴＯ粉末は、ＩＴＯスパッタリングターゲットの材料として用いることができる。かかるＩＴＯスパッタリングターゲットの材料としては、錫含有量がＳｎＯ２換算で２．３〜４５質量％であるのが好ましい。Such ITO powder can be used as a material for an ITO sputtering target. As a material for the ITO sputtering target, it is preferable that the tin content is 2.3 to 45% by mass in terms of SnO 2 .

以下、本発明方法を実施する微粒子の製造装置の一例を図１を参照しながら説明する。  Hereinafter, an example of a fine particle production apparatus for carrying out the method of the present invention will be described with reference to FIG.

この装置は、酸化雰囲気又は窒化雰囲気可能な熱源であるアセチレン炎又はＤＣプラズマ炎からなる火炎１中に供給された金属若しくは合金などの原料２を液流、液滴又は粉末として供給することにより得られる生成物３を気体流体と共に導入する導入口１０と、導入された微粒子に対して霧状の液状流体を噴射する流体噴射手段２０と、液状流体で捕獲された微粒子を気液分離して前記微粒子のスラリーを得る気液分離手段であるサイクロン３０と、液状流体で捕獲できなかった微粒子を含む雰囲気流体の一部を流体滴噴射位置まで戻して循環させる循環手段４０とを具備する。  This apparatus is obtained by supplying a raw material 2 such as a metal or an alloy supplied as a liquid flow, a droplet or a powder into a flame 1 composed of an acetylene flame or a DC plasma flame which is a heat source capable of oxidizing atmosphere or nitriding atmosphere. The product inlet 3 for introducing the product 3 together with the gas fluid, the fluid ejecting means 20 for ejecting a mist-like liquid fluid to the introduced fine particles, and the fine particles captured by the liquid fluid are separated into gas and liquid. A cyclone 30 as gas-liquid separation means for obtaining a slurry of fine particles, and a circulation means 40 for returning a part of the atmospheric fluid containing fine particles that could not be captured by the liquid fluid to a fluid droplet ejecting position and circulating them.

ここで、導入口１０は、生成物を含む気体流を導入できるものであれば特に限定されないが、気体流を吸引するようにしてもよい。  Here, the introduction port 10 is not particularly limited as long as it can introduce a gas flow containing a product, but it may suck the gas flow.

流体噴射手段２０は、導入口１０が設けられた導入管１１の下流側に設けられて流体、例えば、水を噴射する複数の噴射ノズル２１と、噴射ノズル２１へ流体を導入するためにポンプ２２及び流体を湛える流体タンク２３とを有する。噴射ノズル２１からの流体の噴射の方向は特に限定されないが、導入口１０から導入される気体流の流れ方向に向かって合流する方向に噴射するのがよい。導入口１０から導入された気体流に含有される生成物３は、噴霧された流体、例えば、水により冷却され、微粒子として捕獲される。なお、導入管１１の噴射ノズル２１の下流側には、流路を絞ったベンチュリー部１２を設けて気液混合物の流速の低下を防止しているが、ベンチュリー部１２は必ずしも設ける必要はない。また、噴射ノズル２１及びポンプ２２は、必ずしも設ける必要はなく、気体流の流れによる吸引力により液体を吸引して噴射するようにしてもよい。  The fluid ejecting means 20 is provided on the downstream side of the introduction pipe 11 provided with the introduction port 10, a plurality of ejection nozzles 21 for ejecting fluid, for example, water, and a pump 22 for introducing fluid into the ejection nozzle 21. And a fluid tank 23 for holding fluid. The direction in which the fluid is ejected from the ejection nozzle 21 is not particularly limited. The product 3 contained in the gas flow introduced from the introduction port 10 is cooled by a sprayed fluid, for example, water, and captured as fine particles. In addition, although the venturi part 12 which restrict | squeezed the flow path is provided in the downstream of the injection nozzle 21 of the inlet pipe 11, the fall of the flow velocity of a gas-liquid mixture is prevented, The venturi part 12 does not necessarily need to be provided. Further, the injection nozzle 21 and the pump 22 are not necessarily provided, and the liquid may be sucked and jetted by the suction force generated by the gas flow.

導入口１０が設けられた導入管１１は、気液分離手段であるサイクロン３０の導入口３１に連通している。サイクロン３０の導入口３１から導入された気液混合物は、サイクロン本体３２の内壁に沿って周回する渦流３３となって気液分離され、液体成分、すなわち、微粒子を含むスラリーが下部に落下し、気体成分は排気口３４から排出されるようになっている。  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 means. The gas-liquid mixture introduced from the introduction port 31 of the cyclone 30 is separated into a gas-liquid mixture that circulates along the inner wall of the cyclone main body 32, and the liquid component, that is, the slurry containing fine particles falls to the lower part. The gas component is discharged from the exhaust port 34.

本実施形態では、排気口３４に循環手段４０が設けられている。すなわち、排気口３４には、導入管１１の導入口１０近傍に連通する循環パイプ４１が設けられ、循環パイプ４１の途中にブロア４２が介装されており、これらが循環手段４０を構成している。この循環手段４０により、捕獲しきれなかった粉末を噴射ノズル２１の上流側に戻し、捕獲効率を向上させている。  In the present embodiment, the circulation means 40 is provided at the exhaust port 34. That is, the exhaust port 34 is provided with a circulation pipe 41 communicating with the vicinity of the introduction port 10 of the introduction pipe 11, and a blower 42 is interposed in the middle of the circulation pipe 41, and these constitute the circulation means 40. Yes. By this circulation means 40, the powder that could not be captured is returned to the upstream side of the injection nozzle 21 to improve the capture efficiency.

また、サイクロン３０で気液分離された液体成分は水排出口３６から排出され、流体タンク２３に湛えられる。なお、この流体タンク２３に湛えられたスラリーの上澄みの水が循環手段４０により循環されているので、徐々に微粒子成分の濃度の濃いスラリーが得られる。  Further, the liquid component separated by gas and liquid in the cyclone 30 is discharged from the water discharge port 36 and is stored in the fluid tank 23. Since the water in the supernatant of the slurry stored in the fluid tank 23 is circulated by the circulation means 40, a slurry having a concentration of fine particle components is gradually obtained.

サイクロン３０からの排気の大部分は排気口３４から循環パイプ４１に循環されるが、排気の一部、例えば、十分の一程度は第２の排気口３５から排気されるようになっている。  Most of the exhaust from the cyclone 30 is circulated from the exhaust port 34 to the circulation pipe 41, but a part of the exhaust, for example, about one tenth, is exhausted from the second exhaust port 35.

本実施形態では、第２の排気口３５には、第２の気液分離手段である第２のサイクロン５０が排気パイプ４３を介して接続されている。第２のサイクロン５０は、基本的にはサイクロン３０と同一の構造を有して気液分離作用を有する。すなわち、排気パイプ４３が接続される導入口５１から導入された気液混合物は、サイクロン本体５２の内壁に沿って周回する渦流５３となって気液分離され、液体成分、すなわち、微粒子を含むスラリーは、下部に落下し、水排出口５４から排出され、流体タンク６１に溜まるようになっている。さらに詳言すると、排気パイプ４３の途中には流路を絞ったベンチュリー部４４が設けられており、このベンチュリー部４４と、流体タンク６１とを連通する水循環パイプ６２が設けられている。これにより、ベンチュリー部４４の高速の気体の流れにより、流体タンク６１中の水が吸引されてベンチュリー部４４内に噴射され、気体中に残存する微粒子を液体中に捕獲するようにしている。一方、排気口５５には排気パイプ７１が連結され、排気パイプ７１には第２のブロア７２が設けられ、当該第２のブロア７２を介して排気口５５からの気体が排気されるようになっている。なお、水タンク６１の水を排気パイプ４３内に噴霧するには、上述したサイクロン３０のように、ポンプと噴霧ノズルを用いて行ってもよい。また、流体タンク６１には、上述したように、フィルターを設けてもよいし、中和して微粒子を分離する沈降分離槽を設けてもよい。さらに、排気口５５からの排気の一部を排気パイプ４３のベンチュリー部４４の上流側に循環させるようにして、さらに捕獲効率を高めてもよい。  In the present embodiment, the second exhaust port 35 is connected to the second cyclone 50 as the second gas-liquid separation means via the exhaust pipe 43. The second cyclone 50 basically has 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 a gas-liquid mixture that circulates along the inner wall of the cyclone main body 52 and is separated into a liquid component, that is, a slurry containing fine particles. Falls to the lower part, is discharged from the water discharge port 54, and accumulates in the fluid tank 61. More specifically, a venturi section 44 with a narrowed flow path is provided in the middle of the exhaust pipe 43, and a water circulation pipe 62 that connects the venturi section 44 and the fluid tank 61 is provided. Thereby, the water in the fluid tank 61 is sucked by the high-speed gas flow of the venturi section 44 and is injected into the venturi section 44, so that the fine particles remaining in the gas are captured in the liquid. On the other hand, an exhaust pipe 71 is connected to the exhaust port 55, and a second blower 72 is provided in the exhaust pipe 71, and the gas from the exhaust port 55 is exhausted through the second blower 72. ing. In addition, in order to spray the water of the water tank 61 in the exhaust pipe 43, you may carry out using a pump and a spray nozzle like the cyclone 30 mentioned above. Further, as described above, the fluid tank 61 may be provided with a filter, or may be provided with a sedimentation separation tank that neutralizes and separates the fine particles. Furthermore, capture efficiency may be further increased by circulating a part of the exhaust from the exhaust port 55 to the upstream side of the venturi portion 44 of the exhaust pipe 43.

なお、サイクロン３０のみで微粒子の捕獲効率が十分な場合には、第２のサイクロン５０は、必ずしも設ける必要はなく、又は、さらに捕獲効率を高めたい場合には、さらに複数のサイクロンを連結してもよい。  Note that the second cyclone 50 is not necessarily provided when the cyclone 30 alone has sufficient capture efficiency of the fine particles, or a plurality of cyclones are further connected to further increase the capture efficiency. Also good.

以上説明した実施形態の装置を用いて微粒子を製造した例を以下に示す。  An example of producing fine particles using the apparatus of the embodiment described above will be shown below.

［実施例１］
Ｉｎ−Ｓｎ合金（Ｓｎ９．６ｗｔ％）のアトマイズ粉末（平均粒径４５μｍ）を、アセチレン炎に導入してＩＴＯ（Ｉｎ２Ｏ３：ＳｎＯ２＝９０：１０ｗｔ％）粉末を乾式合成し、これをバグフィルターにより乾式回収し、実施例１のＩＴＯ粉末とした。[Example 1]
Atomized powder (average particle size 45 μm) of In—Sn alloy (Sn 9.6 wt%) was introduced into acetylene flame to dry-synthesize ITO (In 2 O 3 : SnO 2 = 90: 10 wt%) powder. The powder was collected by dry using a bag filter and used as the ITO powder of Example 1.

［実施例２］
実施例１と同様にしてアセチレン炎より乾式合成したＩＴＯ粉末を、スプレー水により式回収し、これを実施例２のＩＴＯ粉末とした。[Example 2]
The ITO powder dry-synthesized from the acetylene flame in the same manner as in Example 1 was recovered by spray water and used as the ITO powder of Example 2.

（比較例１）
湿式合成された酸化インジウム粉末を１０００℃で仮焼した酸化インジウム粉末９０質量％と、同様に湿式合成された酸化錫を１０００℃で仮焼した酸化錫粉末１０質量％とを乳鉢で混合したものを比較例１とし、標準品１とした。(Comparative Example 1)
90% by mass of indium oxide powder obtained by calcining wet-synthesized indium oxide powder at 1000 ° C. and 10% by mass of tin oxide powder obtained by calcining wet-synthesized tin oxide at 1000 ° C. in a mortar Was Comparative Example 1 and was designated as Standard Product 1.

（比較例２）
共沈法により湿式合成されたＩＴＯ粉末を比較例２のＩＴＯ粉末とした。(Comparative Example 2)
The ITO powder wet-synthesized by the coprecipitation method was used as the ITO powder of Comparative Example 2.

共沈法による湿式合成の手順は以下の通りである。すなわち、まず、Ｉｎ（４Ｎ）２０ｇを硝酸（試薬特級：濃度６０〜６１％）１３３ｃｃに常温にて溶解し（ｐＨ＝−１．５）、一方、Ｓｎ（４Ｎ）２．１２ｇを塩酸（試薬特級：濃度３５〜３６％）１００ｃｃに常温にて溶解し（ｐＨ＝−１．９）、両者を混合して混酸溶液とした。このとき、析出物はなく、ｐＨは−１．５であった。次いで、この混酸に２５％アンモニア水（試薬特級）を混合して中和してｐＨ６．５としたところ、白い沈殿物を析出した。数時間後、上水を捨てて純水２リットル（Ｌ）にて３回洗浄した後、８０℃にて乾燥させた後、６００℃で３時間培焼、脱水反応させ、湿式合成ＩＴＯ粉末を得た。  The procedure of wet synthesis by the coprecipitation method is as follows. That is, first, 20 g of In (4N) was dissolved in 133 cc of nitric acid (special grade reagent: concentration 60 to 61%) at room temperature (pH = -1.5), while 2.12 g of Sn (4N) was dissolved in hydrochloric acid (reagent). (Special grade: concentration 35 to 36%) dissolved in 100 cc at room temperature (pH = -1.9), and both were mixed to obtain a mixed acid solution. At this time, there was no deposit and pH was -1.5. Subsequently, 25% aqueous ammonia (special grade reagent) was mixed with this mixed acid and neutralized to pH 6.5, whereby a white precipitate was deposited. Several hours later, the water is discarded, washed 3 times with 2 liters (L) of pure water, dried at 80 ° C., cultivated at 600 ° C. for 3 hours, and dehydrated to obtain a wet synthetic ITO powder. Obtained.

（比較例３）
湿式合成された酸化インジウム粉末と酸化錫粉末との混合物（酸化錫１０ｗｔ％）の粉末を用いて１５５０℃以上で焼結した焼結体を粉砕したものを比較例３のＩＴＯ粉末とした。(Comparative Example 3)
An ITO powder of Comparative Example 3 was obtained by pulverizing a sintered body sintered at 1550 ° C. or higher using a wet-synthesized powder of a mixture of indium oxide powder and tin oxide powder (tin oxide 10 wt%).

（試験例１）
各実施例１，２及び各比較例１〜３のＩＴＯ粉末について、ＳｎＯ２固溶量を求めた。手順は以下の通りである。なお、試験の実施に先駆けて、実施例１，２及び比較例２，３のＩＴＯ粉末については、１０００℃×３時間、大気中で仮焼して、微小粒子として析出しているＳｎＯ２を成長させてＳｎＯ２として検出され易いようにした。
１．まず、誘導結合高周波プラズマ分光分析（ＩＣＰ分光分析）した。この結果より、Ｉｎ、Ｓｎ以外は全て酸素Ｏであるとし、そのＯの量は欠損している可能性があると仮定して、ＩｎとＳｎとの比を求め、このＩｎ及びＳｎの全てがＩｎ２Ｏ３、ＳｎＯ２になったとしたときの重量比を算出した。
２．各実施例１，２及び各比較例１〜３のＩＴＯ粉末について、粉末Ｘ線回折（ＸＲＤ：（株）マックサイエンス社製、ＭＸＰ１８ＩＩ）による分析を行い、ＳｎＯ２析出量を求めた。すなわち、回折結果から、間化合物（Ｉｎ４Ｓｎ３Ｏ１２）の有無を確認し、間化合物が検出されない場合には、比較例１の標準品１として各試料のＩｎ２Ｏ３（２２２）積分回折強度及びＳｎＯ２（１１０）積分回折強度の比からＳｎＯ２の析出量（質量％）を求めた。すなわち、ＳｎＯ２の析出量（質量％）は、Ｘ線回折の積分回折強度比から求められるＳｎＯ２の含有量であり、Ｉｎ２Ｏ３に固溶していないＳｎＯ２が１０００℃程度の仮焼により成長してＸ線回折のＳｎＯ２（１１０）のピークとなると仮定している。Ｘ線回折の結果を図２〜図６に示す。
３．１及び２の結果から、ＩＣＰ分析で検出されたが、Ｘ線回折ではＳｎＯ２（１１０）とは検出されないＳｎＯ２を、Ｉｎ２Ｏ３中のＳｎＯ２固溶量とした。(Test Example 1)
For the ITO powders of Examples 1 and 2 and Comparative Examples 1 to 3, the SnO 2 solid solution amount was determined. The procedure is as follows. Prior to the test, the ITO powders of Examples 1 and 2 and Comparative Examples 2 and 3 were calcined in the atmosphere at 1000 ° C. for 3 hours to precipitate SnO 2 precipitated as fine particles. and as easily detected as SnO 2 grown.
1. First, inductively coupled high-frequency plasma spectroscopic analysis (ICP spectroscopic analysis) was performed. From this result, it is assumed that everything except In and Sn is oxygen O, and assuming that there is a possibility that the amount of O is missing, the ratio of In and Sn is obtained. The weight ratio of In 2 O 3 and SnO 2 was calculated.
2. The ITO powders of Examples 1 and 2 and Comparative Examples 1 to 3 were analyzed by powder X-ray diffraction (XRD: manufactured by Mac Science, Inc., MXP18II), and the SnO 2 precipitation amount was determined. That is, from the diffraction results, the presence or absence of an intercalation compound (In 4 Sn 3 O 12 ) is confirmed. If no intercalation compound is detected, the In 2 O 3 (222) integral of each sample is used as the standard product 1 of Comparative Example 1. The precipitation amount (mass%) of SnO 2 was determined from the ratio of the diffraction intensity and the SnO 2 (110) integrated diffraction intensity. That is, the amount of precipitated SnO 2 (mass%) is the content of SnO 2 obtained from integrated diffraction intensity ratio of X-ray diffraction, temporary SnO 2 not dissolved in the In 2 O 3 is about 1000 ° C. It is assumed that it grows by firing and becomes a SnO 2 (110) peak of X-ray diffraction. The results of X-ray diffraction are shown in FIGS.
From 3.1 and 2 results, but was detected by ICP analysis, the X-ray diffraction of SnO 2 not detected and SnO 2 (110), and a SnO 2 solid solution amount in an In 2 O 3.

これらの結果を表１に示す。  These results are shown in Table 1.

この結果、実施例１，２のＩＴＯ粉末では、ＳｎＯ２固溶量が２．３５ｗｔ％、２．４２ｗｔ％と、湿式合成したＩＴＯ粉末である比較例２の２．２６ｗｔ％より多いことがわかった。なお、一度焼結体としたものを粉砕した比較例３のＩＴＯ粉末では間化合物が検出され、ＳｎＯ２固溶量は測定不能であった。As a result, in the ITO powders of Examples 1 and 2 , the SnO 2 solid solution amount is 2.35 wt%, 2.42 wt%, which is larger than 2.26 wt% of Comparative Example 2 which is a wet-synthesized ITO powder. It was. In addition, an intercalation compound was detected in the ITO powder of Comparative Example 3 that was pulverized from a sintered body, and the SnO 2 solid solution amount was not measurable.

Figure 2005066069
Figure 2005066069

［実施例３］
Ｉｎ−Ｓｎ合金（Ｓｎ９．６ｗｔ％）のアトマイズ粉末（平均粒径４５μｍ）を、ＤＣプラズマ炎に導入してＩＴＯ（Ｉｎ２Ｏ３：ＳｎＯ２＝９０：１０ｗｔ％）粉末を乾式合成し、これをスプレー水により湿式回収し、実施例３のＩＴＯ粉末とした。[Example 3]
An In-Sn alloy (Sn 9.6 wt%) atomized powder (average particle size 45 μm) is introduced into a DC plasma flame to dry-synthesize ITO (In 2 O 3 : SnO 2 = 90: 10 wt%) powder. Was collected by spray water and used as the ITO powder of Example 3.

（比較例４）
比較例１と同様に、湿式合成された酸化インジウム粉末を１０００℃で仮焼した酸化インジウム粉末９０質量％と、同様に湿式合成された酸化錫を１０００℃で仮焼した酸化錫粉末１０質量％とを乳鉢で混合したものを比較例４とし、標準品２とした。(Comparative Example 4)
Similarly to Comparative Example 1, 90% by mass of indium oxide powder obtained by calcining wet-synthesized indium oxide powder at 1000 ° C., and 10% by mass of tin oxide powder obtained by calcining wet-synthesized tin oxide at 1000 ° C. Was mixed in a mortar as Comparative Example 4 as Standard 2.

（試験例２）
実施例３及び各比較例４のＩＴＯ粉末について、試験例１と同様にＳｎＯ２固溶量を求めた。なお、粉末Ｘ線回折（ＸＲＤ）はスペクトリス（（株））社製のＸ’ＰｅｒｔＰＲＯ ＭＰＤを用いて分析した。これらの結果を表２に示す。また、Ｘ線回折の結果を図７及び図８に示す。(Test Example 2)
The ITO powder of Example 3 and Comparative Example 4 were determined SnO 2 solid solution amount in the same manner as in Test Example 1. The powder X-ray diffraction (XRD) was analyzed using X'Pert PRO MPD manufactured by Spectris Co., Ltd. These results are shown in Table 2. The results of X-ray diffraction are shown in FIGS.

この結果、実施例３のＩＴＯ粉末では、ＳｎＯ２固溶量が３．００ｗｔ％と、ＤＣプラズマ炎の代わりにアセチレン炎を用いた以外は同等の実施例２のＳｎＯ２固溶量より著しく大きいことがわかった。As a result, in the ITO powder of Example 3, the SnO 2 solid solution amount is 3.00 wt%, which is significantly larger than the equivalent SnO 2 solid solution amount of Example 2 except that an acetylene flame is used instead of the DC plasma flame. I understood it.

Figure 2005066069
Figure 2005066069

Claims (16)

微粒子を製造する方法において、原料を液流、液滴又は粉末として、熱源中に供給し、生成物を霧状の液状流体により微粒子として捕獲し、気液分離により前記微粒子をスラリーとして回収することを特徴とする微粒子の製造方法。In the method for producing fine particles, the raw material is supplied as a liquid stream, droplets or powder into a heat source, the product is captured as fine particles by a mist-like liquid fluid, and the fine particles are recovered as a slurry by gas-liquid separation. A method for producing fine particles characterized by the above. 請求の範囲１において、原料の溶湯から液流又は液滴を形成して前記熱源中に供給することを特徴とする微粒子の製造方法。2. The method for producing fine particles according to claim 1, wherein a liquid flow or droplets are formed from a molten raw material and supplied into the heat source. 請求の範囲１において、原料のアトマイズ粉末を形成して前記熱源中に供給することを特徴とする微粒子の製造方法。2. The method for producing fine particles according to claim 1, wherein an atomized powder of a raw material is formed and supplied into the heat source. 請求の範囲１〜３の何れかにおいて、前記気液分離をサイクロンを用いて行うことを特徴とする微粒子の製造方法。The method for producing fine particles according to any one of claims 1 to 3, wherein the gas-liquid separation is performed using a cyclone. 請求の範囲１〜４の何れかにおいて、前記熱源が、アセチレン炎又はＤＣプラズマ炎であることを特徴とする微粒子の製造方法。The method for producing fine particles according to any one of claims 1 to 4, wherein the heat source is an acetylene flame or a DC plasma flame. 請求の範囲１〜５の何れかにおいて、前記液状流体が、水であることを特徴とする微粒子の製造方法。The method for producing fine particles according to any one of claims 1 to 5, wherein the liquid fluid is water. 請求の範囲１〜６の何れかにおいて、前記原料が、金属、合金、酸化物、窒化物及び酸窒化物から選択される少なくとも一種であることを特徴とする微粒子の製造方法。The method for producing fine particles according to any one of claims 1 to 6, wherein the raw material is at least one selected from metals, alloys, oxides, nitrides, and oxynitrides. 請求の範囲１〜７の何れかにおいて、前記熱源が、酸化雰囲気又は窒化雰囲気の何れかであり、酸化物、窒化物及び酸窒化物の何れかの微粒子を得ることを特徴とする微粒子の製造方法。The production of fine particles according to any one of claims 1 to 7, wherein the heat source is either an oxidizing atmosphere or a nitriding atmosphere to obtain fine particles of oxide, nitride, or oxynitride. Method. 請求の範囲１〜７の何れかにおいて、前記原料が、Ｉｎ−Ｓｎ合金又ＩＴＯ粉末であり、酸化インジウム−酸化錫粉末を製造することを特徴とする微粒子の製造方法。The method for producing fine particles according to any one of claims 1 to 7, wherein the raw material is an In-Sn alloy or ITO powder, and an indium oxide-tin oxide powder is produced. 請求の範囲９において、錫含有量がＳｎＯ２換算で２．３〜４５質量％である酸化インジウム−酸化錫粉末を製造することを特徴とする微粒子の製造方法。The method for producing fine particles according to claim 9, wherein an indium oxide-tin oxide powder having a tin content of 2.3 to 45% by mass in terms of SnO 2 is produced. 請求の範囲１〜１０の何れかにおいて、前記生成物の前記液状流体により捕獲する際の最大速度が、１５０ｍ／ｓｅｃ以下であることを特徴とする微粒子の製造方法。The method for producing fine particles according to any one of claims 1 to 10, wherein a maximum speed when the product is captured by the liquid fluid is 150 m / sec or less. 熱源中に原料を液流、液滴又は粉末として供給することにより得られる生成物を気体流体と共に導入する導入口と、導入された生成物に対して霧状の液状流体を噴射する流体噴射手段と、液状流体で捕獲された微粒子を気液分離して前記微粒子のスラリーを得る気液分離手段と、液状流体で捕獲できなかった微粒子を含む雰囲気流体の一部を流体滴噴射位置まで戻して循環させる循環手段とを具備することを特徴とする微粒子の製造装置。An inlet for introducing a product obtained by supplying a raw material into a heat source as a liquid flow, droplets or powder together with a gaseous fluid, and a fluid ejecting means for ejecting a mist-like liquid fluid to the introduced product Gas-liquid separation means for separating the fine particles captured by the liquid fluid into a gas-liquid separation to obtain a slurry of the fine particles, and returning a part of the atmospheric fluid containing the fine particles that could not be captured by the liquid fluid to the fluid droplet ejection position An apparatus for producing fine particles, comprising a circulation means for circulation. 請求の範囲１２において、前記気液分離手段の下流側にさらに、液状流体で捕獲できなかった微粒子を含む雰囲気流体の一部を導入すると共に霧状の液状流体を噴射し気液分離して前記微粒子のスラリーを得る第２の気液分離手段を具備することを特徴とする微粒子の製造装置。In claim 12, a part of the atmospheric fluid containing fine particles that could not be captured by the liquid fluid is further introduced to the downstream side of the gas-liquid separation means, and a mist-like liquid fluid is injected to perform gas-liquid separation, thereby An apparatus for producing fine particles, comprising second gas-liquid separation means for obtaining a fine particle slurry. 請求の範囲１３において、前記気液分離手段の下流側にさらに、液状流体で捕獲できなかった微粒子を含む雰囲気流体の一部を前記第２の気液分離手段の導入部まで戻す第２の循環手段を具備することを特徴とする微粒子の製造装置。The second circulation according to claim 13, wherein a part of the atmospheric fluid containing fine particles that could not be captured by the liquid fluid is further returned to the downstream side of the gas-liquid separation means to the introduction portion of the second gas-liquid separation means. An apparatus for producing fine particles, characterized by comprising means. 請求の範囲１２〜１４の何れかにおいて、前記気液分離手段がサイクロンであることを特徴とする微粒子の製造装置。The apparatus for producing fine particles according to any one of claims 12 to 14, wherein the gas-liquid separation means is a cyclone. 請求の範囲１２〜１５の何れかにおいて、前記流体噴射手段が噴射した液状流体に微粒子が捕獲される際の最大速度が１５０ｍ／ｓｅｃ以下であることを特徴とする微粒子の製造装置。16. The apparatus for producing fine particles according to any one of claims 12 to 15, wherein a maximum speed when the fine particles are captured by the liquid fluid ejected by the fluid ejecting means is 150 m / sec or less.
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