JP4496875B2 - Indium oxide powder and method for producing the same - Google Patents
Indium oxide powder and method for producing the same Download PDFInfo
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- JP4496875B2 JP4496875B2 JP2004223003A JP2004223003A JP4496875B2 JP 4496875 B2 JP4496875 B2 JP 4496875B2 JP 2004223003 A JP2004223003 A JP 2004223003A JP 2004223003 A JP2004223003 A JP 2004223003A JP 4496875 B2 JP4496875 B2 JP 4496875B2
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本発明は、粒径のばらつきが小さい酸化インジウム粉末とその製造方法に関する。本発明の酸化インジウムは高密度なＩＴＯ焼結体の原料として好適である。 The present invention relates to an indium oxide powder having a small variation in particle size and a method for producing the same. The indium oxide of the present invention is suitable as a raw material for a high-density ITO sintered body.
最近、液晶ディスプレイが広く使用されており、この透明導電膜としてＩＴＯ膜が利用されている。ＩＴＯ膜の成膜方法としては、スプレー法や塗布法などの化学的製法、真空蒸着法やスパッタリング法などの物理的製法が知られている。スパッタリング法は、ＩＴＯターゲット材に高電圧を与えてターゲット材料粒子を高エネルギーで基板表面に衝突させることによって成膜する方法であり、ターゲット材として酸化インジウムと酸化スズとを混合焼結した酸化物焼結体が主に用いられている。 Recently, liquid crystal displays are widely used, and an ITO film is used as the transparent conductive film. As a method for forming an ITO film, a chemical manufacturing method such as a spray method or a coating method, and a physical manufacturing method such as a vacuum evaporation method or a sputtering method are known. The sputtering method is a method of forming a film by applying a high voltage to an ITO target material and causing target material particles to collide with the substrate surface with high energy. An oxide obtained by mixing and sintering indium oxide and tin oxide as a target material. Sintered bodies are mainly used.
スパッタリングによって良質なＩＴＯ膜を形成するために高密度なＩＴＯ焼結体が要求されており、この高密度ＩＴＯ焼結体の原料として粒径のばらつきが小さい酸化インジウムが必要とされている。
In order to form a high-quality ITO film by sputtering , a high-density ITO sintered body is required, and indium oxide having a small variation in particle size is required as a raw material for this high-density ITO sintered body.
高密度ＩＴＯターゲット用原料として用いられる酸化インジウム粉末の製造方法として、従来、硝酸インジウム溶液を中和して生じた水酸化インジウムの沈澱を乾燥して焙焼する方法が知られている。しかし、この中和沈澱法によって製造した酸化インジウム粉末は粒径や比重が不均一であるため高密度なターゲット材が得られないと云う問題がある。上記沈澱法に代え、電解法によって水酸化インジウムを製造し、これを焙焼して酸化インジウム粉末を得る方法が知られている（特許文献１）。しかし、上記電解法によって得られる酸化インジウム粉末は平均粒径や比表面積およびピーク粒径からみると粒径の均一性は未だ不十分であり、高密度ターゲット材を得るためには更に均一性の高いものが望まれる。 As a method for producing an indium oxide powder used as a raw material for a high density ITO target, a method for drying and roasting a precipitate of indium hydroxide generated by neutralizing an indium nitrate solution has been known. However, the indium oxide powder produced by this neutralization precipitation method has a problem that a high-density target material cannot be obtained because the particle size and specific gravity are not uniform. Instead of the precipitation method, a method is known in which indium hydroxide is produced by an electrolytic method, and this is roasted to obtain an indium oxide powder (Patent Document 1). However, the indium oxide powder obtained by the above electrolytic method is still insufficient in uniformity of particle size when viewed from the average particle size, specific surface area, and peak particle size. A high one is desired.
上記電解法の改良法として、金属インジウムを陽極として電解する際に、電解液を攪拌して水酸化インジウム沈澱を懸濁させた状態で電解を行い、生成した水酸化インジウム沈澱を焼成して酸化インジウム粉末を得る方法が知られている（特許文献２）。この方法はＢＥＴ比表面積が１０m2/g以下であって嵩密度が格段に小さく、粒径の均一性に優れた酸化インジウム粉末を得ることができる利点を有している。
従来は上記のように、粒径の均一性に優れた酸化インジウム粉末を得る方法として、電解法による水酸化インジウムの沈澱生成について改良が加えられている。しかし、水酸化インジウムを焼成して酸化インジウム粉末にする工程においても粒径の均一性を阻害する要因があり、焼成温度をコントロールしても焼成炉内の水蒸気分圧が異なれば、得られる酸化インジウム粉末の比表面積のばらつきが大きくなるという問題がある。 Conventionally, as described above, as a method for obtaining an indium oxide powder having excellent particle size uniformity, improvements have been made in the formation of precipitation of indium hydroxide by an electrolytic method. However, in the process of firing indium hydroxide to form indium oxide powder, there is a factor that hinders the uniformity of the particle size, and if the partial pressure of water vapor in the firing furnace is different even if the firing temperature is controlled, the resulting oxidation There is a problem that the variation of the specific surface area of the indium powder becomes large.
本発明は、水酸化インジウムの焼成工程における上記問題を見出し、これを改良したものであり、水酸化インジウムの焼成雰囲気を制御することによって均一性の高い酸化インジウム粉末を得る方法とその酸化インジウム粉末を提供する。 The present invention has found and improved the above problems in the indium hydroxide firing step, and a method for obtaining a highly uniform indium oxide powder by controlling the firing atmosphere of indium hydroxide and the indium oxide powder. I will provide a.
本発明は以下の酸化インジウム粉末とその製造方法に関する。
〔１〕ＢＥＴ値比表面積が１０m2/g〜２０m2/gであり、平均比表面積の標準偏差が０.２以下であることを特徴とする酸化インジウム粉末。
〔２〕ＩＴＯターゲット材料として用いられる上記[１]に記載する酸化インジウム粉末。
〔３〕水酸化インジウムを焼成して酸化インジウムを製造する方法において、水分を含む空気を焼成炉内に導入し、炉内の水蒸気分圧を０.００１〜０.３に制御して焼成することによって、ＢＥＴ値比表面積が１０m2/g〜２０m2/g、平均比表面積の標準偏差が０.２以下である酸化インジウム粉末を製造することを特徴とする酸化インジウム粉末の製造方法。
The present invention relates to the following indium oxide powder and a method for producing the same.
[1] An indium oxide powder having a BET specific surface area of 10 m 2 / g to 20 m 2 / g and a standard deviation of an average specific surface area of 0.2 or less .
[2] The indium oxide powder according to [1], which is used as an ITO target material .
[3] In a method for producing indium oxide by firing indium hydroxide, moisture-containing air is introduced into the firing furnace, and the steam partial pressure in the furnace is controlled to 0.001 to 0.3 for firing. Thus, an indium oxide powder having a BET specific surface area of 10 m 2 / g to 20 m 2 / g and a standard deviation of an average specific surface area of 0.2 or less is produced.
〔具体的な説明〕
本発明は、ＢＥＴ値比表面積が１０m2/g〜２０m2/gであり、平均比表面積の標準偏差が０.２以下であることを特徴とする酸化インジウム粉末と、その製造方法に関する。本発明の酸化インジウム粉末はＩＴＯターゲット材料として好適である。
[Specific description]
The present invention relates to an indium oxide powder having a BET specific surface area of 10 m 2 / g to 20 m 2 / g and a standard deviation of an average specific surface area of 0.2 or less , and a method for producing the same. The indium oxide powder of the present invention is suitable as an ITO target material.
上記比表面積および上記標準偏差を有する酸化インジウム粉末は、水酸化インジウムを焼成して酸化インジウムを製造する方法において、焼成雰囲気の水蒸気分圧を０.００１〜０.３（絶対湿度１g/m 3 〜２００g/m 3 ）に制御して焼成することによって得ることができる。
In the indium oxide powder having the specific surface area and the standard deviation, in the method for producing indium oxide by firing indium hydroxide, the water vapor partial pressure in the firing atmosphere is 0.001 to 0.3 (absolute humidity 1 g / m 3). ˜200 g / m 3 ) can be obtained by firing.
原料となる水酸化インジウムの製造方法は限定されない。例えば、上記特許文献２に記載されているように、金属インジウムを電極に用い、硝酸アンモニウム等を電解液として電解することによって水酸化インジウム沈澱を生成させる際に、電解液を攪拌し、槽内の電解液のｐＨを均一化して電解し、生成した水酸化インジウム沈澱を脱水乾燥して得た水酸化インジウム粉末を用いることができる。 The method for producing indium hydroxide as a raw material is not limited. For example, as described in Patent Document 2 above, indium hydroxide is used as an electrode, and when an indium hydroxide precipitate is produced by electrolysis using ammonium nitrate or the like as an electrolytic solution, the electrolytic solution is stirred, It is possible to use indium hydroxide powder obtained by carrying out electrolysis with uniform pH of the electrolyte and dehydrating and drying the generated indium hydroxide precipitate.
本発明の製造方法は、水酸化インジウムを焼成して酸化インジウムを製造する工程において、焼成雰囲気の水蒸気分圧を０.００１〜０.３（絶対湿度１g/m 3 〜２００g/m 3 ）に制御して焼成する。焼成炉の種類は管状炉または縦型炉など何れでもよい。焼成温度は７００〜９００℃であればよい。
In the production method of the present invention, in the step of producing indium oxide by firing indium hydroxide, the water vapor partial pressure in the firing atmosphere is set to 0.001 to 0.3 (absolute humidity 1 g / m 3 to 200 g / m 3 ). Firing with control. The type of the firing furnace may be a tubular furnace or a vertical furnace. The baking temperature should just be 700-900 degreeC.
上記焼成工程において、焼成雰囲気の水蒸気分圧が０.００１よりも小さい（絶対湿度が１g/m 3 より低い）と、得られる酸化インジウム粉末のＢＥＴ比表面積が大きくなり、かつ平均比表面積の標準偏差が１.０より大きくなる傾向がある。一方、焼成雰囲気の水蒸気分圧を０.３より大きく（絶対湿度を２００g/m 3 より大きく）するのは工業的に高価な設備となり現実的ではなく、また、その効果も上記範囲内の場合と大差ない。焼成雰囲気の水蒸気分圧（または絶対湿度）を上記範囲に保つには、空気を温水中にバブリングして空気中の絶対湿度または水蒸気分圧を上記範囲に調整した後に、これを焼成炉内に導入するればよい。
In the above firing step, when the water vapor partial pressure in the firing atmosphere is smaller than 0.001 (absolute humidity is lower than 1 g / m 3 ) , the BET specific surface area of the obtained indium oxide powder becomes large and the standard of the average specific surface area The deviation tends to be greater than 1.0. On the other hand, if the water vapor partial pressure in the firing atmosphere is larger than 0.3 (the absolute humidity is larger than 200 g / m 3 ), this is an industrially expensive facility, and the effect is also in the above range. Not much different. In order to keep the water vapor partial pressure (or absolute humidity) in the firing atmosphere within the above range, after bubbling air into warm water to adjust the absolute humidity or water vapor partial pressure in the air to the above range, What is necessary is just to introduce.
本発明の酸化インジウム粉末は、ＢＥＴ値比表面積が１０m2g〜２０m2/gであって、平均比表面積の標準偏差が０.２以下であり、粒径の均一性が格段に優れ、しかもＩＴＯターゲット材の原料として好適な粒径を有する。なお、比表面積が上記範囲よりも小さいとＩＴＯターゲット材の原料として粒径が粗く、一方、比表面積が上記範囲よりも大きいと粒径が小さすぎて嵩高くなり、何れも高密度のターゲット材の原料として適さない。また、平均比表面積の標準偏差が１.０より大きいと粒径の均一性が低く、高密度のターゲット材原料として適さない。
The indium oxide powder according to the present invention has a BET specific surface area of 10 m 2 g to 20 m 2 / g, a standard deviation of an average specific surface area of 0.2 or less , and has excellent particle size uniformity. It has a particle size suitable as a raw material for the ITO target material. If the specific surface area is smaller than the above range, the particle size of the ITO target material is coarse. On the other hand, if the specific surface area is larger than the above range, the particle size is too small and bulky. Not suitable as a raw material. Further, if the standard deviation of the average specific surface area is larger than 1.0, the uniformity of the particle size is low and it is not suitable as a high-density target material raw material.
本発明の酸化インジウム粉末はＩＴＯターゲット材の原料として最適な比表面積と均一な粒径を有するので、この酸化インジウムと酸化スズとを混合焼結することによって高密度のＩＴＯターゲット材を得ることができ、このターゲット材を用いて良質なＩＴＯ膜を形成することができる。また、本発明の上記製造方法によれば上記ＢＥＴ比表面積と上記標準偏差を有する酸化インジウム粉末を製造することができる。 Since the indium oxide powder of the present invention has an optimum specific surface area and uniform particle size as a raw material for the ITO target material, a high density ITO target material can be obtained by mixing and sintering this indium oxide and tin oxide. It is possible to form a high-quality ITO film using this target material. Moreover, according to the said manufacturing method of this invention, the indium oxide powder which has the said BET specific surface area and the said standard deviation can be manufactured.
〔実施例および比較例〕
以下、本発明の実施例を比較例と共に示す。各例において、表１に示す量の水酸化インジウム粉末を用い、表１に示す温度で焼成した。焼成炉は管状または縦型の電気炉を用いた。焼成時間は何れも４時間である。また、実施例ではボンベから供給した空気を３０℃〜７５℃の温水にバブリングして空気中に水分を与えたものを焼成炉に導入し、炉内の水蒸気分圧を表１に示す値に調整した。この結果を表１に示した。
[Examples and Comparative Examples]
Examples of the present invention are shown below together with comparative examples. In each example, the amount of indium hydroxide powder shown in Table 1 was used and fired at the temperature shown in Table 1. A tubular or vertical electric furnace was used as the firing furnace. The firing time is 4 hours. In the examples, air supplied from a cylinder was bubbled into hot water of 30 ° C. to 75 ° C. and water was given to the air, and the water vapor partial pressure in the furnace was set to the values shown in Table 1. It was adjusted. The results are shown in Table 1.
表１に示すように、本発明の製造方法によれば、ＢＥＴ値比表面積が１０m2/g〜２０m2/gであって、平均比表面積の標準偏差が０.１６以下の酸化インジウム粉末を得ることができる。炉内湿度を調整せず、従って炉内湿度が本発明の範囲外である比較例ではＢＥＴ比表面積が２０m2/gを上回り、標準偏差も１.０を超える。 As shown in Table 1, according to the production method of the present invention, BET value specific surface area is a 10m 2 / g~20m 2 / g, the indium oxide powder standard deviation is 0.16 or less of the average specific surface area Obtainable. In the comparative example in which the furnace humidity is not adjusted, and therefore the furnace humidity is outside the range of the present invention, the BET specific surface area exceeds 20 m 2 / g and the standard deviation exceeds 1.0.
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| JP6350311B2 (en) * | 2015-01-29 | 2018-07-04 | 住友金属鉱山株式会社 | Method for producing indium oxide powder |
| CN112551572B (en) * | 2020-12-11 | 2023-08-18 | 广西晶联光电材料有限责任公司 | Preparation method of nano indium oxide with large specific surface area |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07187613A (en) * | 1993-08-11 | 1995-07-25 | Sumitomo Chem Co Ltd | Metal oxide power and its production |
| JPH1095615A (en) * | 1996-06-20 | 1998-04-14 | Mitsubishi Materials Corp | Indium oxide powder for high density sintered compact |
| JPH10204669A (en) * | 1997-01-16 | 1998-08-04 | Mitsubishi Materials Corp | Production of indium oxide powder |
| JPH1179745A (en) * | 1997-09-04 | 1999-03-23 | Mitsubishi Materials Corp | Production of indium oxide powder for ito target |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07187613A (en) * | 1993-08-11 | 1995-07-25 | Sumitomo Chem Co Ltd | Metal oxide power and its production |
| JPH1095615A (en) * | 1996-06-20 | 1998-04-14 | Mitsubishi Materials Corp | Indium oxide powder for high density sintered compact |
| JPH10204669A (en) * | 1997-01-16 | 1998-08-04 | Mitsubishi Materials Corp | Production of indium oxide powder |
| JPH1179745A (en) * | 1997-09-04 | 1999-03-23 | Mitsubishi Materials Corp | Production of indium oxide powder for ito target |
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