JPH1017324A - Production of indium oxide power - Google Patents
Production of indium oxide powerInfo
- Publication number
- JPH1017324A JPH1017324A JP16992196A JP16992196A JPH1017324A JP H1017324 A JPH1017324 A JP H1017324A JP 16992196 A JP16992196 A JP 16992196A JP 16992196 A JP16992196 A JP 16992196A JP H1017324 A JPH1017324 A JP H1017324A
- Authority
- JP
- Japan
- Prior art keywords
- indium oxide
- indium
- powder
- oxide powder
- suspension
- 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.)
- Withdrawn
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、水熱合成処理を施
すことにより得られる高密度ＩＴＯターゲットの原料と
なる酸化インジウム粉末に関する。[0001] The present invention relates to an indium oxide powder used as a raw material for a high-density ITO target obtained by performing a hydrothermal synthesis treatment.
【０００２】[0002]
【従来の技術】近年、液晶ディスプレイを中心としたフ
ラットパネルディスプレイの使用が急速に拡大してお
り、現在、この透明導電膜としてはＩＴＯ膜が最も使用
されている。ＩＴＯ膜の製造方法としては、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法等
の物理的製法が知られているが、操作性の簡便さや得ら
れる膜特性が良好である等の理由からＩＴＯターゲット
を用いたスパッタリング法が広く適用されている。特
に、最近ではカラー液晶の普及によるＴＦＴ方式の採用
により、高性能なＩＴＯ膜をより低温で成膜することが
要求されている。2. Description of the Related Art In recent years, the use of flat panel displays, mainly liquid crystal displays, has been rapidly expanding. At present, ITO films are most used as the transparent conductive film. As a method for producing an ITO film, a chemical production method such as a spray method or a coating method, and a physical production method such as a vacuum evaporation method or a sputtering method are known, but the operability is simple and the obtained film characteristics are good. For these reasons, a sputtering method using an ITO target has been widely applied. In particular, recently, with the adoption of the TFT method due to the spread of color liquid crystals, it has been required to form a high-performance ITO film at a lower temperature.
【０００３】このような要求を満足させるためには、Ｉ
ＴＯターゲットを高密度化すれば良いことが知られてい
る。In order to satisfy such demands, I
It is known that the density of the TO target should be increased.
【０００４】ところで、ＩＴＯターゲットは、通常、酸
化インジウム粉末と酸化錫粉末の混合粉末や前記混合粉
末を焼成して得られるインジウム錫複合酸化物粉末（Ｉ
ＴＯ粉末）を加圧成形後、焼結して製造されている。酸
化インジウム粉末の製造方法としては、最も一般的な中
和法の他、電解法（特開平６−１７１９３７）や炭酸塩
法（特開平４−２１９３１５、特開平７−４２１０９）
が知られており、通常これらの方法によって得られた水
酸化インジウム粉末を焼成して得られる。[0004] The ITO target is usually made of a mixed powder of indium oxide powder and tin oxide powder or an indium tin composite oxide powder (I) obtained by firing the mixed powder.
It is manufactured by press molding and sintering (TO powder). As a method for producing indium oxide powder, in addition to the most common neutralization method, an electrolytic method (JP-A-6-171937) and a carbonate method (JP-A-4-219315, JP-A-7-42109)
Is generally obtained by calcining the indium hydroxide powder obtained by these methods.
【０００５】しかしながら、ＩＴＯは難焼結性材料であ
り、これらの粉末を原料として加圧成形後、焼結して
も、その密度を上げることは困難であった。また、ＩＴ
Ｏ焼結体の密度と原料である酸化インジウム粉末の平均
結晶子径との間の相関については、何ら知られていなか
った。However, ITO is a material that is difficult to sinter, and it is difficult to increase the density of these powders even if they are pressed and then sintered. Also, IT
No correlation has been known between the density of the O-sintered body and the average crystallite size of the indium oxide powder as the raw material.
【０００６】[0006]
【発明が解決しようとする課題】本発明の目的は、原料
の一部として用いて焼結すると高密度なＩＴＯ焼結体に
なる酸化インジウム粉末の製造方法を提供することであ
る。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing indium oxide powder which becomes a high-density ITO sintered body when used as a part of a raw material and sintered.
【０００７】[0007]
【課題を解決するための手段】本発明者らは、鋭意検討
の結果、上記目的が、水酸化インジウム粉末を酸又はア
ルカリによって水熱処理することにより得られることを
見いだした。ここに、本発明は次の通りである。Means for Solving the Problems As a result of diligent studies, the present inventors have found that the above object can be obtained by hydrothermally treating indium hydroxide powder with an acid or an alkali. Here, the present invention is as follows.
【０００８】（１）水酸化インジウム粉末を、酸性懸濁
液を用いて水熱処理した後、仮焼することにより得られ
る酸化インジウム粉末の製造方法。 （２）塩酸、硝酸、硫酸、蓚酸のうち１種又は２種以上
を使用し、ｐＨが２以上６以下の酸性懸濁液を用いるこ
とを特徴とする上記（１）記載の製造方法。 （３）水酸化インジウム粉末を、アルカリ性懸濁液を用
いて水熱処理した後、仮焼することにより得られる酸化
インジウム粉末の製造方法。 （４）水酸化ナトリウム、水酸化カリウム、水酸化カル
シウム、アンモニア水のうち１種又は２種以上を使用
し、ｐＨが９以上１３以下のアルカリ性懸濁液を用いる
ことを特徴とする上記（３）記載の製造方法。 （５）圧力２〜１５０ｋｇｆ／ｃｍ2 、温度８０〜３０
０℃で水熱処理することを特徴とする上記（１）ないし
（４）記載の製造方法。 （６）酸化インジウム粉末が、ＢＥＴ比表面積１０ｍ2
／ｇ以下、平均結晶子９０ｎｍ以上、二次粒子のピーク
粒径、平均粒径がともに３μｍ以下であることを特徴と
する上記（１）ないし（５）記載の製造方法。(1) A method for producing an indium oxide powder obtained by subjecting an indium hydroxide powder to hydrothermal treatment using an acidic suspension and then calcining. (2) The method according to (1), wherein one or more of hydrochloric acid, nitric acid, sulfuric acid, and oxalic acid are used, and an acidic suspension having a pH of 2 to 6 is used. (3) A method for producing indium oxide powder obtained by subjecting indium hydroxide powder to hydrothermal treatment using an alkaline suspension and then calcining. (4) The above-mentioned (3), wherein one or more of sodium hydroxide, potassium hydroxide, calcium hydroxide and aqueous ammonia are used, and an alkaline suspension having a pH of 9 to 13 is used. ). (5) Pressure 2-150 kgf / cm 2 , temperature 80-30
The method according to any one of the above (1) to (4), wherein a hydrothermal treatment is performed at 0 ° C. (6) The indium oxide powder has a BET specific surface area of 10 m 2
/ G, an average crystallite of 90 nm or more, a peak particle diameter of secondary particles, and an average particle diameter of 3 μm or less.
【０００９】[0009]
【発明の実施の形態】本発明の請求項１ないし６におけ
る水熱処理に用いられる水酸化インジウム粉末は中和法
や電解法等によって得ることができる。特に、粒径や純
度は限定されないが、望ましくは、平均粒径０．０５〜
１μｍ、純度９９．９９％以上のものが良い。BEST MODE FOR CARRYING OUT THE INVENTION The indium hydroxide powder used in the hydrothermal treatment according to claims 1 to 6 of the present invention can be obtained by a neutralization method, an electrolytic method or the like. In particular, the particle size and purity are not limited, but desirably, the average particle size is 0.05 to
Those having a thickness of 1 μm and a purity of 99.99% or more are preferred.
【００１０】また、本発明で用いられる酸性懸濁液を作
製するのに用いられる酸は特に限定されないが、水酸イ
オンを一部溶解させるという理由から、好ましくは、塩
酸、硝酸、硫酸、蓚酸のうち１種又は２種以上が良く、
更に、好ましくは硝酸が良い。また、酸性懸濁液のｐＨ
も限定されないが、２以上６以下が好ましく、更に好ま
しくは３以上４以下が良い。ｐＨが２未満であるとイン
ジウムが過剰に溶解し歩留まりが悪くなり、６を越える
と溶解しにくく結晶の生長が起こりにくいからである。The acid used for preparing the acidic suspension used in the present invention is not particularly limited, but is preferably hydrochloric acid, nitric acid, sulfuric acid, oxalic acid, for partially dissolving the hydroxide ions. One or more of them are good,
Further, nitric acid is preferred. Also, the pH of the acidic suspension
Although not limited, it is preferably 2 or more and 6 or less, and more preferably 3 or more and 4 or less. If the pH is less than 2, indium is excessively dissolved and the yield is deteriorated. If the pH is more than 6, it is difficult to dissolve and the growth of crystals is less likely to occur.
【００１１】また、本発明で用いられるアルカリ性懸濁
液を作製するのに用いられるアルカリは特に限定されな
いが、可溶性の錯体を形成させるという理由から、好ま
しくは、水酸化ナトリウム、水酸化カリウム、水酸化カ
ルシウム、アンモニア水のうち１種又は２種以上が良
く、更に、好ましくはアンモニア水が良い。また、アル
カリ性懸濁液のｐＨも限定されないが、９以上１３以下
が好ましく、更に好ましくは１０以上１２以下が良い。
ｐＨが９未満であるとインジウム錯体を形成しにくく溶
解しずらいため結晶成長が起こりにくいからであり、１
３を越えると試薬を大量に使うので経済的ではないから
である。The alkali used for preparing the alkaline suspension used in the present invention is not particularly limited, but is preferably sodium hydroxide, potassium hydroxide, water, or the like for forming a soluble complex. One or more of calcium oxide and aqueous ammonia are preferred, and more preferably, aqueous ammonia is preferred. The pH of the alkaline suspension is not limited, but is preferably 9 or more and 13 or less, and more preferably 10 or more and 12 or less.
If the pH is less than 9, it is difficult to form an indium complex and it is difficult to dissolve, so that crystal growth does not easily occur.
If it exceeds 3, it is not economical because a large amount of reagent is used.
【００１２】本発明の請求項１ないし６で行われる水熱
処理は、密閉容器からなるオートクレーブを用いて行う
ことができる。その際、撹拌は行っても行わなくても良
いが、望ましくは行った方が良い。The hydrothermal treatment performed in the first to sixth aspects of the present invention can be performed using an autoclave comprising a closed vessel. At this time, stirring may or may not be performed, but desirably is performed.
【００１３】水熱処理時の懸濁液の圧力や温度は特に限
定されないが、好ましくは、圧力２〜１５０ｋｇｆ／ｃ
ｍ2 、温度８０〜３００℃が良く、更に好ましくは、圧
力８０〜１００ｋｇｆ／ｃｍ2 、温度２００〜２５０℃
が良い。圧力が２ｋｇｆ／ｃｍ2 未満だとインジウムが
溶解しにくく生長しずらいからであり、１５０ｋｇｆ／
ｃｍ2 を越えると装置が大がかりとなり高コストとなる
からであり、また、温度が８０℃未満だと結晶生長が起
こりにくいからであり、３００℃を越えると耐熱材料の
選定が困難となるからである。反応時間は、上記圧力、
温度の条件下で約１０〜１００時間が適当である。ま
た、懸濁液における粉末の懸濁液全体に占める重量比
は、２０〜６０％が適当である。The pressure and temperature of the suspension during the hydrothermal treatment are not particularly limited, but are preferably 2 to 150 kgf / c.
m 2 , temperature 80-300 ° C., more preferably, pressure 80-100 kgf / cm 2 , temperature 200-250 ° C.
Is good. If the pressure is less than 2 kgf / cm 2 , it is difficult for indium to dissolve and it is difficult to grow.
is because exceeding cm 2 and the device becomes expensive becomes bulky, also, is because temperature is less than 80 ° C. hardly occurs crystal growth, because it exceeds 300 ° C. is selected refractory material is difficult is there. The reaction time is the above pressure,
About 10 to 100 hours under temperature conditions are suitable. The weight ratio of the powder to the entire suspension in the suspension is suitably from 20 to 60%.
【００１４】水熱処理後、通常は、デカンテーションに
より洗浄後ろ過し、乾燥工程を経るというプロセスの
後、仮焼を行う。尚、乾燥は通常８０〜１２０℃の温度
で行う。[0014] After the hydrothermal treatment, usually, after washing by decantation, filtration, and a drying step, calcination is performed. The drying is usually performed at a temperature of 80 to 120 ° C.
【００１５】本発明の請求項１ないし６で行われる仮焼
は、真空中、大気中、酸素ガス中等の雰囲気で行うこと
ができるが、安価に酸化物にするという理由から大気雰
囲気が最も好ましい。また、仮焼温度は５００〜１２０
０℃で行うことができ、好ましくは７００〜１０００℃
が良い。仮焼時間は、上記雰囲気、温度の条件下で約１
〜５時間が適当である。The calcination according to the first to sixth aspects of the present invention can be performed in an atmosphere such as vacuum, air, or oxygen gas. However, an air atmosphere is most preferable because oxides can be produced at low cost. . The calcination temperature is 500-120.
0 ° C., preferably 700-1000 ° C.
Is good. The calcination time is about 1 under the above atmosphere and temperature conditions.
~ 5 hours is appropriate.
【００１６】仮焼して得られる酸化インジウム粉末の粒
径は特に限定されないが、酸化錫との混合性を向上させ
るには分散性が必要であることから、好ましくは二次粒
子の平均粒径０．５〜５μｍであり、更に好ましくは平
均粒径０．９〜２μｍが良い。The particle size of the indium oxide powder obtained by calcination is not particularly limited, but the average particle size of the secondary particles is preferably used because dispersibility is required to improve the mixing property with tin oxide. The average particle diameter is preferably 0.5 to 5 μm, more preferably 0.9 to 2 μm.
【００１７】本発明の特徴の１つは、水酸化インジウム
粉末をオートクレーブ等を用いて、水熱処理を行い水酸
化インジウムを再結晶化させ、その後、仮焼すると平均
結晶子径が大きく焼結の少ない酸化インジウム粉末を得
ることができ、このような平均結晶子径の大きい酸化イ
ンジウム粉末を酸化錫粉末と混合し焼結すると得られる
焼結体が高密度化するという新たな知見に基づく技術的
思想にある。水熱処理を行うと平均結晶子径が大きくな
るのは、中和法等による水酸化インジウム粉末に、加圧
・高熱処理を行うことにより、粒子が再溶解しながら再
結晶化するため結晶生長が起こり、一次粒子内の結晶子
が生長するためである。また、平均結晶子径が大きい酸
化インジウム粉末を原料の一部として用いて焼結すると
高密度化が図られるのは、一次粒子がしまっており、真
密度が大きく、しかも二次粒子が生長しずらく、分散性
が良いためである。One of the features of the present invention is that the indium hydroxide powder is subjected to hydrothermal treatment using an autoclave or the like to recrystallize the indium hydroxide, and then, when calcined, the average crystallite diameter becomes large and the sintering becomes difficult. It is possible to obtain a small amount of indium oxide powder, a technical technology based on the new knowledge that when the indium oxide powder having such a large average crystallite diameter is mixed with tin oxide powder and sintered, the resulting sintered body has a high density. In thought. The average crystallite diameter increases when hydrothermal treatment is performed, because the particles are recrystallized while re-dissolving the particles by applying pressure and high heat treatment to indium hydroxide powder by a neutralization method, etc. This occurs because crystallites in the primary particles grow. When indium oxide powder having a large average crystallite diameter is used as a part of the raw material and sintered, a high density is achieved because the primary particles are closed, the true density is large, and the secondary particles grow. This is because the dispersibility is good.
【００１８】また、本発明で得られる酸化インジウム粉
末は、容易に高密度化できるという点から、（６）に記
載されている通り、ＢＥＴ比表面積１０ｍ2 ／ｇ以下、
平均結晶子径９０ｎｍ以上、二次粒子のピーク粒径、平
均粒径がともに３μｍ以下が好ましく、更に好ましく
は、ＢＥＴ比表面積８ｍ2 ／ｇ以下、平均結晶子径１０
０ｎｍ以上、二次粒子のピーク粒径が１．５μｍ以下、
二次粒子の平均粒径が２μｍ以下が良い。ここで、平均
結晶子径は、Ｘ線回折法に基づき回折線のピークの幅か
ら理論的に計算して求めることができる。例えば、平均
結晶子径が大きいと回折ピークが高くなり、又幅は狭く
なって、鋭い明確なピークが現れる。また、二次粒子の
ピーク粒径とは、レーザー分光法、沈降法等で測定した
粒径と重量分布の最大集団により定義される値のことで
ある。また、二次粒子の平均粒径は、例えばマイクロト
ラック法等のレーザー分光法によって測定することがで
きる。ここで、二次粒子とは一次粒子の凝集により形成
される粒子のことをいう。ＢＥＴ比表面積とは、ＢＥＴ
法により測定される単位重量あたりの粒子の表面積のこ
とである。Further, the indium oxide powder obtained by the present invention can be easily densified, and therefore, as described in (6), has a BET specific surface area of 10 m 2 / g or less.
The average crystallite diameter is preferably 90 nm or more, the peak particle diameter of the secondary particles and the average particle diameter are both preferably 3 μm or less, more preferably 8 m 2 / g or less of BET specific surface area, and the average crystallite diameter is
0 nm or more, the peak particle size of the secondary particles is 1.5 μm or less,
The average particle size of the secondary particles is preferably 2 μm or less. Here, the average crystallite diameter can be theoretically calculated from the peak width of the diffraction line based on the X-ray diffraction method. For example, when the average crystallite diameter is large, the diffraction peak becomes high and the width becomes narrow, and a sharp and clear peak appears. The peak particle diameter of the secondary particles is a value defined by the particle diameter measured by laser spectroscopy, sedimentation method, and the like and the maximum population of the weight distribution. The average particle size of the secondary particles can be measured by, for example, laser spectroscopy such as a microtrack method. Here, the secondary particles refer to particles formed by aggregation of the primary particles. BET specific surface area is BET
It is the surface area of the particles per unit weight measured by the method.
【００１９】以下に、実施例及び比較例を記載する。
尚、本発明は本実施例に拘泥されるものではない。Hereinafter, Examples and Comparative Examples will be described.
The present invention is not limited to the present embodiment.
【００２０】[0020]
実施例１ 金属インジウムを硝酸で溶解した後、アンモニア水で加
水分解反応を行って得た水酸化インジウム粉末を原料と
して５００ｇ用いて、容積５ｌのオートクレーブにて、
１０ｇの硫酸溶液を用いｐＨ３．０に調整し温度２２０
℃、圧力３０ｋｇｆ／ｃｍ2 で２０時間、６０ｒｐｍで
撹拌させながら水熱処理を行った。しかる後、大気雰囲
気中で８００℃で５時間仮焼を行った。このようにして
得られた酸化インジウム粉末の平均結晶子径をＸ線回折
法を用いて測定すると８０ｎｍであり、二次粒子の平均
粒径をマイクロトラック法で測定すると２．０μｍであ
った。また、ＢＥＴ比表面積は９．５ｍ2 ／ｇであり、
二次粒子のピーク粒径は０．９μｍであった。この粉末
９０ｇを、平均粒径１０μｍの酸化錫粉末１０ｇとボー
ルミル法にて２４時間混合して、酸化インジウム−酸化
錫混合粉末を得た。この混合粉末７０ｇを原料として用
い、１ｔｆ／ｃｍ2 でプレス成形し、酸素雰囲気中にて
１６００℃で３時間焼結を行った。その結果得られたＩ
ＴＯ焼結体の密度をピクノメーター真比重計測法で測定
すると相対密度９５％であった。この結果を表１に示し
た。Example 1 After dissolving metal indium with nitric acid, a hydrolysis reaction was performed with ammonia water, and 500 g of indium hydroxide powder obtained as a raw material was used in a 5-liter autoclave.
The pH was adjusted to 3.0 using 10 g of sulfuric acid solution and the temperature was adjusted to 220.
The hydrothermal treatment was performed while stirring at 60 rpm for 20 hours at 30 ° C. and a pressure of 30 kgf / cm 2 . Thereafter, calcination was performed at 800 ° C. for 5 hours in the air atmosphere. The average crystallite diameter of the indium oxide powder thus obtained was 80 nm when measured by an X-ray diffraction method, and the average particle diameter of the secondary particles was 2.0 μm when measured by a microtrack method. The BET specific surface area is 9.5 m 2 / g,
The peak particle size of the secondary particles was 0.9 μm. 90 g of this powder was mixed with 10 g of tin oxide powder having an average particle size of 10 μm by a ball mill for 24 hours to obtain an indium oxide-tin oxide mixed powder. Using 70 g of the mixed powder as a raw material, the mixture was press-molded at 1 tf / cm 2 and sintered at 1600 ° C. for 3 hours in an oxygen atmosphere. The resulting I
When the density of the TO sintered body was measured by a true pycnometer specific gravity measurement method, the relative density was 95%. The results are shown in Table 1.
【００２１】[0021]
【表１】 [Table 1]
【００２２】実施例２〜５ 水熱処理時に酸性又はアルカリ性にするための添加媒
質、同じく水熱処理時のｐＨ、温度、圧力、及び仮焼時
の焼成温度を表１のように変えた他は実施例１と同様に
してＩＴＯ焼結体を製造し得られた焼結体の密度、及び
仮焼後の酸化インジウム粉末の平均結晶子径等を実施例
１と同様に測定した。この結果を表１に示した。Examples 2 to 5 Except that the addition medium for making it acidic or alkaline during hydrothermal treatment, and the pH, temperature and pressure during hydrothermal treatment and the calcination temperature during calcination were changed as shown in Table 1, The density of the sintered body obtained by manufacturing the ITO sintered body in the same manner as in Example 1, and the average crystallite diameter of the indium oxide powder after calcination were measured in the same manner as in Example 1. The results are shown in Table 1.
【００２３】実施例６ 金属インジウムを陽極とし、硝酸アンモニウムを電解液
として電流密度７００Ａ／ｍ2 、電解液濃度１モル／ｌ
で電解を行う陽極酸化法にて得た水酸化インジウム粉末
を原料として５００ｇ用いて、容積５ｌのオートクレー
ブにて、２５ｇの塩酸溶液を用いｐＨ２．８に調整し温
度３３０℃、圧力１５０ｋｇｆ／ｃｍ2で２０時間、５
０ｒｐｍで撹拌させながら水熱処理を行った。しかる
後、空気雰囲気中で７００℃で４時間仮焼を行った。こ
のようにして得られた酸化インジウム粉末の平均結晶子
径をＸ線回折法を用いて測定すると１０８ｎｍであり、
二次粒子の平均粒径をマイクロトラック法で測定すると
０．６μｍであった。また、ＢＥＴ比表面積は９．８ｍ
2 ／ｇであり、二次粒子のピーク粒径は１．０μｍであ
った。この粉末９０ｇを、平均粒径１０μｍの酸化錫粉
末１０ｇとボールミル法にて２４時間混合して、酸化イ
ンジウム−酸化錫混合粉末を得た。この混合粉末７０ｇ
を原料として用い、１ｔｆ／ｃｍ2 でプレス成形し、酸
素雰囲気中にて１６００℃で３時間焼結を行った。その
結果得られたＩＴＯ焼結体の密度を比重ビン法で測定す
ると相対密度９８％であった。この結果を表１に示し
た。Example 6 A current density of 700 A / m 2 , an electrolyte concentration of 1 mol / l, using metal indium as an anode and ammonium nitrate as an electrolyte.
Using 500 g of indium hydroxide powder obtained by the anodizing method as a raw material, the pH was adjusted to 2.8 using a 25 g hydrochloric acid solution in a 5 L autoclave, and the temperature was 330 ° C. and the pressure was 150 kgf / cm 2. 20 hours at 5
The hydrothermal treatment was performed while stirring at 0 rpm. Thereafter, calcination was performed at 700 ° C. for 4 hours in an air atmosphere. The average crystallite diameter of the indium oxide powder thus obtained was 108 nm when measured using an X-ray diffraction method.
The average particle size of the secondary particles was 0.6 μm as measured by the microtrack method. The BET specific surface area is 9.8m
2 / g, and the peak particle diameter of the secondary particles was 1.0 μm. 90 g of this powder was mixed with 10 g of tin oxide powder having an average particle size of 10 μm by a ball mill for 24 hours to obtain an indium oxide-tin oxide mixed powder. 70 g of this mixed powder
Was press-formed at 1 tf / cm 2 and sintered at 1600 ° C. for 3 hours in an oxygen atmosphere. When the density of the resulting ITO sintered body was measured by the specific gravity bin method, the relative density was 98%. The results are shown in Table 1.
【００２４】実施例７〜１０ 水熱処理時に酸性又はアルカリ性にするための添加媒
質、同じく水熱処理時のｐＨ、温度、圧力、及び仮焼時
の焼成温度を表２のように変えた他は実施例６と同様に
してＩＴＯ焼結体を製造し得られた焼結体の密度、及び
仮焼後の酸化インジウム粉末の平均粒径及び平均結晶子
径等を実施例６と同様に測定した。この結果を表２に示
した。Examples 7 to 10 Except that the additive medium for making it acidic or alkaline at the time of hydrothermal treatment, and the pH, temperature and pressure during hydrothermal treatment and the calcination temperature during calcination were changed as shown in Table 2, The density of the sintered body obtained by manufacturing an ITO sintered body in the same manner as in Example 6, and the average particle diameter and average crystallite diameter of the calcined indium oxide powder were measured in the same manner as in Example 6. The results are shown in Table 2.
【００２５】[0025]
【表２】 [Table 2]
【００２６】実施例１１ 実施例１〜１０で得られたＩＴＯ焼結体をターゲットと
して用いてＤＣマグネトロンスパッタリング法で成膜を
行ったところ、ショートの原因となるノジュールが発生
せず、長時間にわたって安定な導電性薄膜が得られた。Example 11 A film was formed by a DC magnetron sputtering method using the ITO sintered body obtained in Examples 1 to 10 as a target. A stable conductive thin film was obtained.
【００２７】比較例１ 実施例１〜５で用いた水酸化インジウムと同じ水酸化イ
ンジウム粉末を用いて、水熱処理を行わずに、即仮焼を
行った他は実施例１と同じ工程を径て得たＩＴＯ焼結体
の密度、及び仮焼後の酸化インジウム粉末の平均結晶子
径等を実施例１と同様に測定した。この結果を表２に併
せて示した。Comparative Example 1 The same process as in Example 1 was carried out except that the same indium hydroxide powder as used in Examples 1 to 5 was used and calcined immediately without performing hydrothermal treatment. The density of the obtained ITO sintered body, the average crystallite diameter of the indium oxide powder after calcination, and the like were measured in the same manner as in Example 1. The results are shown in Table 2.
【００２８】比較例２ 実施例６〜１０で用いた水酸化インジウムと同じ水酸化
インジウム粉末を用いて、水熱処理を行わずに、即仮焼
を行った他は実施例６と同じ工程を経て得たＩＴＯ焼結
体の密度、及び仮焼後の酸化インジウム粉末の平均結晶
子径等を実施例１と同様に測定した。この結果を表２に
併せて示した。Comparative Example 2 The same indium hydroxide powder as indium hydroxide used in Examples 6 to 10 was used, except that it was calcined immediately without hydrothermal treatment, but through the same steps as in Example 6. The density of the obtained ITO sintered body, the average crystallite diameter of the indium oxide powder after calcination, and the like were measured in the same manner as in Example 1. The results are shown in Table 2.
【００２９】比較例３ 比較例１〜２で得られたＩＴＯ焼結体をターゲットとし
て用いてＤＣマグネトロンスパッタリング法で成膜を行
ったところ、ショートの原因となるノジュールが多く発
生し、得られた膜の導電特性も悪かった。Comparative Example 3 When a film was formed by a DC magnetron sputtering method using the ITO sintered body obtained in Comparative Examples 1 and 2 as a target, a number of nodules causing a short circuit were generated, and the obtained film was obtained. The conductive properties of the film were also poor.
【００３０】以上により、本実施例のＩＴＯ焼結体はい
ずれも密度が９０％以上であり、高特性であることがあ
きらかである。As described above, all of the ITO sintered bodies of the present embodiment have a density of 90% or more and clearly have high characteristics.
【００３１】[0031]
【発明の効果】表１から明らかなように、本発明の酸化
インジウム粉末を用いると、容易に、スパッタリング特
性等に優れた高性能な高密度ＩＴＯ焼結体が得られる。As is clear from Table 1, when the indium oxide powder of the present invention is used, a high-performance high-density ITO sintered body excellent in sputtering characteristics and the like can be easily obtained.
Claims (6)
いて水熱処理した後、仮焼することにより得られる酸化
インジウム粉末の製造方法。1. A method for producing an indium oxide powder obtained by subjecting an indium hydroxide powder to hydrothermal treatment using an acidic suspension and then calcining it.
種以上を使用し、ｐＨが２以上６以下の酸性懸濁液を用
いることを特徴とする請求項１記載の製造方法。2. One or two of hydrochloric acid, nitric acid, sulfuric acid and oxalic acid.
The method according to claim 1, wherein an acidic suspension having a pH of 2 or more and 6 or less is used.
液を用いて水熱処理した後、仮焼することにより得られ
る酸化インジウム粉末の製造方法。3. A method for producing an indium oxide powder obtained by subjecting an indium hydroxide powder to a hydrothermal treatment using an alkaline suspension and then calcining.
化カルシウム、アンモニア水のうち１種又は２種以上を
使用し、ｐＨが９以上１３以下のアルカリ性懸濁液を用
いることを特徴とする請求項３記載の製造方法。4. The method according to claim 1, wherein one or more of sodium hydroxide, potassium hydroxide, calcium hydroxide and aqueous ammonia is used, and an alkaline suspension having a pH of 9 to 13 is used. Item 3. The production method according to Item 3.
〜３００℃で水熱処理することを特徴とする請求項１な
いし４記載の製造方法。5. A pressure of 2 to 150 kgf / cm 2 and a temperature of 80.
The method according to any one of claims 1 to 4, wherein a hydrothermal treatment is performed at a temperature of 300 to 300 ° C.
０ｍ2 ／ｇ以下、平均結晶子径９０ｎｍ以上、二次粒子
のピーク粒径、平均粒径がともに３μｍ以下であること
を特徴とする請求項１ないし５記載の製造方法。6. An indium oxide powder having a BET specific surface area of 1
0 m 2 / g or less, an average crystallite size 90nm or more, the peak particle diameter of the secondary particles, the production method of claims 1 to 5, wherein the average particle diameter of both 3μm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16992196A JPH1017324A (en) | 1996-06-28 | 1996-06-28 | Production of indium oxide power |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16992196A JPH1017324A (en) | 1996-06-28 | 1996-06-28 | Production of indium oxide power |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH1017324A true JPH1017324A (en) | 1998-01-20 |
Family
ID=15895427
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16992196A Withdrawn JPH1017324A (en) | 1996-06-28 | 1996-06-28 | Production of indium oxide power |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH1017324A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100474846B1 (en) * | 2002-03-22 | 2005-03-09 | 삼성코닝 주식회사 | Indium oxide powder, manufacturing method thereof, and manufacturing method of high density indium tin oxide target using the same |
| US7799312B2 (en) | 2002-03-22 | 2010-09-21 | Samsung Corning Precision Glass Co., Ltd. | Method for manufacturing high-density indium tin oxide target, methods for preparing tin oxide powder and indium oxide powder used therefor |
| KR100993171B1 (en) | 2008-08-27 | 2010-11-09 | 고려대학교 산학협력단 | Gas sensor using nano-porous indium oxide spherical structure and fabrication method thereof |
| CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
| JP2017047353A (en) * | 2015-08-31 | 2017-03-09 | パナソニックＩｐマネジメント株式会社 | Method for recovering indium |
| CN106732517A (en) * | 2016-11-28 | 2017-05-31 | 青岛科技大学 | A kind of preparation method of the indium hydroxide photochemical catalyst with regular cube structure |
| JP2020066566A (en) * | 2018-10-26 | 2020-04-30 | 株式会社アルバック | Manufacturing method of indium oxide powder |
| JP2020066565A (en) * | 2018-10-26 | 2020-04-30 | 株式会社アルバック | Manufacturing method of indium oxide powder |
| JP2021138594A (en) * | 2020-03-06 | 2021-09-16 | ▲鄭▼州大学 | Preparation method of indium oxide spherical powder capable of controllable grain shape |
-
1996
- 1996-06-28 JP JP16992196A patent/JPH1017324A/en not_active Withdrawn
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100474846B1 (en) * | 2002-03-22 | 2005-03-09 | 삼성코닝 주식회사 | Indium oxide powder, manufacturing method thereof, and manufacturing method of high density indium tin oxide target using the same |
| US7799312B2 (en) | 2002-03-22 | 2010-09-21 | Samsung Corning Precision Glass Co., Ltd. | Method for manufacturing high-density indium tin oxide target, methods for preparing tin oxide powder and indium oxide powder used therefor |
| KR100993171B1 (en) | 2008-08-27 | 2010-11-09 | 고려대학교 산학협력단 | Gas sensor using nano-porous indium oxide spherical structure and fabrication method thereof |
| CN102963922A (en) * | 2012-10-26 | 2013-03-13 | 河南圣玛斯光电科技有限公司 | Hydrothermal synthesis method for indium oxide with cubic crystal structure |
| JP2017047353A (en) * | 2015-08-31 | 2017-03-09 | パナソニックＩｐマネジメント株式会社 | Method for recovering indium |
| CN106732517A (en) * | 2016-11-28 | 2017-05-31 | 青岛科技大学 | A kind of preparation method of the indium hydroxide photochemical catalyst with regular cube structure |
| JP2020066566A (en) * | 2018-10-26 | 2020-04-30 | 株式会社アルバック | Manufacturing method of indium oxide powder |
| JP2020066565A (en) * | 2018-10-26 | 2020-04-30 | 株式会社アルバック | Manufacturing method of indium oxide powder |
| JP2021138594A (en) * | 2020-03-06 | 2021-09-16 | ▲鄭▼州大学 | Preparation method of indium oxide spherical powder capable of controllable grain shape |
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