JP2736492B2 - Method for producing indium oxide-tin oxide powder - Google Patents
Method for producing indium oxide-tin oxide powderInfo
- Publication number
- JP2736492B2 JP2736492B2 JP4360973A JP36097392A JP2736492B2 JP 2736492 B2 JP2736492 B2 JP 2736492B2 JP 4360973 A JP4360973 A JP 4360973A JP 36097392 A JP36097392 A JP 36097392A JP 2736492 B2 JP2736492 B2 JP 2736492B2
- Authority
- JP
- Japan
- Prior art keywords
- indium
- powder
- ito
- oxide powder
- tin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Physical Vapour Deposition (AREA)
Description
【0001】[0001]
【産業上の利用分野】この発明は、ITO膜(Indium-T
in Oxide膜)を始めとした酸化インジウム系表示材料等
の製造原料として好適な“酸化インジウム−酸化スズ粉
末(酸化インジウム粉末と酸化スズ粉末との混合粉末
で、 以降はITO粉末と記す)”の製造方法に関するも
のである。The present invention relates to an ITO film (Indium-T
Indium oxide-tin oxide powder (mixed powder of indium oxide powder and tin oxide powder, hereinafter referred to as ITO powder), which is suitable as a raw material for producing indium oxide-based display materials such as in oxide film) It relates to a manufacturing method.
【0002】[0002]
【従来技術とその課題】これまで、亜鉛鉱中に極く微量
含まれていて副産物として回収されていたインジウムの
興味深い特性が次第に明らかになるにつれ、その用途に
関する多くの提案がなされてきたが、近年、インジウム
酸化物、特に“ITO”と呼ばれる“Snを含んだインジ
ウム酸化物(In2O3-SnO2)”の薄膜が有する高い導電性
や透明性に注目が集まり、液晶表示装置,薄膜エレクト
ロルミネッセンス表示装置,放射線検出素子,端末機器
の透明タブレット等の多岐にわたる用途が開かれた。2. Description of the Related Art As the interesting properties of indium, which is contained in a very small amount in zinc ore and recovered as a by-product, have been gradually elucidated, many proposals for its use have been made. In recent years, attention has been focused on high conductivity and transparency of a thin film of indium oxide, particularly, “Indium oxide containing Sn (In 2 O 3 —SnO 2 )” called “ITO”. A wide variety of applications have been opened, such as electroluminescent display devices, radiation detection elements, and transparent tablets for terminal equipment.
【0003】ところで、上述のような装置・機器類の製
造原料として準備される酸化インジウム粉末や酸化スズ
粉末は、従来、図3に示す如きそれぞれの工程に従って
製造されている。[0003] Meanwhile, indium oxide powder and tin oxide powder prepared as a raw material for manufacturing the above-mentioned devices and equipment are conventionally manufactured according to respective steps as shown in FIG.
【0004】即ち、酸化インジウム粉末の場合は、まず
第1段階として、金属インジウムを硝酸で溶解し、これ
をアンモニア水で中和して水酸化インジウムとして沈降
させる。そして、この沈積物(水酸化インジウム)をろ
過,洗浄,乾燥する。次に、第2段階として、得られた
水酸化インジウムを焙焼し、酸化インジウム粉末とす
る。That is, in the case of indium oxide powder, first, as a first step, metal indium is dissolved with nitric acid, which is neutralized with aqueous ammonia and precipitated as indium hydroxide. Then, the deposit (indium hydroxide) is filtered, washed, and dried. Next, as a second stage, the obtained indium hydroxide is roasted to obtain indium oxide powder.
【0005】また、酸化スズ粉末の場合には、第1段階
として金属スズを硝酸で溶解し、これをメタスズ酸とし
て沈降させる。そして、この沈積物(メタスズ酸)をろ
過,洗浄,乾燥し、第2段階として、得られたメタスズ
酸を焙焼し酸化スズ粉末とする。[0005] In the case of tin oxide powder, as a first step, metal tin is dissolved with nitric acid and this is precipitated as metastannic acid. Then, the deposit (metastannous acid) is filtered, washed, and dried. As a second step, the obtained metastannic acid is roasted to obtain tin oxide powder.
【0006】なお、このようにして製造された酸化イン
ジウム粉末並びに酸化スズ粉末は、両者を混合してスパ
ッタリングタ−ゲット等に成形した上で、薄膜を形成す
るためにスパッタリング等の成膜素材として用いられる
ことが多い。[0006] The indium oxide powder and tin oxide powder thus produced are mixed together to form a sputtering target or the like, and then formed into a film forming material such as sputtering to form a thin film. Often used.
【0007】しかしながら、酸化インジウム粉末や酸化
スズ粉末の製造に係る上記方法には次のような問題が指
摘された。 a) 得られる酸化物粉末は諸特性(平均粒径,見掛密度
等)のバラツキが大きく、これがITO系の表示材料等
の“品質バラツキの低減”或いは“高品質化”の阻害要
因となっている。 b) 製造条件(液温,反応速度等)を一定に制御するこ
とが必ずしも容易でなく、これを安定させるために設備
コストが上昇する。 c) 従来とは特性の異なる粉末を要求された場合に、こ
の要求への柔軟な対応ができない。 d) 製造装置が比較的大掛かりとなり、そのため製造条
件を一定に制御しようとするとかなりの労力を要する
上、増産への対応が必ずしも容易とは言えない。 e) 溶解廃液(例えば硝酸アンモニウム)がその都度発
生するのでその処理が必要であり、これがランニングコ
ストを高める。[0007] However, the following problems have been pointed out in the above-mentioned method relating to the production of indium oxide powder and tin oxide powder. a) The resulting oxide powder has large variations in various properties (average particle size, apparent density, etc.), which is a hindrance to "reducing the quality variation" or "improving the quality" of ITO-based display materials. ing. b) It is not always easy to control the production conditions (liquid temperature, reaction rate, etc.) at a constant level, and equipment costs increase to stabilize them. c) When a powder with different characteristics from the conventional one is required, it is not possible to respond flexibly to this requirement. d) The production equipment becomes relatively large-scale, so that constant control of the production conditions requires a considerable amount of labor, and it is not always easy to cope with increased production. e) Dissolved effluent (eg, ammonium nitrate) is generated each time and needs to be treated, which increases running costs.
【0008】このようなことから、本発明が目的とした
のは、上記諸問題を解消し、表示材料の原料等としても
十分に満足できる優れた特性を備えた酸化インジウム粉
末,酸化スズ粉末を、製造性良く安定に、かつコスト安
く提供できる手立てを確立することであった。In view of the above, an object of the present invention is to solve the above problems and provide an indium oxide powder and a tin oxide powder having excellent properties which can be sufficiently satisfied as a raw material of a display material. The objective is to establish a means that can be provided stably at a low cost with good manufacturability.
【0009】[0009]
【課題を解決するための手段】そこで、本発明者等は上
記目的を達成すべく様々な観点から研究を行ったとこ
ろ、次のような知見を得ることができた。The present inventors have conducted research from various viewpoints to achieve the above object, and have obtained the following findings.
【0010】インジウムやスズの酸化物粉末を製造する
に当って、その第1段階として従来の如き「溶解沈澱
法」ではなく「電解法」を採用し、しかもその際にイン
ジウムとスズを別個の陽極として同時に電解処理する
と、比較的低い設備費やランニングコストの下で安定し
た条件にて“水酸化インジウム”と“メタスズ酸”の混
合沈積物を一工程で製造することが可能となる上、この
混合沈積物をか焼することによって非常に幅広い領域の
諸特性(平均粒径,見掛密度等)を有したITO粉末
(酸化インジウム粉末と酸化スズ粉末との混合粉末)を
安定して得ることができ、しかも電解条件の選択によっ
てこれら諸特性をきめ細かくコントロ−ルすることも可
能である。In producing an oxide powder of indium or tin, an "electrolysis method" is adopted as a first step instead of the conventional "dissolution precipitation method", and in addition, indium and tin are separated from each other. Simultaneous electrolytic treatment of the anode makes it possible to produce a mixed deposit of "indium hydroxide" and "metastannic acid" in one step under stable conditions with relatively low equipment costs and running costs. By calcining this mixed sediment, an ITO powder (mixed powder of indium oxide powder and tin oxide powder) having various properties (average particle size, apparent density, etc.) in a very wide range can be stably obtained. It is also possible to finely control these characteristics by selecting the electrolysis conditions.
【0011】本発明は、上記知見事項等に基づいてなさ
れたものであり、「インジウムとスズを別個の陽極とし
て同時に電解し、 これによって得た水酸化インジウムと
メタスズ酸の混合沈積物をか焼することによって、 平均
粒径や見掛密度等の特性バラツキの小さいITO粉末を
安定かつ低コストで、 しかも特性コントロ−ル容易に製
造し得るようにした点」に大きな特徴を有している。The present invention has been made based on the above findings and the like. "Indium and tin are simultaneously electrolyzed as separate anodes, and the resulting mixed deposit of indium hydroxide and metastannic acid is calcined. By doing so, it is possible to produce ITO powder with small variations in characteristics such as average particle diameter and apparent density, stably, at low cost, and easily control the characteristics. "
【0012】ところで、上述したように、本発明に係る
ITO粉末の製造方法では、従来とは異なって、まず電
解液中で金属インジウム及び金属スズを陽極として電解
することにより水酸化インジウムとメタスズ酸を同時に
析出させ、次いでこの混合沈積物をか焼(焙焼)すると
いう工程が採られるが、これらの金属を陽極電解する際
に適用される電解液については特に指定されるものでは
なく、硝酸アンモニウム,硫酸アンモニウム,その他の
電解質等の何れを用いても良いものの、コストや製品の
純度維持の面から硝酸アンモニウム水溶液が好ましいと
言える。By the way, as described above, in the method for producing ITO powder according to the present invention, unlike the conventional method, first, indium hydroxide and metastannic acid are electrolyzed in an electrolytic solution using metal indium and metal tin as anodes. At the same time, and then calcining (roasting) the mixed sediment. However, the electrolytic solution used for anodic electrolysis of these metals is not particularly specified, and ammonium nitrate is used. Any of ammonium, ammonium sulfate, and other electrolytes may be used, but it can be said that an ammonium nitrate aqueous solution is preferable in terms of cost and maintenance of product purity.
【0013】なお、水酸化インジウムとメタスズ酸を同
時に析出させるための“電解法”としては、通常のいわ
ゆる平波による電解法,周期的反転電流による電解法
(PR電解法)の何れを採用しても良い。そして、水酸
化インジウムとメタスズ酸を析出させる際の電解条件を
選択することで、これをか焼して得られるITO粉末の
平均粒径,比表面積又は見掛密度等の制御が可能であ
り、これらの調整は、ITO系の表示材料等の原料とし
て用いた場合における製品品質の著しい改善に結びつ
く。As the "electrolysis method" for simultaneously depositing indium hydroxide and metastannic acid, any of a usual so-called flat-wave electrolysis method and a periodic reversal current electrolysis method (PR electrolysis method) is employed. May be. And, by selecting the electrolysis conditions when depositing indium hydroxide and metastannic acid, it is possible to control the average particle size, specific surface area, apparent density, etc. of the ITO powder obtained by calcining it. These adjustments lead to a remarkable improvement in product quality when used as a raw material such as an ITO display material.
【0014】図1は、この電解法を取り入れた本発明に
係る“ITO粉末の製造工程例”を示している。ここ
で、図1に例示される工程でITO粉末をより安定に製
造するには、好ましくはか焼に供する“水酸化インジウ
ムとメタスズ酸の混合沈積物”を得るための“電解”
を、NH4 NO3 濃度が 0.2〜5mol/L(リットル) 、pHが
4〜9.5 、そして浴温が0〜50℃の硝酸アンモニウム
水溶液中で実施し、その時の電流密度を100〜180
0A/m2 の範囲に制御するのが良い。FIG. 1 shows "an example of a process for producing an ITO powder" according to the present invention incorporating this electrolytic method. Here, in order to more stably produce the ITO powder in the process illustrated in FIG. 1, preferably, “electrolysis” for obtaining “a mixed deposit of indium hydroxide and metastannic acid” to be subjected to calcination.
Is carried out in an aqueous ammonium nitrate solution having an NH 4 NO 3 concentration of 0.2 to 5 mol / L (liter), a pH of 4 to 9.5, and a bath temperature of 0 to 50 ° C., and the current density at that time is 100 to 180
It is better to control the pressure within the range of 0 A / m 2 .
【0015】つまり、電解浴(硝酸アンモニウム水溶
液)のNH4 NO3 濃度が 0.2mol/Lを下回ると電流効
率低下又は電力原単位上昇を招く恐れがあり、また5mo
l/L を超えると薬品消費量の増大が無視できなくなる。
そして、浴のpHが4を下回ると沈積物が微細化して固
液分離困難となり、一方、9.5 を上回る浴の取扱いは安
全上もしくは環境防災上好ましくないので、これを避け
るのが通例である。That is, if the concentration of NH 4 NO 3 in the electrolytic bath (aqueous ammonium nitrate solution) is lower than 0.2 mol / L, the current efficiency may decrease or the power consumption may increase.
If it exceeds l / L, the increase in chemical consumption cannot be ignored.
If the pH of the bath is lower than 4, the sediment becomes finer and solid-liquid separation becomes difficult. On the other hand, handling of the bath higher than 9.5 is not preferable for safety or environmental disaster prevention.
【0016】浴温については、0℃未満に調整すること
は冷却コストの点で不利となり、一方、50℃を超える
温度に維持しようとするとそのための加熱コストが無視
できなくなる上、特にNH4 NO3 の場合にはアンモニ
ア蒸気発生に対応した環境対策が必要となる。更に、電
流密度については、100A/m2 を下回ると生産性が
悪くなり、一方、1800A/m2 を上回る場合には槽
電圧の上昇が著しくなって経済的に不利になる。Adjusting the bath temperature to less than 0 ° C. is disadvantageous in terms of cooling cost. On the other hand, if the temperature is to be maintained at a temperature exceeding 50 ° C., the heating cost cannot be ignored, and in particular, NH 4 NO In case 3 , environmental measures must be taken to cope with the generation of ammonia vapor. Further, with respect to the current density, if the current density is lower than 100 A / m 2 , the productivity is deteriorated. On the other hand, if the current density is higher than 1800 A / m 2 , the cell voltage is significantly increased, which is economically disadvantageous.
【0017】さて、本発明に係る「ITO粉末の製造方
法」によると次のような利点を享受することができ、従
ってその産業上の寄与は極めて大きいと言える。 1) 得られるITO粉末の“諸特性(平均粒径,見掛密
度等)の幅”が広く、これらを電解条件の選択によって
コントロ−ルできる。 2) か焼に供する中間原料たる水酸化インジウムとメタ
スズ酸の混合沈積物の製造が電解法にて同時に行われる
ので連続方式が採用でき、バッチ方式の従来法に比べて
品質管理が容易で、品質そのものも安定する。 3) 電解条件の選択により最終的に得られるITO粉末
の諸特性を微妙にコントロ−ルできるため、これう使用
するITO系の表示材料等の高品質化や品質バラツキの
低減が達成できる。 4) 個別に得た酸化物(酸化インジウム,酸化スズ)同
士を混合してITO粉末とする従来法に比べ、共電解法
で得た混合沈積物をか焼して実質的な混合工程無しにI
TO粉末とする本発明方法では、酸化物の混合がより均
一となって得られるITO粉末は非常に均質である。 5) いわゆる“クロ−ズドシステム”化ができるので、
中和の都度に硝酸及び硝 酸アンモニウム水溶液の廃液が
発生していた従来法に比べてランニングコストの大幅な
低減が達成される。 6) 製造装置がコンパクトであるので、イニシャルコス
ト(建設費)も安価となり増産への対応がしやすい。According to the "production method of ITO powder" according to the present invention, the following advantages can be enjoyed, and it can be said that its industrial contribution is extremely large. 1) The obtained ITO powder has a wide range of "characteristics (average particle size, apparent density, etc.)", and these can be controlled by selecting the electrolysis conditions. 2) Since the production of mixed deposits of indium hydroxide and metastannic acid, which are intermediate raw materials to be calcined, is performed simultaneously by the electrolytic method, a continuous method can be adopted, and quality control is easier than the conventional method of the batch method. The quality itself is stable. 3) Various properties of the finally obtained ITO powder can be delicately controlled by selecting the electrolysis conditions, so that it is possible to achieve high quality and reduction in quality variation of the ITO display material used. 4) Compared with the conventional method of mixing individually obtained oxides (indium oxide, tin oxide) with each other to form ITO powder, calcining the mixed deposit obtained by the co-electrolysis method eliminates a substantial mixing step. I
In the method of the present invention in which a TO powder is used, the ITO powder obtained by mixing the oxides more uniformly is very homogeneous. 5) Since a so-called “closed system” can be made,
Waste of nitric acid and nitric acid aqueous solution of ammonium is a significant reduction in running costs can be achieved as compared with the conventional method that occurred each time the neutralization. 6) Since the manufacturing equipment is compact, the initial cost (construction cost) is low, and it is easy to respond to increased production.
【0018】なお、本発明に係るITO粉末は、これを
前述したITOスパッタリングタ−ゲットに成形してI
TO膜の形成に用いた場合に特に優れた結果を得ること
ができるが、ITO粉末からITOタ−ゲットを製造す
るには一般に図2で示した工程が採られる。The ITO powder according to the present invention is formed into the above-mentioned ITO sputtering target by molding it.
Particularly excellent results can be obtained when used for forming a TO film, but the steps shown in FIG. 2 are generally employed for producing an ITO target from ITO powder.
【0019】続いて、本発明を実施例によって更に具体
的に説明する。Next, the present invention will be described more specifically with reference to examples.
〈実施例1〉10℃の硝酸アンモニウム水溶液(NH4
NO3 濃度:0.5mol/L,pH:8)中において、それぞ
れ表面積の異なる金属インジウムと金属スズとを陽極と
し、陰極電流密度を何れも600A/m2 として、PR
式のパルス通電により同時に電解を行った。そして、電
解槽底の沈積物をろ過,洗浄及び乾燥し、水酸化インジ
ウムとメタスズ酸の混合沈積物を得た。次に、これを1
100℃で焙焼し、平均粒径20μm,見掛密度1.7g/c
m3のITO粉末を得た。Example 1 An aqueous solution of ammonium nitrate (NH 4 ) at 10 ° C.
In NO 3 concentration: 0.5 mol / L, pH: 8), PR was determined by using metal indium and metal tin having different surface areas as anodes and the cathode current density as 600 A / m 2 , respectively.
Electrolysis was performed simultaneously by the pulse current of the formula. Then, the deposit at the bottom of the electrolytic cell was filtered, washed and dried to obtain a mixed deposit of indium hydroxide and metastannic acid. Next, this is 1
Roast at 100 ° C, average particle size 20μm, apparent density 1.7g / c
m 3 of ITO powder was obtained.
【0020】次いで、得られた上記ITO粉末を原料と
し、コ−ルドプレス大気焼結法によりSnO2 含有割合が
10wt%のITOスパッタリングタ−ゲットを製造した
ところ、焼結体の密度は6.70g/cm3であった。Next, an ITO sputtering target having a SnO 2 content of 10 wt% was produced from the obtained ITO powder as a raw material by a cold press atmospheric sintering method, and the density of the sintered body was 6.70 g / g. It was cm 3.
【0021】更に、このITOタ−ゲットをスパッタし
て得られた透明導電膜のシ−ト抵抗や透過率等の諸特性
を調査したところ、LCD(液晶)用としても十分に使
用可能な満足できる結果を示すことが確認された。Further, when the characteristics of the transparent conductive film obtained by sputtering this ITO target, such as sheet resistance and transmittance, were examined, it was found that the film could be used sufficiently for LCD (liquid crystal). It has been confirmed that it shows possible results.
【0022】〈実施例2〉電解浴として浴温:50℃,
NH4 NO3 濃度:1.0mol/L,pH:6の硝酸アンモニ
ウム水溶液を使用した以外は、実施例1の場合と同一条
件でPR方式のパルス電解を行い、電解槽底の沈積物を
ろ過,洗浄及び乾燥して水酸化インジウムとメタスズ酸
の混合沈積物を得た。次に、これを1100℃で焙焼し
たところ、粒径が揃った見掛密度の高いITO粉末が得
られた。Example 2 An electrolytic bath having a bath temperature of 50 ° C.
Except for using an aqueous solution of ammonium nitrate having an NH 4 NO 3 concentration of 1.0 mol / L and a pH of 6, the pulse electrolysis of the PR method was performed under the same conditions as in Example 1, and the deposits at the bottom of the electrolytic cell were filtered and washed. Then, drying was performed to obtain a mixed deposit of indium hydroxide and metastannic acid. Next, when this was roasted at 1100 ° C., an ITO powder having a high apparent density and a uniform particle size was obtained.
【0023】次いで、得られたITO粉末を使用し、実
施例1におけると同様にSnO2 含有割合が10wt%のI
TOスパッタリングタ−ゲットを製造したところ、焼結
体の密度は4.78g/cm3であった。Next, the obtained ITO powder was used and, as in Example 1, an SnO 2 content of 10 wt%
When a TO sputtering target was manufactured, the density of the sintered body was 4.78 g / cm 3 .
【0024】このITOタ−ゲットをスパッタし、得ら
れた透明導電膜のシ−ト抵抗や透過率等の諸特性を調査
したところ、LCD用としても十分に使用可能な満足で
きる結果を示すことが確認された。The ITO target was sputtered, and various characteristics such as sheet resistance and transmittance of the obtained transparent conductive film were examined. Was confirmed.
【0025】[0025]
【効果の総括】以上に説明した如く、この発明によれ
ば、例えばITO膜形成用スパッタリングタ−ゲットの
原材料等としても十分に満足できるITO粉末を、要求
特性に幅広く的確に対応しつつ低コストで提供すること
が可能となるなど、産業上有用な効果がもたらされる。As described above, according to the present invention, for example, ITO powder which can be sufficiently satisfied as a raw material of a sputtering target for forming an ITO film can be produced at a low cost while responding to a wide range of required characteristics. And industrially useful effects are provided.
【図1】本発明に係る“ITO粉末の製造工程”の概要
説明図である。FIG. 1 is a schematic explanatory view of a “production process of ITO powder” according to the present invention.
【図2】ITO粉末からITOスパッタリングタ−ゲッ
トを製造する工程の説明図である。FIG. 2 is an explanatory diagram of a process for producing an ITO sputtering target from ITO powder.
【図3】従来の酸化インジウム粉末及び酸化スズ粉末の
製造工程に関する概要説明図である。FIG. 3 is a schematic explanatory view showing a conventional process for producing indium oxide powder and tin oxide powder.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭63−195101(JP,A) 特開 平6−199523(JP,A) 特開 平6−171937(JP,A) ────────────────────────────────────────────────── ─── Continuation of front page (56) References JP-A-63-195101 (JP, A) JP-A-6-199523 (JP, A) JP-A-6-171937 (JP, A)
Claims (2)
時に電解し、これによって得た水酸化インジウムとメタ
スズ酸の混合沈積物をか焼することを特徴とする、酸化
インジウム−酸化スズ粉末の製造方法。1. A method for producing an indium oxide-tin oxide powder, comprising simultaneously electrolyzing indium and tin as separate anodes and calcining a mixed deposit of indium hydroxide and metastannic acid. .
インジウムとスズの電解を行うことを特徴とする、請求
項1に記載の酸化インジウム−酸化スズ粉末の製造方
法。2. The method for producing indium oxide-tin oxide powder according to claim 1, wherein indium and tin are electrolyzed using an aqueous solution of ammonium nitrate as an electrolytic solution.
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4360973A JP2736492B2 (en) | 1992-12-28 | 1992-12-28 | Method for producing indium oxide-tin oxide powder |
US08/164,125 US5417816A (en) | 1992-12-09 | 1993-12-07 | Process for preparation of indium oxide-tin oxide powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4360973A JP2736492B2 (en) | 1992-12-28 | 1992-12-28 | Method for producing indium oxide-tin oxide powder |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH06199522A JPH06199522A (en) | 1994-07-19 |
JP2736492B2 true JP2736492B2 (en) | 1998-04-02 |
Family
ID=18471665
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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JP4360973A Expired - Lifetime JP2736492B2 (en) | 1992-12-09 | 1992-12-28 | Method for producing indium oxide-tin oxide powder |
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JP (1) | JP2736492B2 (en) |
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KR101324130B1 (en) * | 2007-01-10 | 2013-11-01 | 삼성코닝정밀소재 주식회사 | Indium tin oxide powder and manufacturing method of producing the same |
CN102634816B (en) * | 2011-02-14 | 2014-11-19 | 李小毛 | Preparation method of nanometer tin indium oxide powder |
CN103857830B (en) * | 2011-07-26 | 2016-09-21 | 吉坤日矿日石金属株式会社 | Indium hydroxide or the manufacture method of the compound containing indium hydroxide |
JP6090442B2 (en) * | 2013-05-27 | 2017-03-08 | 住友金属鉱山株式会社 | Method for producing indium hydroxide powder and method for producing indium oxide powder |
CN109536982B (en) * | 2018-12-27 | 2021-04-13 | 广东先导稀材股份有限公司 | Preparation method of nano tin dioxide |
-
1992
- 1992-12-28 JP JP4360973A patent/JP2736492B2/en not_active Expired - Lifetime
Also Published As
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JPH06199522A (en) | 1994-07-19 |
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