JPH0742109B2 - Method for producing indium oxide powder - Google Patents
Method for producing indium oxide powderInfo
- Publication number
- JPH0742109B2 JPH0742109B2 JP2417890A JP41789090A JPH0742109B2 JP H0742109 B2 JPH0742109 B2 JP H0742109B2 JP 2417890 A JP2417890 A JP 2417890A JP 41789090 A JP41789090 A JP 41789090A JP H0742109 B2 JPH0742109 B2 JP H0742109B2
- Authority
- JP
- Japan
- Prior art keywords
- indium
- indium oxide
- relative density
- specific surface
- oxide powder
- 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
Links
Description
【０００１】[0001]
【産業上の利用分野】本発明は、透明導電膜形成用の高
密度ＩＴＯ（酸化錫を含有する酸化インジウムのこと
で、Ｉｎｄｉｕｍ−Ｔｉｎ−Ｏｘｉｄｅの略称）スパッ
タリングターゲット製造用の原料粉である酸化インジウ
ム粉および高密度焼結体の製造方法に関するものであ
る。TECHNICAL FIELD The present invention relates to a high-density ITO (indium oxide containing tin oxide, which is an abbreviation of Indium-Tin-Oxide) for forming a transparent conductive film, which is a raw material powder for manufacturing a sputtering target. The present invention relates to a method for producing indium powder and a high density sintered body.
【０００２】[0002]
【従来の技術】酸化インジウムの製造方法としては下記
の諸法が提案されているが、未だ多くの解決すべき問題
点がある。2. Description of the Related Art The following methods have been proposed as a method for producing indium oxide, but there are still many problems to be solved.
【０００３】Ｉ）インジウム塩水溶液にアンモニア水、
水酸化ナトリウム等の水酸化アルカリを添加して水酸化
物を得、これを乾燥後焼成して酸化インジウムを製造す
る方法である。この方法では生成する水酸化物はゲル状
で難▲ろ▼過性であり、また焼成して得られる酸化物も
硬い塊状であって、粉砕が極めて難しい。I) Ammonia water in an aqueous solution of indium salt,
This is a method for producing an indium oxide by adding an alkali hydroxide such as sodium hydroxide to obtain a hydroxide, and drying and firing the hydroxide. The hydroxide produced by this method is gel-like and difficult to pass through, and the oxide obtained by firing is also a hard lump and is extremely difficult to pulverize.
【０００４】ＩＩ）次は、インジウムメタルあるいは塩
を直接酸化・分解して酸化インジウムを製造する方法で
あるが、この方法では塩の分解に際して多量の窒素酸化
物が発生するので環境上好ましくなく、またメタルの酸
化は塊の中心部まで十分に酸化することが難しい。更
に、この方法で得られる酸化物は硬い塊状であって、上
記したＩ）法同様に粉砕が極めて難しい。II) The following is a method of directly oxidizing and decomposing indium metal or salt to produce indium oxide, but in this method, a large amount of nitrogen oxide is generated when the salt is decomposed, which is not environmentally preferable. In addition, it is difficult to oxidize the metal sufficiently to the center of the lump. Furthermore, the oxide obtained by this method is in the form of a hard lump, and it is extremely difficult to grind it as in the above method I).
【０００５】ＩＩＩ）次は、特開昭５４−４５６９７号
公報に記載されている方法であり、即ちインジウム塩溶
液に尿素を加えて加熱することによりアンモニアを発生
させて水酸化インジウムを生成させ、これを乾燥後焼成
して酸化インジウムを製造する方法である。III) The following is the method described in JP-A-54-45697, that is, urea is added to an indium salt solution and heated to generate ammonia to generate indium hydroxide, This is a method for producing indium oxide by drying and firing it.
【０００６】ＩＶ）次は、特開昭６２−７６２７号公報
ならびに特開平１−２９０５２７号公報に記載の方法で
あり、即ち上記Ｉ）の方法で得られた水酸化物をアルコ
ールやアセトンで洗浄して解砕を容易にする方法、ある
いは有機溶媒を加え蒸留することにより溶媒置換を行な
う方法であるが、この方法では大量の有機溶剤を必要と
する。IV) The following are the methods described in JP-A-62-7627 and JP-A-1-290527, that is, the hydroxide obtained by the above method I) is washed with alcohol or acetone. This is a method for facilitating the crushing, or a method for replacing the solvent by adding an organic solvent and distilling. However, this method requires a large amount of the organic solvent.
【０００７】しかしながら、上記のような従来の技術に
あっては多くの問題点があり、特に次のような欠点があ
る。However, the above-mentioned conventional techniques have many problems, particularly the following drawbacks.
【０００８】イ）上記Ｉ）及びＩＩ）の方法では、得ら
れた酸化物の粒径が粗く、かつ粒子が硬いため事実上微
粉砕できない。B) In the above methods I) and II), the oxide particles obtained are coarse and the particles are hard, so that they cannot be practically pulverized.
【０００９】ロ）次に、ＩＩＩ）の方法では、長時間高
温を保持しないと粒子が生成されず、また該法で最終的
に得られる酸化物は特微的な針状に近い粒子の凝集体と
なる。この形態のままでは、例えば加圧成形法で成形す
る場合に成形性が悪く、成形体の最終特性に悪影響を及
ぼすことになる。(B) Next, in the method of III), particles are not generated unless the temperature is kept high for a long time, and the oxide finally obtained by the method has a characteristic acicular particle-like coagulation. It will be a collection. If this form is left as it is, for example, when it is molded by a pressure molding method, the moldability is poor and the final properties of the molded product are adversely affected.
【００１０】ハ）上記ＩＶ）の方法では、高価な有機溶
剤を大量に使用するため、著しくコスト高となる。C) In the above method IV), since a large amount of expensive organic solvent is used, the cost is remarkably high.
【００１１】上記のように、従来技術には解決すべき多
くの問題点があり、致命的とも言えるイ）ロ）ハ）のよ
うな欠点がある。As described above, the prior art has many problems to be solved, and has the drawbacks such as fatal (a), b) and c).
【００１２】[0012]
【発明が解決しようとする課題】本発明は、上記のよう
な従来技術が有する多くの問題点や諸欠点を解消し、簡
単な解砕程度の処理で分散されて微粉化でき、かつ粒子
が配向性を持たずに一次粒子形状が球形に近い酸化イン
ジウム微粉末を低コストで製造する方法及びスパッタリ
ングターゲット用相対密度７０％以上の高密度焼結体の
製造方法を目的とする。DISCLOSURE OF THE INVENTION The present invention solves many problems and drawbacks of the prior art as described above, can be dispersed and pulverized by a simple crushing process, and particles can be obtained. An object of the present invention is to provide a method for producing an indium oxide fine powder having a primary particle shape close to a sphere without orientation and at a low cost, and a method for producing a high density sintered body having a relative density of 70% or more for a sputtering target.
【００１３】[0013]
【課題を解決するための手段】本発明は、インジウム塩
水溶液から酸化インジウムを製造するに際して、酸化イ
ンジウム合成中間物として炭酸インジウムの沈殿物を生
成させることによって易解砕性の酸化インジウムが製造
できるとの知見に基づき、鋭意研究の結果開発された技
術である。According to the present invention, when indium oxide is produced from an indium salt aqueous solution, easily disintegratable indium oxide can be produced by producing a precipitate of indium carbonate as an indium oxide synthesis intermediate. It is a technology developed as a result of earnest research based on the knowledge.
【００１４】即ち、第１の発明は、６０℃以下のインジ
ウム塩水溶液に炭酸アルカリ，重炭酸アルカリのうちか
ら選ばれる少なくとも１種を加えて反応させた後、固液
分離し、得られた沈殿を乾燥，仮焼することを特徴とす
る比表面積２０ｍ２／ｇ以上の酸化インジウム粉の製造
方法であり、That is, in the first invention, at least one selected from an alkali carbonate and an alkali bicarbonate is added to an aqueous solution of indium salt at 60 ° C. or lower, and the mixture is reacted, followed by solid-liquid separation to obtain a precipitate. A method for producing indium oxide powder having a specific surface area of 20 m 2 / g or more, which comprises drying and calcination
【００１５】第２の発明は、６０℃以下のインジウム塩
水溶液に炭酸アルカリ，重炭酸アルカリのうちから選ば
れる少なくとも１種を加えて反応させた後、固液分離
し、得られた沈殿を乾燥，仮焼して得られた比表面積２
０ｍ２／ｇ以上の酸化インジウム粉８５〜９５重量％と
酸化錫５〜１５重量％とを混合してなることを特徴とす
る酸化錫添加酸化インジウム粉の製造方法である。In a second aspect of the present invention, at least one selected from alkali carbonate and alkali bicarbonate is added to an indium salt aqueous solution at 60 ° C. or lower, and the mixture is reacted, followed by solid-liquid separation and drying the resulting precipitate. , Specific surface area obtained by calcination 2
A method for producing tin oxide-added indium oxide powder, which comprises mixing 85 to 95% by weight of indium oxide powder of 0 m 2 / g or more and 5 to 15% by weight of tin oxide.
【００１６】第３の発明は、６０℃以下のインジウム塩
水溶液に炭酸アルカリ，重炭酸アルカリのうちから選ば
れる少なくとも１種を加えて反応させた後、固液分離
し、得られた沈殿を乾燥，仮焼して得られた比表面２０
ｍ２／以上の酸化インジウム粉８５〜９５重量％と酸化
錫５〜１５重量％とを混合後加圧成形し、焼成すること
を特徴とするスパッタリングターゲット用相対密度７０
％以上の高密度焼結体の製造方法である。In a third aspect of the invention, at least one selected from an alkali carbonate and an alkali bicarbonate is added to an indium salt aqueous solution at 60 ° C. or lower, and the mixture is reacted, followed by solid-liquid separation, and drying the obtained precipitate. , Specific surface 20 obtained by calcination
Relative density 70 for a sputtering target, characterized by mixing 85 to 95% by weight of indium oxide powder of m 2 / or more and 5 to 15% by weight of tin oxide, followed by pressure molding and firing.
% Of the high density sintered body is manufactured.
【００１７】次に、本発明を詳細に説明する。Next, the present invention will be described in detail.
【００１８】インジウム化合物の沈殿を生成させるに際
し、インジウム塩水溶液に炭酸アルカリあるいは重炭酸
アルカリのうちから選ばれた少なくとも１種、好ましく
はアンモニウム塩を沈殿剤として使用し、インジウム濃
度５０〜８０ｇ／ｌの水溶液に１．２〜３．０当量の沈
殿剤を該水溶液の液温を４０〜６０℃に保持しながら添
加して反応させ、インジウム化合物の沈殿を生成させ
た。得られた沈殿物は、炭酸インジウムを主体とした化
合物である。このインジウム化合物の生成反応におい
て、液温が重要な条件であって、６０℃を超える液温で
以上で反応させると水酸化インジウム主体の化合物が沈
殿生成する。In producing the precipitate of the indium compound, at least one selected from alkali carbonate and alkali bicarbonate, preferably ammonium salt, is used in the indium salt aqueous solution as a precipitant, and the indium concentration is 50 to 80 g / l. 1.2 to 3.0 equivalents of a precipitating agent was added to the aqueous solution of 1 while maintaining the liquid temperature of the aqueous solution at 40 to 60 ° C. to cause a reaction, and a precipitate of an indium compound was generated. The obtained precipitate is a compound mainly composed of indium carbonate. In this indium compound formation reaction, the liquid temperature is an important condition, and when the reaction is carried out at the liquid temperature above 60 ° C., the compound mainly containing indium hydroxide precipitates.
【００１９】ここにおいて、本発明者等は、炭酸インジ
ウム主体の沈殿物と水酸化インジウム主体の沈殿物をべ
ースとして、両沈殿物を各々乾燥，仮焼して酸化インジ
ウムを製造し両者の特性を比較したところ、炭酸インジ
ウムを中間生成物として製造した酸化インジウムの方が
著しく易解砕性であり、また仮焼して得られた酸化イン
ジウムの比表面積値も極めて高いことを見出し、本発明
をなすに至ったのである。Here, the present inventors use indium carbonate-based precipitates and indium hydroxide-based precipitates as bases to dry and calcine both precipitates to produce indium oxide. Comparing the characteristics, it was found that indium oxide produced by using indium carbonate as an intermediate product is remarkably easy to disintegrate, and the specific surface area value of indium oxide obtained by calcination is also extremely high. The invention was made.
【００２０】上記の対比として、沈殿剤としてアンモニ
ア水を使用し、インジウム濃度７０ｇ／ｌのインジウム
塩水溶液を液温４０〜６０℃に保持して反応させインジ
ウム化合物を沈殿生成させたところ得られた沈殿物は水
酸化インジウムを主体とする化合物であった。この沈殿
物を乾燥、仮焼して上記同様に酸化インジウムを製造せ
しめたところ、硬い塊状体となり、粉砕し難く、比表面
積値も極めて低く、上記のような良好な酸化インジウム
は得られなかった。In contrast to the above, ammonia water was used as a precipitant, and an indium salt aqueous solution having an indium concentration of 70 g / l was maintained at a liquid temperature of 40 to 60 ° C. to cause a reaction to cause precipitation of an indium compound, which was obtained. The precipitate was a compound mainly composed of indium hydroxide. When this precipitate was dried and calcined to produce indium oxide in the same manner as above, a hard lump was formed, which was difficult to pulverize, and the specific surface area value was extremely low, and thus good indium oxide as described above could not be obtained. .
【００２１】次に、中間生成物として炭酸インジウムを
生成させて（即ち、本発明法によって）焼成温度を変化
させ、種々の比表面積値を有する微粉末を製造した。こ
の酸化インジウム粉の比表面積値を２ｍ２／ｇから５５
ｍ２／ｇの範囲に設定し、これに酸化錫粉末を各々５重
量％となるように添加，混合した後、コールドプレスで
１インチ径のテストピースを成形圧１Ｔｏｎ／ｃｍ２の
条件で成形した後、１５００℃で６０分間焼結し、各比
表面積値の試料に対応するテストピースの相対密度を測
定した。その結果を図１に示す。Next, indium carbonate was produced as an intermediate product (that is, according to the method of the present invention) to change the firing temperature to produce fine powders having various specific surface area values. The specific surface area value of this indium oxide powder is from 2 m 2 / g to 55
After setting the range to m 2 / g, and adding and mixing tin oxide powder to each so as to be 5% by weight, a test piece with a diameter of 1 inch is molded by cold press at a molding pressure of 1 Ton / cm 2. After that, it was sintered at 1500 ° C. for 60 minutes, and the relative density of the test piece corresponding to the sample having each specific surface area value was measured. The result is shown in FIG.
【００２２】図１は、横軸に原料粉比表面積値（ｍ２／
ｇ）を，縦軸に焼結体相対密度（％）をとり、原料粉比
表面積値と焼結体相対密度との関係（１５００℃×６０
分間焼成）を示したグラフであり、○印は成形圧１Ｔｏ
ｎ／ｃｍ２，●印は成形圧１．５Ｔｏｎ／ｃｍ２，△印
は成形圧３．０Ｔｏｎ／ｃｍ２の場合を示したものであ
る。In FIG. 1, the horizontal axis represents the raw powder specific surface area value (m 2 /
g) and the relative density (%) of the sintered body on the vertical axis, and the relationship between the raw material powder specific surface area value and the relative density of the sintered body (1500 ° C. × 60
Is a graph showing (calcining for 1 minute), and ○ indicates a molding pressure of 1To.
n / cm 2 , ● indicates a molding pressure of 1.5 Ton / cm 2 , and Δ indicates a molding pressure of 3.0 Ton / cm 2 .
【００２３】ＩＴＯターゲッ卜として使用される際に、
相対密度が６０％以上、好ましくは７０％以上であるこ
とが必要であり、相対密度が６０％未満の場合は、消耗
速度が速く、また機械的強度が弱くて、使用時に熱衝撃
によって破壊し易く実用的でない。When used as an ITO target,
It is necessary that the relative density is 60% or more, preferably 70% or more. When the relative density is less than 60%, the wear rate is fast and the mechanical strength is weak, and the product is destroyed by thermal shock during use. Easy and not practical.
【００２４】本発明により供されるＩＴＯターゲット
は、図１からも解かるように、原料粉の比表面積値が１
０ｍ２／ｇ以上で成形圧が１Ｔｏｎ／ｃｍ２以上の場合
は、焼結体相対密度が６０％以上となってほぼ実用的と
なり、更に比表面積値が２０ｍ２／ｇ以上の範囲ではそ
の相対密度がほぼ７０％以上となり、更に３０ｍ２／ｇ
以上ではその相対密度が８０％を超え、条件によっては
相対密度９５％程度の高密度のターゲット材が得られる
のである。The ITO target provided by the present invention has a specific surface area value of the raw material powder of 1 as can be seen from FIG.
When the molding pressure is 0 m 2 / g or more and the pressure is 1 Ton / cm 2 or more, the relative density of the sintered body is 60% or more, which is almost practical, and when the specific surface area value is 20 m 2 / g or more, the relative Density is almost 70% or more, further 30m 2 / g
With the above, the relative density exceeds 80%, and depending on the conditions, a high-density target material having a relative density of about 95% can be obtained.
【００２５】上記のように、インジウム塩水溶液から酸
化インジウムを製造するに際して、中間生成物として炭
酸インジウム主体の沈殿物を生成させた後、洗浄，乾
燥，仮焼することにより、易解砕性の酸化インジウムを
製造することができる。従って、微粉砕処理が全く不要
で高密度の焼結体が得られ、しかも粉砕による汚染がな
いので高純度が保たれるのである。As described above, in the production of indium oxide from an indium salt aqueous solution, a precipitate mainly composed of indium carbonate is produced as an intermediate product, which is then washed, dried and calcined so that it can be easily disintegrated. Indium oxide can be produced. Therefore, fine pulverization is not necessary at all, a high-density sintered body can be obtained, and since there is no contamination due to pulverization, high purity is maintained.
【００２６】[0026]
【実施例】実施例１ 金属インジウム１０００ｇを硝酸で溶解させてｐＨ１．
０に調整した後、水を加えて１４ｌのインジウム塩水溶
液を作り、別に沈殿剤として重炭酸アンモニウム３２９
０ｇを準備し、該インジウム塩水溶液に液温が６０℃を
超えないように添加反応させて炭酸インジウムの沈殿を
生成させた。この沈殿を▲ろ▼別して水洗し１００℃で
乾燥した後、表１に示す仮焼温度（５００〜１１００
℃）で仮焼し、解砕した後、酸化錫微粉末（比表面積値
４ｍ２／ｇ）を各々５重量％になるように添加・混合し
た後、１〜３Ｔｏｎ／ｃｍ２の成形圧で成形し、１５０
０℃で６０分間焼成してＩＴＯの焼結体を試作した。ま
た、比較例として、沈殿剤としてアンモニア水（２８％
濃度）を使用し、その他の諸条件は上記の本実施例と同
様として粉体及びその焼結体を試作した。Example 1 1000 g of indium metal was dissolved in nitric acid to obtain a pH of 1.
After adjusting to 0, water was added to make 14 l of indium salt aqueous solution, and ammonium bicarbonate 329 was added as a precipitant.
0 g was prepared, and an indium carbonate aqueous solution was added and reacted so that the liquid temperature did not exceed 60 ° C. to generate a precipitate of indium carbonate. This precipitate was separated by filtration, washed with water and dried at 100 ° C., and then the calcination temperature shown in Table 1 (500 to 1100).
Calcination) and crushing, and then tin oxide fine powder (specific surface area value of 4 m 2 / g) was added and mixed so as to be 5% by weight respectively, and then at a molding pressure of 1 to 3 Ton / cm 2. Molded, 150
A sintered body of ITO was produced by firing at 0 ° C. for 60 minutes. In addition, as a comparative example, ammonia water (28%
Concentration and other conditions were the same as those in the above-described example, and a powder and a sintered body thereof were manufactured as a prototype.
【００２７】上記のようにして試作した本発明に係る焼
結体及び比較焼結体について焼結体相対密度を測定し
た。その結果を表１に示す。The relative density of the sintered bodies of the sintered body according to the present invention and the comparative sintered body produced as described above was measured. The results are shown in Table 1.
【００２８】[0028]
【表１】 [Table 1]
【００２９】表１の結果から解るように、仮焼温度９８
０℃以下で各成形圧（１〜３Ｔｏｎ／ｃｍ２）で試作し
た焼結体Ｎｏ．３〜Ｎｏ．６の焼結体相対密度は６０％
を超え、特にＮｏ．４〜Ｎｏ．６では相対密度７５％以
上となる。また、比較例Ｎｏ．７でも相対密度７０％程
度の焼結体は得られるが、本発明法に係るＮｏ．４，Ｎ
ｏ．５，Ｎｏ．６と比較するとはるかに劣り、相対密度
を向上させ難いことが解る。As can be seen from the results in Table 1, the calcination temperature is 98
Sintered body No. produced as a trial at each forming pressure (1 to 3 Ton / cm 2 ) at 0 ° C. or less. 3 to No. 6 has a relative density of 60%
, Especially No. 4 to No. In No. 6, the relative density is 75% or more. In addition, Comparative Example No. Even with No. 7, a sintered body having a relative density of about 70% can be obtained. 4, N
o. 5, No. It is understood that it is much inferior to that of No. 6, and it is difficult to improve the relative density.
【００３０】実施例２ 実施例１と同様にして硝酸インジウム溶液と重炭酸アン
モニウムを準備し、炭酸インジウム沈殿を生成させる場
合の反応温度（液温）を２０〜６５℃の範囲で変化させ
て炭酸インジウム沈殿を生成させ、これを水洗，乾燥し
た後、更に仮焼温度を５７０℃，６５０℃，７２０℃，
９００℃及び１０００℃と変化させて仮焼し解砕した
後、実施例１同様に酸化錫微粉末を添加，混合し、成形
圧３．０Ｔｏｎ／ｃｍ２で成形して１５００℃で６０分
間焼成し、ＩＴＯの焼結体を試作した。これら試作焼結
体の相対密度を測定し、炭酸インジウム湿式生成反応時
の反応温度と焼結体相対密度との関係を求めた。その結
果を図２に示す。Example 2 An indium nitrate solution and ammonium bicarbonate were prepared in the same manner as in Example 1, and the reaction temperature (liquid temperature) for producing the indium carbonate precipitate was changed within the range of 20 to 65 ° C. After the indium precipitate was generated, washed with water and dried, the calcination temperature was further changed to 570 ° C, 650 ° C, 720 ° C,
After calcination by changing the temperature to 900 ° C. and 1000 ° C. and crushing, tin oxide fine powder was added and mixed in the same manner as in Example 1, molded at a molding pressure of 3.0 Ton / cm 2 , and fired at 1500 ° C. for 60 minutes. Then, an ITO sintered body was manufactured as a prototype. The relative densities of these prototype sintered bodies were measured, and the relationship between the reaction temperature and the relative density of the sintered bodies during the wet formation reaction of indium carbonate was determined. The result is shown in FIG.
【００３１】図２は横軸に反応温度（℃）を、縦軸に焼
結体相対密度（％）をとり、仮焼温度別にプロットした
反応温度と焼結体相対密度との関係を示したグラフであ
り、口印は仮焼温度５７０℃，△印は仮焼温度６５０
℃，●印は仮焼温度７２０℃，〇印は仮焼温度９００
℃，▲印は仮焼温度１０００℃の場合の曲線である。In FIG. 2, the reaction temperature (° C.) is plotted on the horizontal axis and the relative density (%) of the sintered body is plotted on the vertical axis, and the relationship between the reaction temperature and the relative density of the sintered body plotted by calcination temperature is shown. It is a graph, the mark is calcination temperature 570 ° C, and the triangle is calcination temperature 650
℃, ● indicates calcination temperature 720 ℃, ○ indicates calcination temperature 900
℃, ▲ is a curve when the calcination temperature is 1000 ℃.
【００３２】図２から解るように、仮焼温度９００℃以
下の場合、反応温度を６０℃以下好ましくは３５〜６０
℃の範囲で炭酸インジウム沈殿を生成させることによ
り、得られた焼結体の相対密度はほぼ７０％以上とな
る。また、反応温度４０〜５５℃の範囲では相対密度７
５％以上となり、仮焼温度５５０〜７００℃の範囲で反
応温度４０〜５５℃の範囲では相対密度８５％以上とな
ることが解る。As can be seen from FIG. 2, when the calcination temperature is 900 ° C. or lower, the reaction temperature is 60 ° C. or lower, preferably 35 to 60.
By forming the indium carbonate precipitate in the range of ° C, the relative density of the obtained sintered body becomes approximately 70% or more. Further, in the reaction temperature range of 40 to 55 ° C., the relative density is 7
It can be seen that the relative density is 5% or more, and the relative density is 85% or more in the range of the calcination temperature of 550 to 700 ° C. and the reaction temperature of 40 to 55 ° C.
【００３３】[0033]
【発明の効果】本発明法によれば、酸化インジウムを湿
式反応を用いて合成するに際し、中間生成物として、水
酸化インジウムではなく、炭酸インジウムを生成させる
ことによって酸化インジウムの解砕性が著しく向上さ
れ、結果的に微粉砕工程がほとんど必要なく、常温加圧
成形−常圧焼結プロセスによってスパッタリングターゲ
ット用相対密度７０％以上の高密度焼結体が低コストで
製造することができるのである。According to the method of the present invention, when synthesizing indium oxide by a wet reaction, indium carbonate is produced as an intermediate product instead of indium hydroxide, so that the crushability of indium oxide is significantly increased. As a result, a high-density sintered body having a relative density of 70% or more for a sputtering target can be manufactured at low cost by a room temperature pressure molding-normal pressure sintering process, which requires almost no fine pulverization step. .
【００３４】また、本発明法によれば、到達相対密度が
高く、粉砕による汚染が防止できるので、高純度の高密
度焼結体を製造することができるのである。Further, according to the method of the present invention, since the reached relative density is high and contamination due to crushing can be prevented, a high-purity high-density sintered body can be manufactured.
【図１】原料粉比表面積と焼結体相対密度との関係を示
すグラフである。FIG. 1 is a graph showing a relationship between a specific surface area of raw material powder and a relative density of a sintered body.
【図２】反応温度と焼結体相対密度との関係を示すグラ
フである。FIG. 2 is a graph showing the relationship between reaction temperature and relative density of a sintered body.
Claims (3)
アルカリ，重炭酸アルカリのうちから選ばれる少なくと
も１種を加えて反応させた後、固液分離し、得られた沈
殿を乾燥，仮焼することを特徴とする比表面積２０ｍ２
／ｇ以上の酸化インジウム粉の製造方法。1. An indium salt aqueous solution at 60 ° C. or lower is added with at least one selected from an alkali carbonate and an alkali bicarbonate, and the mixture is reacted, followed by solid-liquid separation, and the obtained precipitate is dried and calcined. Specific surface area of 20 m 2
/ G or more of the method for producing indium oxide powder.
アルカリ，重炭酸アルカリのうちから選ばれる少なくと
も１種を加えて反応させた後、固液分離し、得られた沈
殿を乾燥，仮焼して得られた比表面積２０ｍ２／ｇ以上
の酸化インジウム粉８５〜９５重量％と酸化錫５〜１５
重量％とを混合してなることを特徴とする酸化錫添加酸
化インジウム粉の製造方法。2. At least one selected from an alkali carbonate and an alkali bicarbonate is added to an aqueous indium salt solution having a temperature of 60 ° C. or lower and reacted, followed by solid-liquid separation, and the obtained precipitate is dried and calcined. 85 to 95% by weight of indium oxide powder having a specific surface area of 20 m 2 / g or more and tin oxide of 5 to 15
A method for producing tin oxide-added indium oxide powder, characterized by being mixed with a weight percentage.
アルカリ，重炭酸アルカリのうちから選ばれる少なくと
も１種を加えて反応させた後、固液分離し、得られた沈
殿を乾燥，仮焼して得られた比表面積２０ｍ２／ｇ以上
の酸化インジウム粉８５〜９５重量％と酸化錫５〜１５
重量％とを混合後加圧成形し、焼成することを特徴とす
るスパッタリングターゲット用相対密度７０％以上の高
密度焼結体の製造方法。3. At least one selected from alkali carbonate and alkali bicarbonate is added to an aqueous solution of indium salt at 60 ° C. or lower to react, then solid-liquid separation is performed, and the obtained precipitate is dried and calcined. 85 to 95% by weight of indium oxide powder having a specific surface area of 20 m 2 / g or more and tin oxide of 5 to 15
A method for producing a high-density sintered body having a relative density of 70% or more for a sputtering target, characterized in that the mixture is mixed with 1% by weight and pressure-molded and fired.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2417890A JPH0742109B2 (en) | 1990-12-19 | 1990-12-19 | Method for producing indium oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2417890A JPH0742109B2 (en) | 1990-12-19 | 1990-12-19 | Method for producing indium oxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04219315A JPH04219315A (en) | 1992-08-10 |
| JPH0742109B2 true JPH0742109B2 (en) | 1995-05-10 |
Family
ID=18525904
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2417890A Expired - Lifetime JPH0742109B2 (en) | 1990-12-19 | 1990-12-19 | Method for producing indium oxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0742109B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL1004635C2 (en) * | 1995-12-06 | 1999-01-12 | Sumitomo Chemical Co | Indium oxide tin oxide powders and method of producing them. |
| DE102006015538A1 (en) * | 2006-03-31 | 2007-10-11 | H. C. Starck Gmbh & Co. Kg | Apparatus and process for the preparation of compounds by precipitation |
| WO2019051737A1 (en) * | 2017-09-14 | 2019-03-21 | 孟永辉 | Method for preparing high-purity nano-tin dioxide spherical powder |
| CN115482965A (en) * | 2022-09-16 | 2022-12-16 | 北京高压科学研究中心 | Method for improving conductivity of transparent conductive oxide and blue light filtering efficiency |
-
1990
- 1990-12-19 JP JP2417890A patent/JPH0742109B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04219315A (en) | 1992-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4992003B2 (en) | Method for producing metal oxide fine particles | |
| TWI401211B (en) | Indium oxide powder and method for producing same | |
| CA2221825C (en) | Spheroidally agglomerated basic cobalt (ii) carbonate and spheroidally agglomerated cobalt (ii) hydroxide, process for their production and their use | |
| JPS638260A (en) | Praparation of zirconia mixture and zirconia mixture thereby | |
| JPH0472774B2 (en) | ||
| US5866493A (en) | Method of manufacturing a sintered body of indium tin oxide | |
| JPH0457613B2 (en) | ||
| JP3314388B2 (en) | Method for producing indium hydroxide, indium oxide and ITO sintered body | |
| JPH0137331B2 (en) | ||
| JPH0742109B2 (en) | Method for producing indium oxide powder | |
| JPH0624977B2 (en) | Needle-shaped titanium dioxide and method for producing the same | |
| JP2843909B2 (en) | Method for producing yttrium oxide transparent sintered body | |
| JPS62297215A (en) | Method for controlling crystal particle diameter of uo2 pellet | |
| JPH0238527B2 (en) | ||
| JPS6235970B2 (en) | ||
| JPS61122121A (en) | Production of rare earth metal oxide powder | |
| JPS6212009A (en) | Formation of indium oxide based low resistance transparent thin film | |
| JP2002255656A (en) | Method for producing nano-crystal grain dense sintered body | |
| KR101324130B1 (en) | Indium tin oxide powder and manufacturing method of producing the same | |
| JPS61251517A (en) | Production of perovskite type oxide | |
| JP2000119023A (en) | Production of bismuth(iii) oxide | |
| JPS5826894A (en) | Preparation of fine powder of cobalt oxalate | |
| JPH0678190B2 (en) | Method for producing zirconium titanate-based ceramics | |
| JPS63112450A (en) | Manufacture of high density perovskite sintered body | |
| JP3052461B2 (en) | Manufacturing method of magnetic powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080510 Year of fee payment: 13 |
|
| S111 | Request for change of ownership or part of ownership |
Free format text: JAPANESE INTERMEDIATE CODE: R313115 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080510 Year of fee payment: 13 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090510 Year of fee payment: 14 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090510 Year of fee payment: 14 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100510 Year of fee payment: 15 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110510 Year of fee payment: 16 |
|
| EXPY | Cancellation because of completion of term | ||
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110510 Year of fee payment: 16 |