JPH11228220A - Production of ito sintered compact by slurry casting process - Google Patents
Production of ito sintered compact by slurry casting processInfo
- Publication number
- JPH11228220A JPH11228220A JP10027177A JP2717798A JPH11228220A JP H11228220 A JPH11228220 A JP H11228220A JP 10027177 A JP10027177 A JP 10027177A JP 2717798 A JP2717798 A JP 2717798A JP H11228220 A JPH11228220 A JP H11228220A
- Authority
- JP
- Japan
- Prior art keywords
- slurry
- specific surface
- hours
- surface area
- sintered body
- 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.)
- Pending
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- Manufacturing Of Electric Cables (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Producing Shaped Articles From Materials (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、スパッタリング法
で透明導電膜の形成に用いられるＩＴＯターゲットの製
造に関する。The present invention relates to the production of an ITO target used for forming a transparent conductive film by a sputtering method.
【０００２】[0002]
【従来の技術】ＩＴＯ薄膜は液晶ディスプレイ等の透明
導電膜として広く用いられている。このＩＴＯ薄膜の形
成法としては、ＩＴＯ焼結体をターゲット材として使用
するスパッタリング成膜法が一般的である。2. Description of the Related Art ITO thin films are widely used as transparent conductive films for liquid crystal displays and the like. As a method of forming the ITO thin film, a sputtering film forming method using an ITO sintered body as a target material is generally used.
【０００３】近年、液晶ディスプレイサイズの拡大とと
もにＩＴＯターゲット材の大型化が進んでいる。従来、
ＩＴＯ焼結体の製造方法としては金型プレス法により成
形し、得られた成形体を焼成する方法がある。しかし金
型プレス法は成形サイズの大型化に伴い、設備費が増加
するなどの問題がある。In recent years, the size of an ITO target material has been increasing with the increase in the size of a liquid crystal display. Conventionally,
As a method for producing an ITO sintered body, there is a method of molding by a die pressing method and firing the obtained molded body. However, the die press method has problems such as an increase in equipment cost as the molding size increases.
【０００４】設備費が安価な方法として石膏型等を利用
した泥漿鋳込み成形法があるが、金型プレス法と比較し
て成形体の抗折強度、成形密度が低いために焼成により
クラックなどの欠陥が発生しやすく、また高密度の焼結
体が必ずしも得られない（例えば特公平６−６５９号公
報）。泥漿鋳込み成形後、冷間静水圧プレスにより圧密
化し、密度の向上を図る方法があるが、冷間静水圧プレ
スを施すことにより、設備費が増加する（例えば特公平
８−１１７１１号公報）。[0004] As a method with a low equipment cost, there is a slurry casting method using a gypsum mold or the like. However, since the bending strength and the molding density of the molded body are lower than those of a die pressing method, cracks and the like are caused by firing. Defects are likely to occur, and a high-density sintered body cannot always be obtained (for example, Japanese Patent Publication No. 6-659). There is a method of increasing the density by consolidation by a cold isostatic press after the slip casting, but equipment cost increases by applying the cold isostatic press (for example, Japanese Patent Publication No. H8-11711).
【０００５】[0005]
【発明が解決しようとする課題】本発明の目的は、泥漿
鋳込み法により成形した成形体の抗折強度を高め、焼成
後にクラック、割れなどの欠陥がない大型サイズで高密
度のＩＴＯ焼結体を製造することにある。SUMMARY OF THE INVENTION An object of the present invention is to increase the transverse rupture strength of a molded article formed by a slurry casting method, and to provide a large-sized, high-density ITO sintered body free from defects such as cracks and cracks after firing. Is to manufacture.
【０００６】[0006]
【課題を解決するための手段】本発明者等は、酸化イン
ジウム粉の比表面積を変えることで泥漿鋳込み成形体の
強度が変化することに着目し、成形サイズの大型化に適
した条件を見い出した。また酸化錫粉の比表面積が７．
２ｍ2 ／ｇ以上の場合、酸化インジウムの比表面積に関
係なくクラックが発生しやすいことを見い出した。これ
らの知見に基づいて、酸化インジウム及び酸化錫の比表
面積をある特定の範囲に限定したところ、クラック、割
れなどの欠陥のない高密度ＩＴＯ焼結体を得ることがで
き、本発明を完成させるに至った。尚、ここでいう比表
面積は、ＢＥＴ法で測定される値である。Means for Solving the Problems The present inventors have focused on the fact that the strength of a slurry cast molded body changes by changing the specific surface area of indium oxide powder, and have found conditions suitable for increasing the molding size. Was. The specific surface area of the tin oxide powder is 7.
When it is 2 m 2 / g or more, it has been found that cracks are easily generated regardless of the specific surface area of indium oxide. Based on these findings, when the specific surface areas of indium oxide and tin oxide were limited to a specific range, a high-density ITO sintered body free from defects such as cracks and cracks could be obtained, and the present invention was completed. Reached. Here, the specific surface area is a value measured by the BET method.
【０００７】本発明は、下記の事項をその特徴としてい
る。 （１） 比表面積４．６ｍ2 ／ｇ以上１４．７ｍ2 ／ｇ
以下の酸化インジウム粉と、比表面積７．２ｍ2 ／ｇ以
下の酸化錫粉をイオン交換水で調製してスラリーを作
り、このスラリーを泥漿鋳込み成形型を用いて成形体と
し、得られた成形体を乾燥後、焼成することを特徴とす
るＩＴＯ焼結体の製造方法。 （２） 上記（１）の方法で製造された成形体を乾燥
後、酸素雰囲気で焼成して得られる相対密度９７．５％
（密度６．９７ｇ／ｃｍ3 ）以上のＩＴＯ焼結体。The present invention has the following features. (1) Specific surface area of 4.6 m 2 / g or more and 14.7 m 2 / g
The following indium oxide powder and tin oxide powder having a specific surface area of 7.2 m 2 / g or less were prepared with ion-exchanged water to form a slurry, and this slurry was formed into a compact using a slurry casting mold. A method for producing an ITO sintered body, comprising drying and firing the body. (2) The relative density obtained by drying the molded body produced by the method of (1) and firing in an oxygen atmosphere is 97.5%.
(Density 6.97 g / cm 3 ) or more ITO sintered body.
【０００８】本発明を以下に詳細に説明する。本発明の
泥漿鋳込み法によるＩＴＯ焼結体の製造工程は、図１に
示す通りである。以下に、その各製造工程について説明
する。The present invention will be described in detail below. The manufacturing process of the ITO sintered body by the slurry casting method of the present invention is as shown in FIG. Hereinafter, each manufacturing process will be described.
【０００９】（ａ） 原料粉の調整 市販の酸化インジウム粉、酸化錫粉は、微粒で凝集しや
すいために仮焼処理によって微粒子を粒成長させる。こ
のとき仮焼処理温度によって酸化インジウム粉、酸化錫
粉の比表面積を変えることができる。(A) Preparation of Raw Material Powder Since commercially available indium oxide powder and tin oxide powder are fine and easily aggregated, fine particles are grown by calcining. At this time, the specific surface area of the indium oxide powder and the tin oxide powder can be changed depending on the calcination temperature.
【００１０】酸化インジウム粉の比表面積は、４．６〜
１４．６ｍ2 ／ｇとする。比表面積が１４．６ｍ2 ／ｇ
超であると焼結体にクラックが発生しやすい。また、比
表面積が４．６ｍ2 ／ｇ未満であると、脱脂後の抗折強
度が小さく、成形体や焼結体にクラックや割れが発生し
やすくなる。The specific surface area of the indium oxide powder is from 4.6 to
It is set to 14.6 m 2 / g. Specific surface area is 14.6m 2 / g
If it is more than one, cracks tend to occur in the sintered body. On the other hand, when the specific surface area is less than 4.6 m 2 / g, the transverse rupture strength after degreasing is small, and cracks and cracks are liable to be generated in the formed body and the sintered body.
【００１１】（ｂ） スラリーの調製 酸化インジウム、酸化錫、イオン交換水を樹脂製ポット
に入れボールミルにより粉砕、混合する。酸化錫組成は
５〜１０ｗｔ％が好ましい。その後、水及び分散剤、バ
インダーを加えて、湿式ボールミルによりスラリーを調
製する。容器はポリエチレン製、ポリプロピレン製、ナ
イロン製のものなどが使用できる。ボールはジルコニア
製、樹脂製のものなどが使用できる。分散剤はポリカル
ボン酸系のものが使用でき、バインダーとしてはワック
スエマルジョン系、アクリルエマルジョン系のものが使
用できる。(B) Preparation of slurry Indium oxide, tin oxide, and ion-exchanged water are put into a resin pot and ground and mixed by a ball mill. The tin oxide composition is preferably from 5 to 10% by weight. Thereafter, water, a dispersant, and a binder are added, and a slurry is prepared by a wet ball mill. The container can be made of polyethylene, polypropylene, nylon, or the like. The ball may be made of zirconia or resin. A polycarboxylic acid-based dispersant can be used, and a wax emulsion-based or acrylic emulsion-based dispersant can be used as a binder.
【００１２】（ｃ） スラリーの鋳込み成形 スラリーに消泡剤を添加して減圧脱気する。消泡剤はア
ミド系のものなどが使用できる。脱気したスラリーを、
図２に示す成形型に鋳込み、フィルターの下型面側を減
圧し、スラリー中の水分を排水することにより成形す
る。本発明で限定した酸化インジウム粉、酸化錫粉から
スラリーを調製した場合、成形型は図２に示す成形型に
限定されるものではなく、石膏型、樹脂型を使用するこ
とができる。(C) Casting of the slurry An antifoaming agent is added to the slurry and the slurry is degassed under reduced pressure. An amide-based defoaming agent can be used. The degassed slurry is
The molding is performed by casting into a mold shown in FIG. 2, reducing the pressure on the lower mold side of the filter, and draining the water in the slurry. When a slurry is prepared from the indium oxide powder and the tin oxide powder limited in the present invention, the molding die is not limited to the molding die shown in FIG. 2, but a gypsum die or a resin die can be used.
【００１３】（ｄ） 成形体の乾燥、脱脂 成形体は室温で乾燥後、熱風循環式脱脂炉を使用して残
留水分及びバインダーを除去する。脱脂温度は４００〜
６００℃が好ましい。(D) Drying and Degreasing of the Molded Body After the molded body is dried at room temperature, residual moisture and binder are removed by using a hot air circulation type degreasing furnace. Degreasing temperature is 400 ~
600 ° C. is preferred.
【００１４】（ｅ） 成形体の焼成 残留水分及びバインダーを除去した成形体を焼成するこ
とにより、ＩＴＯ焼結体を得ることができる。また、焼
成を酸素雰囲気下で行うことにより相対密度９７．５％
（６．９７ｇ／ｃｍ3 ）以上のＩＴＯ焼結体を得ること
ができる。焼成温度は１４００〜１６００℃が好まし
い。(E) Firing of the molded body By firing the molded body from which residual moisture and binder have been removed, an ITO sintered body can be obtained. Further, by performing the firing in an oxygen atmosphere, the relative density is 97.5%.
(6.97 g / cm 3 ) or more of ITO sintered body can be obtained. The firing temperature is preferably from 1400 to 1600 ° C.
【００１５】[0015]
【実施例】以下に、本発明を実施例と比較例により更に
説明する。実施例１ 比表面積８．０７ｍ2 ／ｇの酸化インジウム粉９００ｇ
と比表面積２．２ｍ2／ｇの酸化錫粉１００ｇ、イオン
交換水３０ｇ及び直径５ｍｍのジルコニアボールを樹脂
製ポットに入れ２０時間ボールミル混合を行った。次に
イオン交換水１７８．３ｇとポリカルボン酸系分散剤
７．９ｇを入れ、１時間ボールミル混合した。１時間後
にワックス系バインダー９．９ｇを添加し、１９時間ボ
ールミル混合を行った。The present invention will be further described below with reference to examples and comparative examples. Example 1 900 g of indium oxide powder having a specific surface area of 8.07 m 2 / g
And 100 g of tin oxide powder having a specific surface area of 2.2 m 2 / g, 30 g of ion-exchanged water, and zirconia balls having a diameter of 5 mm were placed in a resin pot and mixed with a ball mill for 20 hours. Next, 178.3 g of ion-exchanged water and 7.9 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 9.9 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００１６】次にスラリーにアミド系消泡剤０．２ｇを
添加し減圧脱気を行った。このスラリーの濃度は８３％
だった。このスラリーを図２に示す構造の成形サイズ１
９０ｍｍφの成形用型に鋳込み、減圧−７６０ｍｍＨｇ
で排水した成形体を得た。成形体は２５℃乾燥後、６０
０℃で９時間脱脂を行った。脱脂後の抗折強度は０．９
４ｋｇｆ／ｍｍ2 であった。脱脂した成形体を酸素雰囲
気にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。
ＩＴＯ焼結体の寸法は１５７．３ｍｍφ×６．１ｍｍで
あり、密度は９９．４％（７．１１ｇ／ｃｍ3 ）であっ
た。尚、スラリー濃度の定義は次の通りである。 スラリー濃度（％）＝溶質重量／（溶質重量＋溶媒重
量）×１００Next, 0.2 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 83%
was. This slurry was formed into a molding size 1 having the structure shown in FIG.
Cast into a molding die of 90mmφ, reduced pressure -760mmHg
To obtain a molded body. After drying at 25 ° C.,
Degreasing was performed at 0 ° C. for 9 hours. Flexural strength after degreasing is 0.9
It was 4 kgf / mm 2 . The degreased molded body was fired at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body.
The dimensions of the ITO sintered body were 157.3 mmφ × 6.1 mm, and the density was 99.4% (7.11 g / cm 3 ). The definition of the slurry concentration is as follows. Slurry concentration (%) = solute weight / (solute weight + solvent weight) × 100
【００１７】実施例２ 比表面積８．５２ｍ2 ／ｇの酸化インジウム粉７２００
ｇと、比表面積２．９５ｍ2 ／ｇの酸化錫粉８００ｇ、
イオン交換水２４０ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１４４０ｇとポリカルボン酸
系分散剤６４ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを８０ｇ添加し１９時間ボ
ールミル混合を行った。 Example 2 Indium oxide powder 7200 having a specific surface area of 8.52 m 2 / g
g of tin oxide powder having a specific surface area of 2.95 m 2 / g,
240 g of ion-exchanged water was placed in a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1440 g of ion-exchanged water and 64 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 80 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００１８】次にスラリーにアミド系消泡剤１．６ｇを
添加し減圧脱気を行った。このスラリーの濃度は８３％
だった。このスラリーを、図２に示す構造の成形サイズ
７００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７
６０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、
脱脂処理を６００℃で３時間行った。その後、酸素雰囲
気にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。
このときのＩＴＯ焼結体の寸法は５７８ｍｍ×２４７ｍ
ｍ×６．９ｍｍであり、焼結体の密度は９７．７％
（６．９９ｇ／ｃｍ3 ）であった。焼結体にクラック、
割れなどの欠陥がなかった。Next, 1.6 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 83%
was. This slurry was cast into a mold having a structure shown in FIG. 2 and having a molding size of 700 mm × 300 mm.
Drained at 60 mmHg to obtain a molded body. After drying the molded body,
The degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body.
At this time, the size of the ITO sintered body was 578 mm × 247 m.
mx 6.9 mm, and the density of the sintered body is 97.7%
(6.99 g / cm 3 ). Cracks in the sintered body,
There were no defects such as cracks.
【００１９】実施例３ 比表面積８．０７ｍ2 ／ｇの酸化インジウム粉７２００
ｇと、比表面積２．６８ｍ2 ／ｇの酸化錫粉８００ｇ、
イオン交換水２４０ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１４４０ｇとポリカルボン酸
系分散剤６４ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを８０ｇ添加し１９時間ボ
ールミル混合を行った。 Example 3 Indium oxide powder 7200 having a specific surface area of 8.07 m 2 / g
g of tin oxide powder having a specific surface area of 2.68 m 2 / g,
240 g of ion-exchanged water was placed in a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1440 g of ion-exchanged water and 64 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 80 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００２０】次にスラリーにアミド系消泡剤１．６ｇを
添加し減圧脱気を行った。このスラリーの濃度は８３％
であった。このスラリーを図２に示す構造の成形サイズ
７００ｍｍ×８００ｍｍの成形用型に鋳込み、減圧−７
６０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、
脱脂処理を６００℃で３時間行った。その後、酸素雰囲
気にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。
このときのＩＴＯ焼結体の寸法は５７８ｍｍ×２４７ｍ
ｍ×７．３ｍｍであり、焼結体の密度は９８．１％
（７．０１ｇ／ｃｍ3 ）であった。焼結体にクラック、
割れなどの欠陥がなかった。Next, 1.6 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 83%
Met. This slurry was cast into a mold having a structure shown in FIG. 2 and having a molding size of 700 mm × 800 mm.
Drained at 60 mmHg to obtain a molded body. After drying the molded body,
The degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body.
At this time, the size of the ITO sintered body was 578 mm × 247 m.
mx 7.3 mm, and the density of the sintered body is 98.1%
(7.01 g / cm 3 ). Cracks in the sintered body,
There were no defects such as cracks.
【００２１】実施例４ 比表面積６．８６ｍ2 ／ｇの酸化インジウム粉６７５０
ｇと、比表面積３．３８ｍ2 ／ｇの酸化錫粉７５０ｇ、
イオン交換水２２５ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１３４８．２ｇとポリカルボ
ン酸系分散剤６０ｇを入れ１時間ボールミル混合した。
１時間後にワックス系バインダーを７５ｇ添加し１９時
間ボールミル混合を行った。 Example 4 Indium oxide powder 6750 having a specific surface area of 6.86 m 2 / g
g of tin oxide powder having a specific surface area of 3.38 m 2 / g,
225 g of ion-exchanged water was put into a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1348.2 g of ion-exchanged water and 60 g of a polycarboxylic acid-based dispersant were added and mixed with a ball mill for 1 hour.
One hour later, 75 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００２２】次にスラリーにアミド系消泡剤１．４ｇを
添加し減圧脱気を行った。このスラリーの濃度は８３％
だった。このスラリーを、図２に示す構造の成形サイズ
７００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７
６０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、
脱脂処理を６００℃で３時間行った。その後、酸素雰囲
気にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。
このときのＩＴＯ焼結体の寸法は５６５ｍｍ×２４２ｍ
ｍ×７．１ｍｍであり、焼結体の密度は９８．７％
（７．０５ｇ／ｃｍ3 ）であった。焼結体にクラック、
割れなどの欠陥がなかった。Next, 1.4 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 83%
was. This slurry was cast into a mold having a structure shown in FIG. 2 and having a molding size of 700 mm × 300 mm.
Drained at 60 mmHg to obtain a molded body. After drying the molded body,
The degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body.
At this time, the size of the ITO sintered body was 565 mm × 242 m.
mx 7.1 mm, and the density of the sintered body is 98.7%
(7.05 g / cm 3 ). Cracks in the sintered body,
There were no defects such as cracks.
【００２３】実施例５ 比表面積６．５４ｍ2 ／ｇの酸化インジウム粉７２００
ｇと、比表面積２．４９ｍ2 ／ｇの酸化錫粉８００ｇ、
イオン交換水２４０ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１４４０ｇとポリカルボン酸
系分散剤６４ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを８０ｇ添加し１９時間ボ
ールミル混合を行った。 Example 5 Indium oxide powder 7200 having a specific surface area of 6.54 m 2 / g
g, tin oxide powder 800 g having a specific surface area of 2.49 m 2 / g,
240 g of ion-exchanged water was placed in a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1440 g of ion-exchanged water and 64 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 80 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００２４】次にスラリーにアミド系消泡剤１．６ｇを
添加し減圧脱気を行った。このスラリーの濃度は８３％
だった。このスラリーを図２に示す構造の成形サイズ７
００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７６
０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、脱
脂処理を６００℃で３時間行った。その後、酸素雰囲気
にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。こ
のときのＩＴＯ焼結体の寸法は５７２ｍｍ×２４５ｍｍ
×７．３ｍｍであり、焼結体の密度は９８．６％（７．
０３ｇ／ｃｍ3 ）であった。焼結体にクラック、割れな
どの欠陥がなかった。Next, 1.6 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 83%
was. This slurry was molded to a size of 7 having the structure shown in FIG.
Cast into a 00 mm x 300 mm molding die,
Drained at 0 mmHg to obtain a molded body. After drying the compact, a degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. At this time, the size of the ITO sintered body was 572 mm × 245 mm.
× 7.3 mm, and the density of the sintered body was 98.6% (7.
03 g / cm 3 ). There were no cracks, cracks or other defects in the sintered body.
【００２５】実施例６ 比表面積６．６４の酸化インジウム粉１８０００ｇと、
比表面積３．１１の酸化錫粉２０００ｇ、イオン交換水
６００ｇ及び直径５ｍｍのジルコニアボールを樹脂製ポ
ットに入れ２０時間ボールミル混合を行った。次にイオ
ン交換水３５９２ｇとポリカルボン酸系分散剤１６０ｇ
を入れ１時間ボールミル混合した。１時間後にワックス
系バインダーを２００ｇ添加し１９時間ボールミル混合
を行った。 Example 6 18000 g of indium oxide powder having a specific surface area of 6.64,
2000 g of tin oxide powder having a specific surface area of 3.11, 600 g of ion-exchanged water, and zirconia balls having a diameter of 5 mm were placed in a resin pot and mixed with a ball mill for 20 hours. Next, 3592 g of ion-exchanged water and 160 g of a polycarboxylic acid-based dispersant were used.
And mixed with a ball mill for 1 hour. One hour later, 200 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００２６】次にスラリーにアミド系消泡剤４ｇを添加
し減圧脱気を行った。このスラリーの濃度は８３％だっ
た。このスラリーを図２に示す構造の成形サイズ１２７
０ｍｍ×３７５ｍｍの成形用型に鋳込み、減圧−７６０
ｍｍＨｇで排水し成形体を得た。成形体は２５℃乾燥
後、６００℃で３時間脱脂を行い、酸素雰囲気にて１５
５０℃で８時間焼成してＩＴＯ焼結体を得た。ＩＴＯ焼
結体の寸法は１０４６ｍｍ×３０８ｍｍ×７．９ｍｍで
あり、焼結体の密度は９８．８％（７．０６ｇ／ｃ
ｍ3 ）であった。長軸が１０００ｍｍ以上の大型ＩＴＯ
焼結体を得ることができた。Next, 4 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry was 83%. This slurry was formed into a molding size 127 having the structure shown in FIG.
0mm x 375mm casting mold, decompression -760
Drained at mmHg to obtain a molded body. The molded body was dried at 25 ° C, degreased at 600 ° C for 3 hours, and dried in an oxygen atmosphere for 15 hours.
It was fired at 50 ° C. for 8 hours to obtain an ITO sintered body. The dimensions of the ITO sintered body were 1046 mm × 308 mm × 7.9 mm, and the density of the sintered body was 98.8% (7.06 g / c).
m 3 ). Large ITO with a long axis of 1000mm or more
A sintered body was obtained.
【００２７】比較例１ 比表面積４．２２ｍ2 ／ｇの酸化インジウム粉９００ｇ
と、比表面積２．２ｍ2 ／ｇの酸化錫粉１００ｇ、アル
コール系バインダー７．９ｇ及び直径１０ｍｍのジルコ
ニアボールを樹脂製ポットに入れ２０時間ボールミル混
合を行った。処理粉を成形サイズ１９０ｍｍφ、圧力１
０００ｋｇｆ／ｃｍ2 でプレス成形した。成形体は６０
０℃で３時間脱脂を行った。脱脂後の抗折強度は０．７
２ｋｇｆ／ｃｍ2 だった。脱脂した成形体を酸素雰囲気
にて１５５０℃で８時間焼成し高密度ＩＴＯ焼結体を得
た。ＩＴＯ焼結体の寸法は１６６．０ｍｍφ×５．７ｍ
ｍであり、密度は９９．０％（７．０８ｇ／ｃｍ3 ）で
あった。 Comparative Example 1 900 g of indium oxide powder having a specific surface area of 4.22 m 2 / g
And 100 g of tin oxide powder having a specific surface area of 2.2 m 2 / g, 7.9 g of an alcohol-based binder, and zirconia balls having a diameter of 10 mm were placed in a resin pot and mixed with a ball mill for 20 hours. Processed powder is molded at 190mmφ, pressure 1
Press molding was performed at 000 kgf / cm 2 . The molded body is 60
Degreasing was performed at 0 ° C. for 3 hours. Flexural strength after degreasing is 0.7
It was 2 kgf / cm 2 . The degreased molded body was fired in an oxygen atmosphere at 1550 ° C. for 8 hours to obtain a high-density ITO sintered body. The size of the ITO sintered body is 166.0mmφ × 5.7m
m, and the density was 99.0% (7.08 g / cm 3 ).
【００２８】比較例２ 比表面積４．５３ｍ2 ／ｇの酸化インジウム粉９００ｇ
と、比表面積２．２ｍ2 ／ｇの酸化錫粉１００ｇ、イオ
ン交換水３０ｇ及び直径５ｍｍのジルコニアボールを樹
脂製ポットに入れ２０時間ボールミル混合を行った。次
にイオン交換水１２８．７ｇとポリカルボン酸系分散剤
４．５ｇを入れ１時間ボールミル混合した。１時間後に
ワックス系バインダー９．９ｇを添加し１９時間ボール
ミル混合を行った。 Comparative Example 2 900 g of indium oxide powder having a specific surface area of 4.53 m 2 / g
And 100 g of tin oxide powder having a specific surface area of 2.2 m 2 / g, 30 g of ion-exchanged water, and zirconia balls having a diameter of 5 mm were placed in a resin pot and mixed with a ball mill for 20 hours. Next, 128.7 g of ion-exchanged water and 4.5 g of a polycarboxylic acid-based dispersant were added and mixed for 1 hour with a ball mill. One hour later, 9.9 g of a wax-based binder was added, and the mixture was mixed in a ball mill for 19 hours.
【００２９】次にスラリーにアミド系消泡剤０．４ｇを
添加し、減圧脱気を行った。このスラリーの濃度は８６
％だった。このスラリーを、図２に示す構造の成形サイ
ズ１９０ｍｍφの成形用型に鋳込み、減圧−７６０ｍｍ
Ｈｇで排水し成形体を得た。成形体は２５℃乾燥後、６
００℃で３時間脱脂を行った。脱脂後の抗折強度は、
０．６０ｋｇｆ／ｍｍ2 だった。脱脂した成形体を酸素
雰囲気にて１５５０℃で８時間焼成しＩＴＯ焼結体を得
た。ＩＴＯ焼結体の寸法は、１６０．６ｍｍφ×５．９
ｍｍであり、密度は９９．７％（７．１３ｇ／ｃｍ3 ）
であった。Next, 0.4 g of an amide-based antifoaming agent was added to the slurry, and deaeration was performed under reduced pressure. The concentration of this slurry is 86
%was. This slurry was cast into a mold having a structure shown in FIG.
Drained with Hg to obtain a molded body. After drying the molded body at 25 ° C, 6
Degreasing was performed at 00 ° C. for 3 hours. The bending strength after degreasing is
It was 0.60 kgf / mm 2 . The degreased molded body was fired at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. The size of the ITO sintered body is 160.6 mmφ × 5.9.
mm, and the density is 99.7% (7.13 g / cm 3 ).
Met.
【００３０】比較例３ 比表面積４．２２ｍ2 ／ｇの酸化インジウム粉９００ｇ
と、比表面積２．２ｍ2 ／ｇの酸化錫粉１００ｇ、イオ
ン交換水３０ｇ及び直径５ｍｍのジルコニアボールを樹
脂製ポットに入れ２０時間ボールミル混合を行った。次
にイオン交換水１０８．９ｇとポリカルボン酸系分散剤
４．７ｇを入れ１時間ボールミル混合した。１時間後に
ワックス系バインダー７．９ｇを添加し１９時間ボール
ミル混合を行った。 Comparative Example 3 900 g of indium oxide powder having a specific surface area of 4.22 m 2 / g
And 100 g of tin oxide powder having a specific surface area of 2.2 m 2 / g, 30 g of ion-exchanged water, and zirconia balls having a diameter of 5 mm were placed in a resin pot and mixed with a ball mill for 20 hours. Next, 108.9 g of ion-exchanged water and 4.7 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 7.9 g of a wax-based binder was added, and the mixture was mixed in a ball mill for 19 hours.
【００３１】次にスラリーにアミド系消泡剤０．５ｇを
添加し減圧脱気を行った。このスラリーの濃度は８７％
だった。このスラリーを、図２に示す構造の成形サイズ
１９０ｍｍφの成形用型に鋳込み、減圧−７６０ｍｍＨ
ｇで排水し成形体を得た。成形体は２５℃乾燥後、６０
０℃で８時間脱脂を行った。脱脂後の抗折強度は０．５
０ｋｇｆ／ｍｍ2 だった。脱脂した成形体を酸素雰囲気
にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。Ｉ
ＴＯ焼結体の寸法は１６６．０ｍｍφ×５．５ｍｍであ
り、密度は９９．９％（７．１４ｇ／ｃｍ3 ）であっ
た。Next, 0.5 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 87%
was. This slurry is cast into a mold having a structure shown in FIG.
g to obtain a molded product. After drying at 25 ° C.,
Degreasing was performed at 0 ° C. for 8 hours. Flexural strength after degreasing is 0.5
It was 0 kgf / mm 2 . The degreased molded body was fired at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. I
The dimensions of the TO sintered body were 166.0 mmφ × 5.5 mm, and the density was 99.9% (7.14 g / cm 3 ).
【００３２】比較例４ 比表面積１４．７ｍ2 ／ｇの酸化インジウム粉７２００
ｇと、比表面積２．４８２ｍ2 ／ｇの酸化錫粉８００
ｇ、イオン交換水２４０ｇを直径５ｍｍのジルコニアボ
ールとともに樹脂製ポットに入れ２０時間ボールミル混
合を行った。次にイオン交換水２０００ｇとポリカルボ
ン酸系分散剤６４ｇを入れ１時間ボールミル混合した。
１時間後にワックス系バインダーを８０ｇ添加し１９時
間ボールミル混合を行った。 Comparative Example 4 Indium oxide powder 7200 having a specific surface area of 14.7 m 2 / g
g and tin oxide powder 800 having a specific surface area of 2.482 m 2 / g
g and 240 g of ion-exchanged water together with a zirconia ball having a diameter of 5 mm were placed in a resin pot and mixed with a ball mill for 20 hours. Next, 2000 g of ion-exchanged water and 64 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour.
One hour later, 80 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００３３】次にスラリーにアミド系消泡剤１．６ｇを
添加し減圧脱気を行った。このスラリーの濃度は７６％
だった。このスラリーを図２に示す構造の成形サイズ７
００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７６
０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、脱
脂処理を６００℃で３時間行った。その後、酸素雰囲気
にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。こ
のときのＩＴＯ焼結体の寸法は５２２ｍｍ×２２４ｍｍ
×７．１ｍｍであり、焼結体の密度は９８．５％（７．
０４ｇ／ｃｍ3 ）であった。焼結体に１０ｍｍ〜２０ｍ
ｍのクラックが６本発生した。Next, 1.6 g of an amide-based antifoaming agent was added to the slurry and deaeration was performed under reduced pressure. The concentration of this slurry is 76%
was. This slurry was molded to a size of 7 having the structure shown in FIG.
Cast into a 00 mm x 300 mm molding die,
Drained at 0 mmHg to obtain a molded body. After drying the compact, a degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. At this time, the size of the ITO sintered body was 522 mm × 224 mm.
× 7.1 mm, and the density of the sintered body was 98.5% (7.
04 g / cm 3 ). 10mm to 20m for sintered body
m cracks occurred.
【００３４】比較例５ 比表面積７．７３ｍ2 ／ｇの酸化インジウム粉７２００
ｇと、比表面積７．６２ｍ2 ／ｇの酸化錫粉８００ｇ、
イオン交換水４００ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１４４０ｇとポリカルボン酸
系分散剤８０ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを８０ｇ添加し１９時間ボ
ールミル混合を行った。 Comparative Example 5 Indium oxide powder 7200 having a specific surface area of 7.73 m 2 / g
g of tin oxide powder having a specific surface area of 7.62 m 2 / g,
400 g of ion-exchanged water was put into a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1440 g of ion-exchanged water and 80 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 80 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００３５】次にスラリーにアミド系消泡剤１．６ｇを
添加し減圧脱気を行った。このスラリーの濃度は８２％
だった。このスラリーを図２に示す構造の成形サイズ７
００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７６
０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、脱
脂処理を６００℃で３時間行った。その後、酸素雰囲気
にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。こ
のときのＩＴＯ焼結体の寸法は５７５ｍｍ×２４６ｍｍ
×７．４ｍｍであり、焼結体の密度は９７．８％（６．
９９ｇ／ｃｍ3 ）であった。焼結体に長さ４〜２６ｍｍ
のクラックが１９本発生した。Next, 1.6 g of an amide-based antifoaming agent was added to the slurry, and deaeration was performed under reduced pressure. The concentration of this slurry is 82%
was. This slurry was molded to a size of 7 having the structure shown in FIG.
Cast into a 00 mm x 300 mm molding die,
Drained at 0 mmHg to obtain a molded body. After drying the compact, a degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. The size of the ITO sintered body at this time is 575 mm x 246 mm
× 7.4 mm, and the density of the sintered body was 97.8% (6.
99 g / cm 3 ). 4 to 26 mm length for sintered body
19 cracks occurred.
【００３６】比較例６ 比表面積７．７３ｍ2 ／ｇの酸化インジウム粉８１００
ｇと、比表面積７．２３ｍ2 ／ｇの酸化錫粉９００ｇ、
イオン交換水４５０ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１７１０ｇとポリカルボン酸
系分散剤９４ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを９０ｇ添加し１９時間ボ
ールミル混合を行った。このスラリーの濃度は８１％だ
った。このスラリーを図２に示す構造の成形サイズ７０
０ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７６０
ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、脱脂
処理を６００℃で３時間行った。脱脂後の密度は６３％
（４．５ｇ／ｃｍ3 ）であった。成形体は脱脂により中
央部分で２つに割れた。 Comparative Example 6 Indium oxide powder 8100 having a specific surface area of 7.73 m 2 / g
g of tin oxide powder having a specific surface area of 7.23 m 2 / g;
450 g of ion-exchanged water was put into a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1710 g of ion-exchanged water and 94 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 90 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours. The concentration of this slurry was 81%. This slurry was formed into a molding size 70 having the structure shown in FIG.
Cast into a 0 mm x 300 mm molding die and decompress -760
Drained at mmHg to obtain a molded body. After drying the compact, a degreasing treatment was performed at 600 ° C. for 3 hours. 63% density after degreasing
(4.5 g / cm 3 ). The molded body was split into two at the center by degreasing.
【００３７】比較例７ 比表面積４．５３ｍ2 ／ｇの酸化インジウム粉８１００
ｇと、比表面積２．６８ｍ2 ／ｇの酸化錫粉９００ｇ、
イオン交換水２７０ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１１７０ｇとポリカルボン酸
系分散剤４１ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを９０ｇ添加し１９時間ボ
ールミル混合を行った。 Comparative Example 7 Indium oxide powder 8100 having a specific surface area of 4.53 m 2 / g
g of tin oxide powder having a specific surface area of 2.68 m 2 / g;
270 g of ion-exchanged water was put in a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1170 g of ion-exchanged water and 41 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 90 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００３８】次にスラリーにアミド系消泡剤４．５ｇを
添加し減圧脱気を行った。このスラリーの濃度は８６％
だった。このスラリーを図２に示す構造の成形サイズ７
００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７６
０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、脱
脂処理を６００℃で３時間行った。その後、酸素雰囲気
にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。こ
のときのＩＴＯ焼結体の寸法は５９３ｍｍ×２５４ｍｍ
×７．７ｍｍであり、焼結体の密度は９８．６％（７．
０５ｇ／ｃｍ3 ）であった。焼結体に２０ｍｍのクラッ
クが発生した。Next, 4.5 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 86%
was. This slurry was molded to a size of 7 having the structure shown in FIG.
Cast into a 00 mm x 300 mm molding die,
Drained at 0 mmHg to obtain a molded body. After drying the compact, a degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. At this time, the size of the ITO sintered body was 593 mm × 254 mm.
× 7.7 mm, and the density of the sintered body was 98.6% (7.
05 g / cm 3 ). A 20 mm crack was generated in the sintered body.
【００３９】比較例８ 比表面積４．５０ｍ2 ／ｇの酸化インジウム粉７２００
ｇと、比表面積７．６２ｍ2 ／ｇの酸化錫粉８００ｇ、
イオン交換水２４０ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１４４０ｇとポリカルボン酸
系分散剤６４ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを８０ｇ添加し１９時間ボ
ールミル混合を行った。 Comparative Example 8 Indium oxide powder 7200 having a specific surface area of 4.50 m 2 / g
g of tin oxide powder having a specific surface area of 7.62 m 2 / g,
240 g of ion-exchanged water was placed in a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1440 g of ion-exchanged water and 64 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 80 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００４０】次にスラリーにアミド系消泡剤１．６ｇを
添加し減圧脱気を行った。このスラリーの濃度は８３％
だった。このスラリーを図２に示す構造の成形サイズ７
００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７６
０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、脱
脂処理を６００℃で３時間行った。その後、酸素雰囲気
にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。こ
のときのＩＴＯ焼結体の寸法は５８８ｍｍ×２５１ｍｍ
×７．１ｍｍであり、焼結体の密度は９７．９％（７．
００ｇ／ｃｍ3 ）であった。焼結体に１２ｍｍ及び１７
ｍｍのクラックが発生した。Next, 1.6 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 83%
was. This slurry was molded to a size of 7 having the structure shown in FIG.
Cast into a 00 mm x 300 mm molding die,
Drained at 0 mmHg to obtain a molded body. After drying the compact, a degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. At this time, the dimensions of the ITO sintered body were 588 mm × 251 mm.
× 7.1 mm, and the density of the sintered body was 97.9% (7.
00 g / cm 3 ). 12mm and 17
mm cracks occurred.
【００４１】比較例９ 比表面積３．６８ｍ2 ／ｇの酸化インジウム粉８１００
ｇと、比表面積２．６５ｍ2 ／ｇの酸化錫粉９００ｇ、
イオン交換水２７０ｇを直径５ｍｍのジルコニアボール
とともに樹脂製ポットに入れ２０時間ボールミル混合を
行った。次にイオン交換水１１７０ｇとポリカルボン酸
系分散剤４１ｇを入れ１時間ボールミル混合した。１時
間後にワックス系バインダーを９０ｇ添加し１９時間ボ
ールミル混合を行った。 Comparative Example 9 Indium oxide powder 8100 having a specific surface area of 3.68 m 2 / g
g of tin oxide powder having a specific surface area of 2.65 m 2 / g;
270 g of ion-exchanged water was put in a resin pot together with zirconia balls having a diameter of 5 mm, and mixed in a ball mill for 20 hours. Next, 1170 g of ion-exchanged water and 41 g of a polycarboxylic acid-based dispersant were added and mixed in a ball mill for 1 hour. One hour later, 90 g of a wax-based binder was added, and ball mill mixing was performed for 19 hours.
【００４２】次にスラリーにアミド系消泡剤４．５ｇを
添加し減圧脱気を行った。このスラリーの濃度は８６％
だった。このスラリーを図２に示す構造の成形サイズ７
００ｍｍ×３００ｍｍの成形用型に鋳込み、減圧−７６
０ｍｍＨｇで排水し成形体を得た。成形体を乾燥後、脱
脂処理を６００℃で３時間行った。その後、酸素雰囲気
にて１５５０℃で８時間焼成しＩＴＯ焼結体を得た。こ
のときのＩＴＯ焼結体の寸法は５９７ｍｍ×２５５ｍｍ
×７．５ｍｍであり、焼結体の密度は９８．６％（７．
０５ｇ／ｃｍ3 ）であった。焼結体に１５ｍｍのクラッ
クが発生した。Next, 4.5 g of an amide-based antifoaming agent was added to the slurry, followed by degassing under reduced pressure. The concentration of this slurry is 86%
was. This slurry was molded to a size of 7 having the structure shown in FIG.
Cast into a 00 mm x 300 mm molding die,
Drained at 0 mmHg to obtain a molded body. After drying the compact, a degreasing treatment was performed at 600 ° C. for 3 hours. Then, it was baked at 1550 ° C. for 8 hours in an oxygen atmosphere to obtain an ITO sintered body. At this time, the size of the ITO sintered body was 597 mm × 255 mm.
× 7.5 mm, and the density of the sintered body was 98.6% (7.
05 g / cm 3 ). A 15 mm crack occurred in the sintered body.
【００４３】表１は酸化錫の比表面積を固定した条件で
の酸化インジウムの比表面積とＩＴＯターゲットの抗折
強度を示している。酸化インジウムの比表面積が等しい
場合、泥漿鋳込み法で成形したＩＴＯ成形体はプレス成
形したＩＴＯ成形体に比較して抗折強度が低い。しかし
ながら、酸化インジウムの比表面積を高くすることで抗
折強度を高めることができる。Table 1 shows the specific surface area of indium oxide and the bending strength of the ITO target when the specific surface area of tin oxide was fixed. When the specific surface area of indium oxide is equal, the ITO molded body formed by the slurry casting method has a lower bending strength than the pressed ITO molded body. However, the bending strength can be increased by increasing the specific surface area of indium oxide.
【００４４】[0044]
【表１】 [Table 1]
【００４５】表２に内寸法７００ｍｍ×３００ｍｍで成
形したＩＴＯ成形体の密度及び欠陥の有無を示す。使用
した酸化インジウム、酸化錫の原料粉の比表面積が本発
明で限定した範囲から外れるとクラック、脱脂割れなが
の欠陥が発生する。Table 2 shows the density and the presence / absence of defects of the ITO molded body having an inner size of 700 mm × 300 mm. If the specific surface area of the used indium oxide or tin oxide raw material powder is out of the range defined in the present invention, cracks and degreasing cracks are generated.
【００４６】[0046]
【表２】 [Table 2]
【００４７】[0047]
【発明の効果】本発明によれば、酸化インジウムと酸化
錫の原料粉の比表面積を適正範囲に選択することによ
り、泥漿鋳込み成形法により従来の比べて大型で欠陥の
ない高密度ＩＴＯ焼結体が得られる。According to the present invention, by selecting the specific surface area of the raw material powder of indium oxide and tin oxide within an appropriate range, a high-density ITO sintering which is larger than the conventional one and has no defect can be performed by a slurry casting method. The body is obtained.
【図１】本発明に係る泥漿鋳込み法によるＩＴＯターゲ
ットの製造工程を示す説明図である。FIG. 1 is an explanatory view showing a production process of an ITO target by a slurry casting method according to the present invention.
【図２】本発明の泥漿鋳込み法に使用される成形型の説
明図である。FIG. 2 is an explanatory view of a molding die used in the slurry casting method of the present invention.
１ スラリー ２ 成形用型枠 ３ 成形用下型 ４ フィルター ５ シール材 ６ 水抜き孔 DESCRIPTION OF SYMBOLS 1 Slurry 2 Mold form 3 Lower mold 4 Filter 5 Sealing material 6 Drain hole
フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｈ０１Ｂ 13/00 ５０３ Ｃ０４Ｂ 35/00 Ｄ Continued on the front page (51) Int.Cl. 6 Identification code FI H01B 13/00 503 C04B 35/00 D
Claims (2)
／ｇ以下の酸化インジウム粉と、比表面積７．２ｍ2 ／
ｇ以下の酸化錫粉をイオン交換水で調製してスラリーを
作り、このスラリーを泥漿鋳込み成形法により成形体と
し、得られた成形体を乾燥後、焼成することを特徴とす
るＩＴＯ焼結体の製造方法。1. A specific surface area of 4.6 m 2 / g or more and 14.6 m 2.
/ G or less of indium oxide powder and a specific surface area of 7.2 m 2 /
g of tin oxide powder or less with ion-exchanged water to form a slurry, and this slurry is formed into a compact by a slurry casting method, and the obtained compact is dried and fired. Manufacturing method.
成形体を乾燥後、酸素雰囲気で焼成して得られる相対密
度９７．５％（密度６．９７ｇ／ｃｍ3 ）以上のＩＴＯ
焼結体。2. An ITO manufactured by the method according to claim 1.
An ITO having a relative density of 97.5% (density 6.97 g / cm 3 ) or more obtained by drying the molded body and firing in an oxygen atmosphere
Sintered body.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10027177A JPH11228220A (en) | 1998-02-09 | 1998-02-09 | Production of ito sintered compact by slurry casting process |
| TW088101590A TW548256B (en) | 1998-02-04 | 1999-02-02 | Filtration-type mold and method for producing ceramic sintered body using the mold |
| KR10-1999-0003841A KR100453621B1 (en) | 1998-02-04 | 1999-02-04 | Filtration forming mold and method for producing ceramics sintered body using the same |
| CN99100765A CN1121358C (en) | 1998-02-04 | 1999-02-04 | Filtration-type mold and mehtod for producing ceramic sintered body using the mold |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10027177A JPH11228220A (en) | 1998-02-09 | 1998-02-09 | Production of ito sintered compact by slurry casting process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11228220A true JPH11228220A (en) | 1999-08-24 |
Family
ID=12213800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10027177A Pending JPH11228220A (en) | 1998-02-04 | 1998-02-09 | Production of ito sintered compact by slurry casting process |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11228220A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100370401B1 (en) * | 2000-08-31 | 2003-01-30 | 삼성코닝 주식회사 | Method for preparing indium tin oxide powder from indium tin oxide scrap |
| KR100370402B1 (en) * | 2000-08-31 | 2003-01-30 | 삼성코닝 주식회사 | Method for preparing indium tin oxide powder from indium tin oxide scrap |
| JP2006222408A (en) * | 2005-01-14 | 2006-08-24 | Ricoh Co Ltd | Conductive wiring structure and manufacturing method thereof |
| JP2009537426A (en) * | 2006-05-18 | 2009-10-29 | イドロ−ケベック | Ceramic preparation process, the ceramic thus obtained and its use as a sputtering target in particular |
| JP2011140235A (en) * | 2011-04-04 | 2011-07-21 | Ulvac Japan Ltd | Mold and method for producing plate-shaped sintered body |
-
1998
- 1998-02-09 JP JP10027177A patent/JPH11228220A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100370401B1 (en) * | 2000-08-31 | 2003-01-30 | 삼성코닝 주식회사 | Method for preparing indium tin oxide powder from indium tin oxide scrap |
| KR100370402B1 (en) * | 2000-08-31 | 2003-01-30 | 삼성코닝 주식회사 | Method for preparing indium tin oxide powder from indium tin oxide scrap |
| JP2006222408A (en) * | 2005-01-14 | 2006-08-24 | Ricoh Co Ltd | Conductive wiring structure and manufacturing method thereof |
| JP4675144B2 (en) * | 2005-01-14 | 2011-04-20 | 株式会社リコー | Method for manufacturing conductor wiring structure |
| JP2009537426A (en) * | 2006-05-18 | 2009-10-29 | イドロ−ケベック | Ceramic preparation process, the ceramic thus obtained and its use as a sputtering target in particular |
| JP2011140235A (en) * | 2011-04-04 | 2011-07-21 | Ulvac Japan Ltd | Mold and method for producing plate-shaped sintered body |
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