JP2000061917A - Ito molding and manufacture thereof and manufacture of ito sintered body - Google Patents

Ito molding and manufacture thereof and manufacture of ito sintered body

Info

Publication number
JP2000061917A
JP2000061917A JP10237499A JP23749998A JP2000061917A JP 2000061917 A JP2000061917 A JP 2000061917A JP 10237499 A JP10237499 A JP 10237499A JP 23749998 A JP23749998 A JP 23749998A JP 2000061917 A JP2000061917 A JP 2000061917A
Authority
JP
Japan
Prior art keywords
slurry
density
molding
ito
molded 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
Application number
JP10237499A
Other languages
Japanese (ja)
Inventor
Isao Nakamura
村 功 中
Yoichiro Emori
森 洋一郎 江
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsui Mining and Smelting Co Ltd
Original Assignee
Mitsui Mining and Smelting Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsui Mining and Smelting Co Ltd filed Critical Mitsui Mining and Smelting Co Ltd
Priority to JP10237499A priority Critical patent/JP2000061917A/en
Publication of JP2000061917A publication Critical patent/JP2000061917A/en
Pending legal-status Critical Current

Links

Abstract

PROBLEM TO BE SOLVED: To provide moldings whose molding density is uniform by molding slurry consisting of indium oxide and tin oxide by casting above a specific pressure value with the help of a gypsum mold and setting the density irregularities below a specified value with an erosion region having a heavily tall shape. SOLUTION: It is possible to obtain ITO moldings with 58% or more molding density by making the specific surface area of indium oxide 3-8 m2/g through a temporary burning treatment. In this ease, a cold static water pressure pressing work is not required and the slurry pressure to be applied is 3 kg/cm2 or more to obtain the moldings with 1.5% or less density irregularities. The gypsum mold is preferably molded at 10 kg/cm2 or less slurry pressure from the viewpoint of its strength. The ITO moldings are dried at a room temperature. The ITO moldings with 98.5% or more relative density can be obtained by baking the moldings in an oxygen atmosphere. The baking temperature is preferably 1400-1600 deg.C.

Description

【発明の詳細な説明】Detailed Description of the Invention

【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。
TECHNICAL FIELD 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 for forming this ITO thin film, a sputtering film forming method using an ITO sintered body as a target material is generally used.

【0003】スパッタリング法では、マグネットによっ
て制御されたプラズマをターゲットに衝突させるため、
ターゲットがマグネットの形状に沿ってエロージョンを
受け、使用効率が低いという問題がある。使用効率を上
げるために、例えば特開昭57−185973号公報及
び特開昭60−39158号公報にはターゲットの消耗
の激しい部分の厚みを大きくしたターゲットを用いるこ
とが記載されている。エロージョンを受ける領域(以
下、「エロージョン領域」という)を厚くしたターゲッ
トの製造法としては、金型プレス法により厚みの異なる
平板型のターゲットを複数成形し、これを焼成、加工し
てITOターゲットを得、バッキングプレートとよばれ
る支持体にハンダなどを用いて貼りあわせる方法があ
る。しかしこの方法では複数のターゲットを貼りあわせ
るために、ターゲットの継ぎ目が異常放電の原因となる
などの悪影響が考えられる。
In the sputtering method, plasma controlled by a magnet collides with a target,
There is a problem that the target is subject to erosion along the shape of the magnet, and the usage efficiency is low. In order to improve the use efficiency, for example, JP-A-57-185973 and JP-A-60-39158 disclose that a target in which the thickness of a portion where the target is severely worn is increased is used. As a method of manufacturing a target in which a region to be subjected to erosion (hereinafter, referred to as "erosion region") is thickened, a plurality of flat plate-shaped targets having different thicknesses are molded by a die pressing method, and the targets are baked and processed to form an ITO target. Then, there is a method in which it is attached to a support called a backing plate using solder or the like. However, in this method, since a plurality of targets are bonded together, it is possible that the seams of the targets may cause abnormal discharge.

【0004】金型プレス法によってエロージョン領域を
厚高にした成形体を作成する方法も考えられるが、成形
体の厚高部分の密度低下が発生し、焼成によって得られ
る焼結体の厚高部分に、色むらや密度低下等の欠陥が発
生する。
A method of forming a molded body having a thick erosion region by a die pressing method is also conceivable. However, the density of the thick portion of the molded body is reduced, and the thick portion of the sintered body obtained by firing. In addition, defects such as color unevenness and density decrease occur.

【0005】石膏型を使用し、常圧でスラリーを注入す
る泥漿鋳込み法によってエロージョン領域を厚高にした
ターゲットを成形し、これを冷間静水圧プレスによって
均一化、圧密化させ、焼成、加工してITOターゲット
を作成する方法がある(例えば、特開平1−29076
4号公報)。しかしこの方法では、圧密化するために冷
間静水圧プレスを使用するためコスト高となる。
A gypsum mold is used to mold a target having a thick erosion region by a slurry casting method in which a slurry is injected at normal pressure, and this is homogenized and consolidated by a cold isostatic press, followed by firing and processing. Then, there is a method for producing an ITO target (for example, Japanese Patent Laid-Open No. 1-29076).
4 publication). However, this method is costly because a cold isostatic press is used for consolidation.

【0006】複合セラミックス等の高強度材料を成形型
に使用した高圧泥漿鋳込み法によって成形密度の均一な
成形体を得る方法がある(例えば特開平8−32571
6号公報)。しかしこれは平板型の成形例のみであり、
エロージヨン領域が厚高な形状の成形例がなく、さらに
成形密度の均一性に関する数値限定による良好な焼結体
が得られる具体的な説明がなされたものではない。
There is a method of obtaining a molded body having a uniform molding density by a high-pressure slurry casting method using a high-strength material such as composite ceramics in a molding die (for example, Japanese Unexamined Patent Publication No. 8-32571).
No. 6). However, this is only a flat plate type molding example,
There is no example of molding in which the erosion region has a thick shape, and moreover, no specific explanation has been given that a good sintered body can be obtained by the numerical limitation on the uniformity of the molding density.

【0007】[0007]

【発明が解決しようとする課題】本発明の目的は、使用
効率を高めるためにエロージョン領域が厚高な形状をも
ち、成形密度が均一なITO成形体をスラリー加圧泥漿
鋳込み法で安価に製造する方法を提供することにある。
SUMMARY OF THE INVENTION An object of the present invention is to inexpensively produce an ITO molded product having a thick erosion region and a uniform molding density by a slurry pressure slurry casting method in order to improve the use efficiency. To provide a way to do.

【0008】また本発明の他の目的は、成形密度の均一
性を数値で規定し、規定値内のITO成形体を焼成する
ことにより厚高部分に色むらや密度低下等の欠陥の無い
高密度ITO焼結体を製造する方法を提供することにあ
る。
Another object of the present invention is to specify the uniformity of the molding density numerically, and by firing the ITO molded body within the specified value, there is no defect such as color unevenness or density decrease in the thick portion. It is to provide a method for manufacturing a density ITO sintered body.

【0009】[0009]

【課題を解決するための手段】本発明者らは、泥漿鋳込
み法によって得られたエロージョン領域が厚高な形状を
もつITO成形体を切断、サンプリングしてITO成形
体の各部分の密度を測定し、密度むらが非常に小さくな
る成形条件を見い出した。ここで密度むらとは、測定し
た各部分の密度の最大値と最小値の差の、平均密度に対
する百分率として定義した。さらにITO成形体の密度
むらと、焼成によって得られた焼結体の欠陥を検討し、
エロージョン領域が厚高の形状をもつ良好な高密度の焼
結体を得るための成形体の条件を見い出した。ここでい
う焼結体の欠陥とは、厚高部分の凹凸(中央部分のへこ
み)、クラック、色むらのことである。
The inventors of the present invention measure the density of each part of the ITO molded body by cutting and sampling an ITO molded body having a thick erosion region obtained by a slurry casting method. Then, the molding conditions that the density unevenness becomes extremely small were found. Here, the density unevenness is defined as the percentage of the difference between the maximum value and the minimum value of the measured density of each part with respect to the average density. Furthermore, the density unevenness of the ITO molded body and the defects of the sintered body obtained by firing were examined,
The condition of the compact was found to obtain a good high-density sintered body having a thick and thick erosion region. The defects of the sintered body referred to here are irregularities in the thick portion (dents in the central portion), cracks, and color unevenness.

【0010】さらに、本発明者らは、酸化インジウム粉
の比表面積を限定することにより、緻密なITO成形体
が得られ、その結果ITO成形体が十分な強度を持ち乾
燥、脱脂、焼成工程でのハンドリングが容易となること
および良好な高密度の焼結体が得られることを見い出し
た。ここでいう比表面積とは、BET法で測定した値の
ことである。これらの知見に基づいて、本発明を完成す
るに至った。
Further, the inventors of the present invention can obtain a dense ITO molded body by limiting the specific surface area of the indium oxide powder, and as a result, the ITO molded body has sufficient strength in the drying, degreasing and firing steps. It has been found that it is easy to handle and that a good high density sintered body can be obtained. The specific surface area here is a value measured by the BET method. The present invention has been completed based on these findings.

【0011】本発明は、下記の事項をその特徴としてい
る。 (1)酸化インジウムと酸化錫からなるスラリーに圧力
3kg/cm2 以上で石膏型を用いて泥漿鋳込み成形し
て得られる、エロージョン領域が厚高な形状を持ち、密
度むらが1.5%以下であるITOの成形体。 (2)酸化インジウムと酸化錫からなるスラリーに圧力
10kg/cm2 以上で、樹脂及び無機粉体からなる型
を用いて泥漿鋳込み成形して得られる、エロージョン領
域が厚高な形状を持ち、密度むらが1.0%以下のIT
O成形体。 (3)比表面積3〜15m2 /gの酸化インジウムと、
比表面積1〜8m2 /gの酸化錫からなるスラリーに圧
力3kg/cm2 以上で泥漿鋳込み成形して得られる、
エロージョン領域が厚高な形状を持ち、密度むらが1.
5%以下で、かつ相対密度50%以上のITO成形体。 (4)比表面積3〜8m2 /gの酸化インジウムと、比
表面積1〜8m2 /g酸化錫からなるスラリーに圧力3
kg/cm2 以上で泥漿鋳込み成形して得られる、エロ
ージョン領域が厚高な形状を持ち、密度むらが1.5%
以下でかつ相対密度58%以上のITO成形体。
The present invention is characterized by the following items. (1) Slurry consisting of indium oxide and tin oxide, obtained by casting with a gypsum mold at a pressure of 3 kg / cm 2 or more, has a thick erosion region, and density unevenness of 1.5% or less. Which is a molded body of ITO. (2) The erosion region has a thick shape and a dense shape obtained by casting a slurry of indium oxide and tin oxide at a pressure of 10 kg / cm 2 or more using a mold made of resin and inorganic powder, IT with unevenness of 1.0% or less
O molded body. (3) Indium oxide having a specific surface area of 3 to 15 m 2 / g,
It is obtained by slurry-molding tin oxide having a specific surface area of 1 to 8 m 2 / g at a pressure of 3 kg / cm 2 or more.
The erosion area has a thick shape, and uneven density is 1.
An ITO molded product having a relative density of 5% or less and a relative density of 50% or more. (4) and indium oxide having a specific surface area of 3 to 8 m 2 / g, the pressure in the slurry comprising a specific surface area 1~8m 2 / g tin oxide 3
The erosion area is thick and has a density variation of 1.5%, which is obtained by casting with sludge at a pressure of more than kg / cm 2.
An ITO molded body having the following and a relative density of 58% or more.

【0012】(5)(a)原料として酸化インジウム粉
と酸化錫粉を用い、仮焼処理によって酸化インジウムの
比表面積を3〜15m2 /g、酸化錫の比表面積を1〜
8m2/gにする原料粉の仮焼工程、(b)仮焼した酸
化インジウムと酸化錫およびイオン交換水を樹脂製ポッ
トにいれ、乾式ボールミルで粉砕、混合し、その後水、
分散剤およびバインダーを加えて湿式ボールミルでスラ
リーを調製してスラリーの粘度を200cp以下、濃度
を65%以上にするスラリーの調製工程、(c)調製し
たスラリーに消泡剤を添加して滅圧脱気する工程、
(d)脱気したスラリーを成形型を用いた加圧による泥
漿鋳込み法により、エロージョン領域が厚高部分を有す
るITO成形体を成形する成形工程、および(e)厚高
部分を有するITO成形体を室温で乾燥後、脱脂炉を用
いて400〜600℃で脱脂する工程、からなることを
特徴とするITO成形体の製造方法。
(5) (a) Using indium oxide powder and tin oxide powder as raw materials, the specific surface area of indium oxide is 3 to 15 m 2 / g and the specific surface area of tin oxide is 1 to 1 by calcination treatment.
Calcination step of raw material powder to be 8 m 2 / g, (b) Put calcined indium oxide, tin oxide and ion-exchanged water into a resin pot, pulverize and mix with a dry ball mill, and then water,
A slurry is prepared by adding a dispersant and a binder with a wet ball mill so that the viscosity of the slurry is 200 cp or less and the concentration is 65% or more. (C) A defoaming agent is added to the prepared slurry to depressurize it. Degassing process,
(D) Molding step of molding an ITO molded body having a thick portion in the erosion region by a slurry casting method by pressurizing the degassed slurry with a molding die, and (e) an ITO molded body having a thick portion And a step of degreasing at 400 to 600 ° C. using a degreasing furnace after drying at room temperature.

【0013】(6)(d)工程において、成形型として
石膏型が使用され、スラリー加圧圧力が3kg/cm2
以上10kg/cm2 以下であり、エロージョン領域が
厚高部分を有するITO成形体の密度むらが1.5%以
下である前記(5)に記載のITO成形体の製造方法。 (7)(d)工程において、成形型として樹脂および無
機粉体からなる型が使用され、スラリー加圧圧力が10
kg/cm2 以上100kg/cm2 以下であり、エロ
ージョン領域が厚高部分を有するITO成形体の密度む
らが1.0%以下である前記(5)に記載のITO成形
体の製造方法。 (8)石膏型の表面、または樹脂および無機粉体からな
る型の表面に1〜10μmの気孔をもつ成形型を使用す
ることを特徴とする前記(6)または(7)に記載のI
TO成形体の製造方法。 (9)前記(1)〜(8)で得られたITO成形体に酸
素雰囲気下で1400〜1600℃の温度で焼成するこ
とを特徴とする相対密度98.5%以上のITO焼結体
の製造方法。
In step (6) and (d), a gypsum mold is used as a mold and the slurry pressure is 3 kg / cm 2.
The method for producing an ITO molded body according to (5) above, wherein the density is 10 kg / cm 2 or less and the density unevenness of the ITO molded body having an erosion region having a thick portion is 1.5% or less. (7) In the step (d), a mold made of resin and inorganic powder is used as the molding mold, and the slurry pressurizing pressure is 10
The method for producing an ITO molded body according to the above (5), wherein the density of the ITO molded body is not less than 100 kg / cm 2 and not more than 100 kg / cm 2 , and the density unevenness of the ITO molded body having a thick portion in the erosion region is 1.0% or less. (8) I according to the above (6) or (7), characterized in that a molding die having pores of 1 to 10 μm is used on the surface of the plaster mold or the surface of the mold made of resin and inorganic powder.
Method for manufacturing TO molded body. (9) An ITO sintered body having a relative density of 98.5% or more, which is obtained by firing the ITO molded body obtained in (1) to (8) above at a temperature of 1400 to 1600 ° C. in an oxygen atmosphere. Production method.

【0014】以下に、本発明を詳細に説明する。本発明
の泥漿鋳込み法によるITO成形体および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。 (a)原料粉の仮焼 原料粉としては、市販の酸化インジウム粉、酸化錫粉が
使用できる。原料粉が微粒で凝集しやすい場合は、仮焼
処理によって微粒子を粒成長させてもよい。仮焼処理に
よって酸化インジウムの比表面積を3〜15m2 /gに
すると、成形密度50%以上のITO成形体を得ること
ができる。また仮焼処理によって酸化インジウムの比表
面積を3〜8m2 /gにすると、成形密度58%以上の
ITO成形体を得ることができる。酸化錫の比表面積は
1〜8m2 /gが好ましい。
The present invention will be described in detail below. The steps of manufacturing the ITO molded body and the ITO sintered body by the slurry casting method of the present invention are as shown in FIG. The respective manufacturing steps will be described below. (A) As the calcined raw material powder of the raw material powder, commercially available indium oxide powder and tin oxide powder can be used. When the raw material powder is fine and easily aggregates, fine particles may be grown by calcination. When the specific surface area of indium oxide is set to 3 to 15 m 2 / g by the calcination treatment, an ITO molded body having a molding density of 50% or more can be obtained. When the specific surface area of indium oxide is set to 3 to 8 m 2 / g by the calcination treatment, an ITO molded body having a molding density of 58% or more can be obtained. The specific surface area of tin oxide is preferably 1 to 8 m 2 / g.

【0015】(b)ボールミルによる粉砕、混合 酸化インジウム、酸化錫、イオン交換水を樹脂製ポット
に入れ乾式ボールミルにより粉砕、混合する。酸化錫は
5〜10wt%が好ましい。その後、水および分散剤、
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る。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。スラリーの粘度は200c
p以下が好ましく、スラリーの濃度は65%以上が好ま
しい。
(B) Grinding with a ball mill, mixed Indium oxide, tin oxide, and ion-exchanged water are put into a resin pot and ground and mixed with a dry ball mill. The tin oxide content is preferably 5 to 10 wt%. Then water and dispersant,
A binder is added and a slurry is prepared by a wet ball mill. A container made of polyethylene, polypropylene, nylon, or the like can be used. Balls made of zirconia, resin, etc. can be used. As the dispersant, a polycarboxylic acid type can be used. As the binder, a wax emulsion type or an acrylic emulsion type can be used. The viscosity of the slurry is 200c
p or less is preferable, and the concentration of the slurry is preferably 65% or more.

【0016】(c)脱気 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。
(C) A defoaming agent is added to the degassed slurry and degassed under reduced pressure. As the defoaming agent, an amide type defoaming agent can be used.

【0017】(d)スラリーの泥漿鋳込み成形 脱気したスラリーを石膏あるいは樹脂及び無機粉体から
なる成形型を使用して泥漿鋳込み法により成形し、図2
に示す形状の成形体を得る。泥漿鋳込み成形とは、常圧
あるいは加圧によりスラリーを型に注入し、スラリー中
の水分を成形型の多孔質面を介して除き、成形体を得る
方法である。成形型としては、石膏型や樹脂及び無機粉
体からなる型が使用できる。
(D) Slurry Slurry Casting Molding The degassed slurry is molded by a slurry casting method using a molding die made of gypsum or resin and inorganic powder, as shown in FIG.
A molded product having the shape shown in is obtained. Slurry casting is a method in which the slurry is poured into a mold under normal pressure or pressure and the water content in the slurry is removed through the porous surface of the mold to obtain a molded body. As the mold, a plaster mold or a mold made of resin and inorganic powder can be used.

【0018】石膏型は、1〜10μmの気孔をもつ型が
使用できる。石膏型は吸水性に優れているためスラリー
を常圧で注入しても成形が可能であるが、厚高部分を有
する成形体を成形する場合、成形体の密度むらをなくす
ためには冷間静水圧プレス加工が必須である。本発明で
は冷間静水圧プレス加工を必要とせず、スラリー圧力3
kg/cm2 以上で成形することにより密度むら1.5
%以下の成形体が得られる。石膏型はその強度から10
kg/cm2 以下のスラリー圧力で成形することが好ま
しい。
As the gypsum mold, a mold having pores of 1 to 10 μm can be used. Since the plaster mold has excellent water absorption, it can be molded even if the slurry is injected at normal pressure.However, when molding a molded product with thick parts, cold molding is required to eliminate uneven density of the molded product. Hydrostatic pressing is essential. The present invention does not require cold isostatic pressing and does not require a slurry pressure of 3
Density unevenness is 1.5 by molding at more than kg / cm 2.
% Or less of the molded product is obtained. Gypsum mold is 10 because of its strength
It is preferable to mold at a slurry pressure of kg / cm 2 or less.

【0019】樹脂及び無機粉体からなる型は、吸水性、
通水性に乏しいためにスラリーを加圧して鋳込むのが好
ましく、また1〜10μmの気孔をもつものが使用でき
る。この型は、強度が高く、高圧でスラリーを注入し成
形時間を大幅に短縮することが可能である。またこの型
を使用して厚高部分を有する成形体を成形する場合、ス
ラリー圧力10kg/cm2 以上で成形することにより
密度むら1.0%以下の成形体が得られ、石膏型と比較
して成形時間を短縮できる。樹脂及び無機粉体からなる
型は、スラリーの漏れ、型固定治具のコストの問題から
スラリー圧力100kg/cm2 以下で使用することが
好ましい。
The mold made of resin and inorganic powder is
Since the water permeability is poor, it is preferable to pressurize the slurry for casting, and one having pores of 1 to 10 μm can be used. This mold has high strength and can inject the slurry at a high pressure to significantly shorten the molding time. Further, when a molded product having a thick portion is molded using this mold, a molded product having a density unevenness of 1.0% or less is obtained by molding at a slurry pressure of 10 kg / cm 2 or more. Molding time can be shortened. A mold made of resin and inorganic powder is preferably used at a slurry pressure of 100 kg / cm 2 or less from the viewpoint of leakage of slurry and cost of a mold fixing jig.

【0020】(e)成形体の乾燥、脱脂 ITO成形体は室温で乾燥された後、熱風循環式脱脂炉
等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。
(E) Drying and degreasing of the molded body After the ITO molded body is dried at room temperature, residual moisture and binder are removed using a hot air circulation type degreasing furnace or the like. The degreasing temperature is preferably 400 to 600 ° C.

【0021】(f)ITO成形体焼成成形体を酸素雰囲
気下焼成することにより相対密度98.5%以上のIT
O焼結体を得ることができる。焼成温度は1400〜1
600℃が好ましい。
(F) Baking of ITO molded body IT having a relative density of 98.5% or more is obtained by firing the molded body in an oxygen atmosphere.
An O sintered body can be obtained. The firing temperature is 1400-1
600 ° C. is preferred.

【0022】[0022]

【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7.1m2 /gの酸化インジウム粉2250g
と、比表面積3.4m2 /gの酸化錫粉250g、イオ
ン交換水75g及び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450gとポリカルボン酸系分散剤20gを入れ、1
時間ボールミルで混合した。1時間後にワックス系バイ
ンダー25gを添加し、19時間ボールミル混合を行っ
た。スラリーにアミド系消泡剤1.3gを添加し減圧脱
気を行った。このスラリーの濃度は81%だった。
EXAMPLES The present invention will be further described below with reference to Examples and Comparative Examples. Example 1 2250 g of indium oxide powder having a specific surface area of 7.1 m 2 / g
Then, 250 g of tin oxide powder having a specific surface area of 3.4 m 2 / g, 75 g of ion-exchanged water and zirconia balls were put in a resin pot and mixed by a ball mill for 20 hours. Next, add 450 g of ion-exchanged water and 20 g of polycarboxylic acid-based dispersant, and add 1
Mix in ball mill for hours. After 1 hour, 25 g of a wax-based binder was added and ball mill mixing was performed for 19 hours. 1.3 g of an amide defoaming agent was added to the slurry and degassing under reduced pressure was performed. The concentration of this slurry was 81%.

【0023】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)×100 次に石膏型を用いてスラリー圧力4.0kg/m2 、成
形時間60分の条件で泥漿鋳込み成形し、成形サイズ2
45×245×11t(5t)のITO成形体を得た。
成形体は室温で乾燥後、600℃で3時間脱脂を行っ
た。成形体を、図3に示す位置で切断し、平板(5t)
部分、テーパー部分(5.11t部分)、厚高部分(1
1t部分)から約20mm角の大きさにサンプリングし
て試料とした。成形体1枚から試料を60個以上サンプ
リングした。
The definition of the slurry concentration is as follows. Slurry concentration (%) = solute weight / (solute weight + solvent weight) × 100 Next, using a gypsum mold, slurry casting was performed under the conditions of a slurry pressure of 4.0 kg / m 2 and a molding time of 60 minutes, and a molding size of 2
An ITO molded body of 45 × 245 × 11t (5t) was obtained.
The molded body was dried at room temperature and then degreased at 600 ° C. for 3 hours. The molded body is cut at the position shown in FIG. 3 to obtain a flat plate (5t).
Part, tapered part (5.11t part), thick part (1
Samples were obtained by sampling from the 1t portion) to a size of about 20 mm square. 60 or more samples were sampled from one molded body.

【0024】次に、サンプリングした試料の表面を清浄
にし、質量を測定した。さらに試料に防水処理を施すた
めに油に浸し、その後油を軽く拭きとり、試料を針金等
で水中に吊したときの天秤の読みを測定し、成形密度を
求めた。
Next, the surface of the sampled sample was cleaned and the mass was measured. Further, the sample was immersed in oil for waterproofing, and then the oil was wiped lightly, and the reading of the balance when the sample was suspended in water with a wire or the like was measured to obtain the molding density.

【0025】成形密度の計算方法は、式1による。The calculation method of the molding density is according to the equation 1.

【式1】 ただし、 D:成形密度(%) A:試料の質量(g) B:防水処理した試料の質量(g) C:防水処理した試料を水中に吊したときの天秤の読み
(g) ρ:試験温度における水の密度(g/cm3 ) ITOの真密度を7.15(g/cm3 )とし、各サン
プルの成形密度から密度むらを求めた。
[Formula 1] However, D: Molding density (%) A: Mass of sample (g) B: Mass of waterproofed sample (g) C: Reading of balance when suspending waterproofed sample in water (g) ρ: Test Density of water at temperature (g / cm 3 ) The true density of ITO was 7.15 (g / cm 3 ), and the density unevenness was determined from the molding density of each sample.

【0026】密度むらの計算方法は、式2による。The calculation method of the density unevenness is based on Equation 2.

【式2】 ただし、 ΔD:密度むら(%) Dmax :成形密度最大値(%) Dmin :成形密度最小値(%) Dave :成形密度の平均値(%)[Formula 2] However, ΔD: Density unevenness (%) D max : Molding density maximum value (%) D min : Molding density minimum value (%) D ave : Molding density average value (%)

【0027】成形密度及び密度むらの測定結果を、表1
に示す。脱脂した成形体の1/2を酸素雰囲気にて15
50℃で8時間焼成しITO焼結体を得た。ITO焼結
体の密度、焼結体の欠陥の有無について、表2に示す。
The measurement results of the molding density and the density unevenness are shown in Table 1.
Shown in. ½ of the degreased compact in oxygen atmosphere
It was baked at 50 ° C. for 8 hours to obtain an ITO sintered body. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0028】焼成密度の計算方法は、次の通りである。 密度(%)=重量/体積/7.15×100 成形密度分布を測定するときの試料のサンプリング方法
を、図3に示す。成形体を長軸(L)方向に1/2に切
断し、片側について厚さ別に1〜6の部分に切断する。
The method for calculating the firing density is as follows. Density (%) = weight / volume / 7.15 × 100 The sampling method of the sample when measuring the molding density distribution is shown in FIG. The molded body is cut in half in the direction of the long axis (L), and cut on one side into 1 to 6 parts according to thickness.

【0029】実施例2 比表面積14.7m2 /gの酸化インジウム粉と比表面
積3.2m2 /gの酸化錫粉を使用して泥漿鋳込み成形
した以外は実施例1と同様に成形し、成形密度、密度む
らを測定し、その後焼成した。成形密度、密度むらの測
定結果を、表1に示す。ITO焼結体の密度、焼結体の
欠陥の有無について、表2に示す。
[0029] is molded in the same manner as in Example 1 except that the molded inclusive mud漿鋳using tin oxide powder of the indium oxide powder and a specific surface area of 3.2 m 2 / g of Example 2 specific surface area 14.7 m 2 / g, The molding density and the density unevenness were measured, and then firing was performed. Table 1 shows the measurement results of the molding density and the density unevenness. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0030】実施例3 比表面積3.2m2 /gの酸化インジウム粉と比表面積
3.2m2 /gの酸化錫粉を使用し、スラリー圧力4.
0kg/cm2 、成形時間60分で泥漿鋳込み成形した
以外は実施例1と同様に成形し、成形密度、密度むらを
測定し、焼成した。成形密度、密度むらの測定結果を、
表1に示す。ITO焼結体の密度、焼結体の欠陥の有無
について、表2に示す。
[0030] Using the tin oxide powder of the indium oxide powder and a specific surface area of 3.2 m 2 / g Example 3 specific surface area of 3.2 m 2 / g, the slurry pressure 4.
Molding was performed in the same manner as in Example 1 except that the slurry was cast and molded at 0 kg / cm 2 and the molding time was 60 minutes, and the molding density and the density unevenness were measured, and firing was performed. Measurement results of molding density and density unevenness
It shows in Table 1. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0031】実施例4 比表面積6.8m2 /gの酸化インジウム粉5400g
と比表面積2.5m2/gの酸化錫粉600g、イオン
交換水180g及び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1080gとポリカルボン酸系分散剤48g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60gを添加し19時間ボールミル混合を行った。
スラリーにアミド系消泡剤3gを添加し、減圧脱気を行
った。このスラリーの濃度は81%であった。
Example 4 5400 g of indium oxide powder having a specific surface area of 6.8 m 2 / g
Then, 600 g of tin oxide powder having a specific surface area of 2.5 m 2 / g, 180 g of ion-exchanged water and zirconia balls were put in a resin pot and mixed by a ball mill for 20 hours. Next, add 1080 g of ion-exchanged water and 48 g of polycarboxylic acid type dispersant, and add 1
Ball mill mixed for hours. After 1 hour, 60 g of a wax binder was added and ball mill mixing was performed for 19 hours.
The slurry was degassed under reduced pressure by adding 3 g of an amide defoaming agent. The concentration of this slurry was 81%.

【0032】次に樹脂及び無機粉体からなる型を用いて
スラリー圧力4.0kg/cm2 、成形時間60分の条
件で泥漿鋳込み成形し、成形サイズ730×252×1
1t(5t)mmの成形体を得た。成形体は室温で乾燥
後、600℃で3時間脱脂を行った。脱脂後に実施例1
と同じ方法で成形密度、密度むらを求めた。成形密度、
密度むらの測定結果を、表1に示す。脱脂した成形体を
実施例1と同様の方法で焼成した。ITO焼結体の密
度、焼結体の欠陥の有無について、表2に示す。
Next, using a mold made of resin and inorganic powder, slurry casting was carried out under the conditions of a slurry pressure of 4.0 kg / cm 2 and a molding time of 60 minutes, and a molding size of 730 × 252 × 1.
A molded product of 1 t (5 t) mm was obtained. The molded body was dried at room temperature and then degreased at 600 ° C. for 3 hours. Example 1 after degreasing
The molding density and the density unevenness were determined by the same method as described above. Molding density,
Table 1 shows the measurement results of the density unevenness. The degreased compact was fired in the same manner as in Example 1. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0033】実施例5 比表面積6.0m2 /gの酸化インジウム粉と比表面積
2.5m2 /gの酸化錫粉を使用し、スラリー圧力1
0.0kg/cm2 で泥漿鋳込み成形した以外は実施例
4と同様に成形し、成形密度、密度むらを測定し、焼成
した。成形密度、密度むらの測定結果を、表1に示す。
ITO焼結体の密度、焼結体の欠陥の有無について、表
2に示す。
[0033] Using the tin oxide powder of the indium oxide powder and a specific surface area of 2.5 m 2 / g in Example 5 specific surface area of 6.0 m 2 / g, the slurry pressure 1
Molding was carried out in the same manner as in Example 4 except that sludge casting was carried out at 0.0 kg / cm 2 , and the molding density and density unevenness were measured and fired. Table 1 shows the measurement results of the molding density and the density unevenness.
Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0034】実施例6 比表面積6.5m2 /gの酸化インジウム粉と比表面積
3.3m2 /gの酸化錫粉を使用し、スラリー圧力1
5.0kg/cm2 で泥漿鋳込み成形した以外は実施例
4と同様に成形し、成形密度を測定し、焼成した。IT
O焼結体の密度、焼結体の欠陥の有無について、表2に
示す。
[0034] Using the tin oxide powder of the indium oxide powder and a specific surface area of 3.3 m 2 / g of Example 6 specific surface area 6.5m 2 / g, the slurry pressure 1
Molding was performed in the same manner as in Example 4 except that the slurry was cast at 5.0 kg / cm 2 , and the molding density was measured and fired. IT
Table 2 shows the density of the O sintered body and the presence or absence of defects in the sintered body.

【0035】実施例7 比表面積6.9m2 /gの酸化インジウム粉と比表面積
3.0m2 /gの酸化錫粉を使用し、スラリー圧力2
2.0kg/cm2 で泥漿鋳込み成形した以外は実施例
4と同様に成形し、成形密度、密度むらを測定し、焼成
した。成形密度、密度むらの測定結果を表1に示す。I
TO焼結体の密度、焼結体の欠陥の有無について、表2
に示す。
[0035] Using the tin oxide powder of the indium oxide powder and a specific surface area of 3.0 m 2 / g Example 7 specific surface area 6.9 m 2 / g, the slurry pressure 2
Molding was performed in the same manner as in Example 4 except that the slurry was cast at 2.0 kg / cm 2 , and the molding density and density unevenness were measured and fired. Table 1 shows the measurement results of the molding density and the density unevenness. I
Table 2 shows the density of the TO sintered body and the presence or absence of defects in the sintered body.
Shown in.

【0036】比較例1 比表面積7.1m2 /gの酸化インジウム粉と比表面積
3.1m2 /gの酸化錫粉を使用し、スラリー圧力1.
0kg/cm2 で泥漿鋳込み成形した以外は実施例1と
同様に成形し、成形密度、密度むらを測定した。成形密
度、密度むらの測定結果を表1に示す。ITO成形体の
厚高部分に凹凸が生じ、これにより研削加工代の増大が
必要となった。
[0036] Using the tin oxide powder of the indium oxide powder and a specific surface area of 3.1m 2 / g of Comparative Example 1 specific surface area of 7.1 m 2 / g, the slurry pressure 1.
Molding was performed in the same manner as in Example 1 except that the slurry was cast at 0 kg / cm 2 , and the molding density and density unevenness were measured. Table 1 shows the measurement results of the molding density and the density unevenness. Irregularities were formed in the thick part of the ITO molded body, which required an increase in the grinding allowance.

【0037】比較例2 比表面積6.8m2 /gの酸化インジウム粉と比表面積
2.5m2 /gの酸化錫粉を使用し、スラリー圧力1.
5kg/cm2 、成形時間230分で泥漿鋳込み成形し
た以外は実施例1と同様に成形し、成形密度、密度むら
を測定した。成形密度、密度むらの測定結果を表1に示
す。ITO焼結体の密度、焼結体の欠陥の有無について
表2に示す。
[0037] Using the tin oxide powder of the indium oxide powder and a specific surface area of 2.5 m 2 / g of Comparative Example 2 specific surface area of 6.8 m 2 / g, the slurry pressure 1.
Molding was carried out in the same manner as in Example 1 except that sludge casting was carried out at 5 kg / cm 2 for 230 minutes, and the molding density and density unevenness were measured. Table 1 shows the measurement results of the molding density and the density unevenness. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0038】比較例3 比表面積6.9m2 /gの酸化インジウム粉と比表面積
3.0m2 /gの酸化錫粉を使用し、スラリー圧力1.
5kg/cm2 で泥漿鋳込み成形した以外は実施例1と
同様に成形し、成形密度、密度むらを測定した。成形密
度、密度むらの測定結果を表1に示す。ITO成形体の
厚高部分に凹凸が生じ、これにより研削加工代の増大が
必要となった。
[0038] Using the tin oxide powder of the indium oxide powder and a specific surface area of 3.0 m 2 / g of Comparative Example 3 specific surface area of 6.9 m 2 / g, the slurry pressure 1.
Molding was performed in the same manner as in Example 1 except that the slurry was cast at 5 kg / cm 2 , and the molding density and density unevenness were measured. Table 1 shows the measurement results of the molding density and the density unevenness. Irregularities were formed in the thick part of the ITO molded body, which required an increase in the grinding allowance.

【0039】比較例4 比表面積6.0m2 /gの酸化インジウム粉と比表面積
2.5m2 /gの酸化錫粉を使用し、スラリー圧力2.
0kg/cm2 で泥漿鋳込み成形した以外は実施例1と
同様に成形し、成形密度、密度むらを測定した。成形密
度、密度むらの測定結果を表1に示す。成形体に25m
mのクラックがあった。
[0039] Using the tin oxide powder of the indium oxide powder and a specific surface area of 2.5 m 2 / g in Comparative Example 4 specific surface area of 6.0 m 2 / g, the slurry pressure 2.
Molding was performed in the same manner as in Example 1 except that the slurry was cast at 0 kg / cm 2 , and the molding density and density unevenness were measured. Table 1 shows the measurement results of the molding density and the density unevenness. 25m for molded body
There were m cracks.

【0040】比較例5 比表面積6.3m2 /gの酸化インジウム粉5400g
と比表面積2.5m2/gの酸化錫粉600g、イオン
交換水180g及び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1080gとポリカルボン酸系分散剤48g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60gを添加し、19時間ボールミル混合を
行った。スラリーにアミド系消泡剤3gを添加し減圧脱
気を行った。このスラリーの濃度は81%だった。
Comparative Example 5 5400 g of indium oxide powder having a specific surface area of 6.3 m 2 / g
Then, 600 g of tin oxide powder having a specific surface area of 2.5 m 2 / g, 180 g of ion-exchanged water and zirconia balls were put in a resin pot and mixed for 20 hours with a ball mill. Next, 1080 g of ion-exchanged water and 48 g of a polycarboxylic acid-based dispersant were added and mixed by a ball mill for 1 hour. After 1 hour, 60 g of a wax-based binder was added and ball mill mixing was performed for 19 hours. The slurry was degassed under reduced pressure by adding 3 g of an amide-based defoaming agent. The concentration of this slurry was 81%.

【0041】次に石膏型を用いてスラリー圧力1.0k
g/cm2 、成形時間90分の条件で泥漿鋳込み成形
し、成形サイズ715×250×11t(5t)mmの
成形体を得た。成形体は室温で乾燥後、600℃で3時
間脱脂を行った。成形密度は58.2%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I
TO焼結体を得た。ITO焼結体の密度、焼結体の欠陥
の有無について表2に示す。
Next, using a plaster mold, the slurry pressure was 1.0 k.
Slurry casting was carried out under the conditions of g / cm 2 and molding time of 90 minutes to obtain a molded product having a molding size of 715 × 250 × 11t (5t) mm. The molded body was dried at room temperature and then degreased at 600 ° C. for 3 hours. The molding density was 58.2%. The degreased compact is fired in an oxygen atmosphere at 1550 ° C. for 8 hours I
A TO sintered body was obtained. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0042】比較例6 比表面積7.1m2 /gの酸化インジウム粉と比表面積
3.1m2 /gの酸化錫粉を使用し、スラリー圧力1.
0kg/cm2 、成形時間50分で泥漿鋳込み成形した
以外は実施例1と同様に成形し、成形密度を測定し、焼
成した。成形密度は59.4%だった。ITO焼結体の
密度、焼結体の欠陥の有無について表2に示す。
[0042] Using the tin oxide powder of the indium oxide powder and a specific surface area of 3.1m 2 / g of Comparative Example 6 specific surface area of 7.1 m 2 / g, the slurry pressure 1.
Molding was carried out in the same manner as in Example 1 except that sludge casting was carried out at 0 kg / cm 2 and molding time of 50 minutes, the molding density was measured, and firing was carried out. The molding density was 59.4%. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0043】比較例7 比表面積6.4m2 /gの酸化インジウム粉と比表面積
3.0m2 /gの酸化錫粉を使用し、スラリー圧力2.
0kg/cm2 、成形時間90分で泥漿鋳込み成形した
以外は実施例1と同様に成形し、成形密度を測定し、焼
成した。成形密度は57.8%だった。ITO焼結体の
密度、焼結体の欠陥の有無について表2に示す。
[0043] Using the tin oxide powder of the indium oxide powder and a specific surface area of 3.0 m 2 / g of Comparative Example 7 specific surface area of 6.4 m 2 / g, the slurry pressure 2.
Molding was carried out in the same manner as in Example 1 except that sludge casting was carried out at 0 kg / cm 2 and molding time of 90 minutes, the molding density was measured, and firing was carried out. The molding density was 57.8%. Table 2 shows the density of the ITO sintered body and the presence or absence of defects in the sintered body.

【0044】成形時のスラリー圧力、成形時間、成形密
度、密度むらの値を表1に示す。スラリー圧力3kg/
cm2 以上で成形した場合、密度むらが1.5%以下の
非常に均一な成形体が得られる。樹脂及び無機粉体から
なる型を使用して、スラリー圧力10kg/cm2 以上
で成形すると密度むらが1.0%以下の成形体が得ら
れ、成形時間が短縮できるという利点がある。
Table 1 shows the values of slurry pressure, molding time, molding density and density unevenness during molding. Slurry pressure 3kg /
When molded with a cm 2 or more, a very uniform molded body having a density unevenness of 1.5% or less can be obtained. When a mold made of resin and inorganic powder is used and molded at a slurry pressure of 10 kg / cm 2 or more, a molded product having a density unevenness of 1.0% or less is obtained, and there is an advantage that the molding time can be shortened.

【0045】比表面積3〜15m2 /gの酸化インジウ
ムと、酸化錫からなるスラリーをスラリー加圧3kg/
cm2 以上で泥漿鋳込み成形することにより、エロージ
ョン領域が厚高な形状を持ち、密度むらが1.5%以下
であり、相対密度50%以上の成形体が得られる。また
比表面積3〜8m2 /gの酸化インジウムと、酸化錫か
らなるスラリーをスラリー加圧3kg/cm2 以上で泥
漿鋳込み成形することにより、エロージョン領域が厚高
な形状を持ち、密度むらが1.5%以下であり、相対密
度58%以上の成形体が得られる。
A slurry composed of indium oxide having a specific surface area of 3 to 15 m 2 / g and tin oxide was applied with a slurry pressure of 3 kg /
By sludge casting at cm 2 or more, a molded product having a thick erosion region, density unevenness of 1.5% or less, and relative density of 50% or more can be obtained. Further, by injecting a slurry of indium oxide having a specific surface area of 3 to 8 m 2 / g and tin oxide at a slurry pressure of 3 kg / cm 2 or more, the erosion region has a thick shape and density unevenness is 1 A molded product having a relative density of not more than 0.5% and a relative density of not less than 58% is obtained.

【0046】スラリー圧力と焼成密度、焼成後の欠陥の
関係を表2に示す。スラリー圧力1〜2kg/cm2
成形した密度むらが1.8%以上ある成形体では、焼成
により表面の色むら、厚高部分の凹凸、クラック等が発
生しやすい。スラリー圧力3kg/cm2 以上で成形し
た密度むらが1.0%以下の成形体では表面の色むら、
厚高部分の凹凸、クラック等の欠陥は発生しない。
Table 2 shows the relationship between the slurry pressure, the firing density, and the defects after firing. A molded product molded with a slurry pressure of 1 to 2 kg / cm 2 and having a density unevenness of 1.8% or more is liable to cause color unevenness on the surface, unevenness of thick portions, cracks and the like due to firing. In the case of a molded body having a density unevenness of 1.0% or less formed by a slurry pressure of 3 kg / cm 2 or more, surface unevenness of color,
No defects such as unevenness and cracks in the thick portion occur.

【0047】実施例および比較例において測定したスラ
リー圧力と成形体の密度むらの関係を、図4に示す。
FIG. 4 shows the relationship between the slurry pressure measured in Examples and Comparative Examples and the density unevenness of the molded body.

【0048】成形体の密度分布について図5及び図6に
示す。図5はスラリー圧力1.5kg/cm2 で成形し
た成形体の形状と成形密度の関係を示す。スラリー圧力
1.5kg/cm2 で成形した場合、厚高部分の脱水が
不十分となり成形密度が低くなる。成形密度が低い箇所
では焼成による収縮率が大きく、焼成密度も低くなるた
め凹凸や色むらが発生しやすい。また成形体の端面及び
厚高部分で密度のばらつき(標準偏差)が大きく、焼成
時の収縮の差によるクラックが発生しやすい。
The density distribution of the molded body is shown in FIGS. 5 and 6. FIG. 5 shows the relationship between the shape and the molding density of a molded body molded at a slurry pressure of 1.5 kg / cm 2 . In the case of molding with a slurry pressure of 1.5 kg / cm 2 , dehydration of the thick portion becomes insufficient and the molding density becomes low. In a portion where the molding density is low, the shrinkage rate due to firing is large, and the firing density is also low, so unevenness and uneven color are likely to occur. Further, the density variation (standard deviation) is large on the end face and the thick portion of the molded body, and cracks are likely to occur due to the difference in shrinkage during firing.

【0049】図6にスラリー圧力22kg/cm2 で成
形した成形体の厚さ形状と成形密度の関係を示す。スラ
リー圧力22kg/cm2 で成形した場合、厚高部分の
脱水が十分に行われるため厚さによらず成形密度がほぼ
均一になる。このような成形体では焼成による収縮の
差、密度むらが小さく欠陥のない良好な焼結体が得られ
る。尚、スラリー圧力4kg/cm2 以上で成形した成
形体の形状と成形密度の関係は図6と同様の結果にな
る。
FIG. 6 shows the relationship between the thickness shape and the molding density of a molded body molded at a slurry pressure of 22 kg / cm 2 . In the case of molding at a slurry pressure of 22 kg / cm 2 , the high density portion is sufficiently dehydrated, so that the molding density becomes substantially uniform regardless of the thickness. With such a compact, it is possible to obtain a good sintered body that has no difference in shrinkage due to firing and uneven density and has no defects. The relationship between the shape and the molding density of the molded body molded at a slurry pressure of 4 kg / cm 2 or more has the same result as in FIG.

【0050】[0050]

【表1】 [Table 1]

【0051】[0051]

【表2】 [Table 2]

【0052】[0052]

【発明の効果】本発明によれば、泥漿鋳込み成形法にお
ける酸化インジウム粉の比表面積を限定しスラリー圧力
を適正範囲に選択することにより冷間静水圧プレス加工
を必要とせず、エロージョン領域を厚高にした形状をも
つ密度むらが小さく、厚高部に凹凸のないITO成形体
が得られる。このITO成形体を酸素雰囲気下で焼成す
ることにより良好な高密度焼結体が得られる。
According to the present invention, by limiting the specific surface area of the indium oxide powder in the slurry casting method and selecting the slurry pressure within an appropriate range, cold isostatic pressing is not required and the erosion area can be thickened. It is possible to obtain an ITO molded body having a heightened shape with small density unevenness and no unevenness in the thick portion. A good high density sintered body can be obtained by firing this ITO molded body in an oxygen atmosphere.

【0053】[0053]

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明に係る加圧鋳込み法によるITOターゲ
ットの製造工程及び密度測定試料のサンプリングに関す
る説明図である。
FIG. 1 is an explanatory diagram relating to a manufacturing process of an ITO target by a pressure casting method according to the present invention and sampling of a density measurement sample.

【図2】本発明の泥漿鋳込み法で得られる成形体の形状
を説明する図である。
FIG. 2 is a diagram illustrating the shape of a molded product obtained by the sludge casting method of the present invention.

【図3】成形密度分布を測定するときの試料のサンプリ
ング方法を示す図である。
FIG. 3 is a diagram showing a sampling method of a sample when measuring a molding density distribution.

【図4】スラリー圧力と成形体の密度むらの関係を示す
図である。
FIG. 4 is a diagram showing a relationship between slurry pressure and density unevenness of a molded body.

【図5】スラリー圧力1〜2kg/cm2 で成形したと
きの厚さ形状と成形密度の関係を比較例2のデータを用
いて示した図である。
FIG. 5 is a diagram showing the relationship between the thickness shape and the molding density when molded under a slurry pressure of 1 to 2 kg / cm 2 , using the data of Comparative Example 2.

【図6】スラリー圧力4kg/cm2 以上で成形したと
きの厚さ形状と成形密度の関係を実施例7のデータを用
いて示した図である。
FIG. 6 is a diagram showing the relationship between the thickness profile and the molding density when molded at a slurry pressure of 4 kg / cm 2 or more, using the data of Example 7.

【符号の説明】[Explanation of symbols]

斜線 厚高部分 横線 平板部分 L 長軸長さ W 短軸長さ T1 厚高部分厚さ T2 平板部分厚さ Diagonal line Thick part Horizontal line Flat plate part L major axis length W Short axis length T1 Thickness High part thickness T2 flat plate thickness

───────────────────────────────────────────────────── フロントページの続き Fターム(参考) 4G030 AA34 AA39 BA02 BA15 CA07 CA08 GA08 GA09 GA14 GA16 GA18 GA20 GA25 GA27 GA33 PA21 4G052 CA05 CB14 CC02 CC05 CC15 4K029 BA45 BA47 BC09 DC05 DC09 DC12 5G323 BA02 BB06 BC01    ─────────────────────────────────────────────────── ─── Continued front page    F-term (reference) 4G030 AA34 AA39 BA02 BA15 CA07                       CA08 GA08 GA09 GA14 GA16                       GA18 GA20 GA25 GA27 GA33                       PA21                 4G052 CA05 CB14 CC02 CC05 CC15                 4K029 BA45 BA47 BC09 DC05 DC09                       DC12                 5G323 BA02 BB06 BC01

Claims (9)

【特許請求の範囲】[Claims] 【請求項1】酸化インジウムと酸化錫からなるスラリー
に圧力3kg/cm2 以上で石膏型を用いて泥漿鋳込み
成形して得られる、エロージョン領域が厚高な形状を持
ち、密度むらが1.5%以下であることを特徴とするI
TO成形体。
1. An erosion region having a thick shape and a density unevenness of 1.5, which is obtained by molding a slurry of indium oxide and tin oxide at a pressure of 3 kg / cm 2 or more using a gypsum mold. % Or less I
TO molded body.
【請求項2】酸化インジウムと酸化錫からなるスラリー
に圧力10kg/cm2 以上で樹脂及び無機粉体からな
る型を用いて泥漿鋳込み成形して得られる、エロージョ
ン領域が厚高な形状を持ち、密度むらが1.0%以下で
あることを特徴とするITO成形体。
2. An erosion region having a thick shape obtained by casting a slurry of indium oxide and tin oxide at a pressure of 10 kg / cm 2 or more using a mold made of resin and inorganic powder, An ITO molded product having a density unevenness of 1.0% or less.
【請求項3】比表面積3〜15m2 /gの酸化インジウ
ムと、比表面積1〜8m2 /gの酸化錫からなるスラリ
ーに圧力3kg/cm2 以上で泥漿鋳込み成形して得ら
れる、エロージョン領域が厚高な形状を持ち、密度むら
が1.5%以下で、かつ相対密度50%以上であること
を特徴とするITO成形体。
And indium oxide wherein a specific surface area 3~15m 2 / g, obtained by molding inclusive mud漿鋳at a pressure 3 kg / cm 2 or more slurry comprising tin oxide having a specific surface area 1~8m 2 / g, the erosion region Has a thick shape and has an uneven density of 1.5% or less and a relative density of 50% or more.
【請求項4】比表面積3〜8m2 /gの酸化インジウム
と、比表面積1〜8m2 /gの酸化錫からなるスラリー
に圧力3kg/cm2 以上で泥漿鋳込み成形して得られ
る、エロージョン領域が厚高な形状を持ち、密度むらが
1.5%以下で、かつ相対密度58%以上であることを
特徴とするITOの成形体。
And indium oxide wherein a specific surface area of 3 to 8 m 2 / g, obtained by molding inclusive mud漿鋳at a pressure 3 kg / cm 2 or more slurry comprising tin oxide having a specific surface area 1~8m 2 / g, the erosion region Has a thick shape and has a density unevenness of 1.5% or less and a relative density of 58% or more.
【請求項5】(a)原料として酸化インジウム粉と酸化
錫粉を用い、酸化インジウムの比表面積を3〜15m2
/g、酸化錫の比表面積を1〜8m2 /gに仮焼処理す
る原料粉の仮焼工程、 (b)仮焼した酸化インジウムと酸化錫およびイオン交
換水を樹脂製ポットに入れ、乾式ボールミルで粉砕、混
合し、その後水、分散剤およびバインダーを加えて湿式
ボールミルでスラリーを調製してスラリーの粘度を20
0cp以下、濃度を65%以上にするスラリーの調製工
程、 (c)調製したスラリーに消泡剤を添加して滅圧脱気す
る工程、 (d)脱気したスラリーを成形型を用いた加圧による泥
漿鋳込み法により、エロージョン領域が厚高部分を有す
るITO成形体を成形する成形工程、および(e)厚高
部分を有するITO成形体を室温で乾燥後、脱脂炉を用
いて400〜600℃で脱脂する工程、からなることを
特徴とするITO成形体の製造方法。
5. (a) Indium oxide powder and tin oxide powder are used as raw materials, and the specific surface area of indium oxide is 3 to 15 m 2.
/ G, a calcination step of the raw material powder for calcination so that the specific surface area of tin oxide is 1 to 8 m 2 / g, (b) The calcined indium oxide, tin oxide, and ion-exchanged water are put in a resin pot and dried. Grind and mix with a ball mill, and then add water, a dispersant and a binder to prepare a slurry with a wet ball mill to adjust the viscosity of the slurry to 20.
0 cp or less, a step of preparing a slurry having a concentration of 65% or more, (c) a step of adding an antifoaming agent to the prepared slurry to degas it under pressure, and (d) adding the degassed slurry using a molding die. A molding step of molding an ITO molded body having a thick portion in an erosion region by a slurry casting method by pressure, and (e) 400 to 600 using a degreasing furnace after drying the ITO molded body having a thick portion at room temperature. A method for producing an ITO molded body, which comprises a step of degreasing at ℃.
【請求項6】(d)工程において、成形型として石膏型
が使用され、スラリー加圧圧力が3kg/cm2 以上1
0kg/cm2 以下であり、エロージョン領域が厚高部
分を有するITO成形体の密度むらが1.5%以下であ
ることを特徴とする請求項5に記載のITO成形体の製
造方法。
6. A gypsum mold is used as a mold in the step (d), and the slurry pressure is 3 kg / cm 2 or more.
The method for producing an ITO molded body according to claim 5, wherein the density is 0 kg / cm 2 or less, and the density unevenness of the ITO molded body having an erosion region having a thick portion is 1.5% or less.
【請求項7】(d)工程において、成形型として樹脂お
よび無機粉体からなる型が使用され、スラリー加圧圧力
が10kg/cm2 以上100kg/cm2 以下であ
り、エロージョン領域が厚高部分を有するITO成形体
の密度むらが1.0%以下であることを特徴とする請求
項5に記載のITO成形体の製造方法。
7. In the step (d), a mold made of resin and inorganic powder is used as a molding mold, the slurry pressure is 10 kg / cm 2 or more and 100 kg / cm 2 or less, and the erosion region is a thick portion. 6. The method for producing an ITO molded body according to claim 5, wherein the density unevenness of the ITO molded body having the above is 1.0% or less.
【請求項8】石膏型の表面、または樹脂および無機粉体
からなる型の表面に1〜10μmの気孔をもつ成形型を
使用することを特徴とする請求項6または7に記載のI
TO成形体の製造方法。
8. The mold according to claim 6, wherein a molding die having pores of 1 to 10 μm is used on the surface of the plaster mold or the surface of the mold made of resin and inorganic powder.
Method for manufacturing TO molded body.
【請求項9】請求項1〜8で得られたITO成形体を酸
素雰囲気下で1400〜1600℃の温度で焼成するこ
とを特徴とする相対密度98.5%以上のITO焼結体
の製造方法。
9. Production of an ITO sintered body having a relative density of 98.5% or more, which comprises firing the ITO molded body obtained in any one of claims 1 to 8 at a temperature of 1400 to 1600 ° C. in an oxygen atmosphere. Method.
JP10237499A 1998-08-24 1998-08-24 Ito molding and manufacture thereof and manufacture of ito sintered body Pending JP2000061917A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP10237499A JP2000061917A (en) 1998-08-24 1998-08-24 Ito molding and manufacture thereof and manufacture of ito sintered body

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP10237499A JP2000061917A (en) 1998-08-24 1998-08-24 Ito molding and manufacture thereof and manufacture of ito sintered body

Publications (1)

Publication Number Publication Date
JP2000061917A true JP2000061917A (en) 2000-02-29

Family

ID=17016232

Family Applications (1)

Application Number Title Priority Date Filing Date
JP10237499A Pending JP2000061917A (en) 1998-08-24 1998-08-24 Ito molding and manufacture thereof and manufacture of ito sintered body

Country Status (1)

Country Link
JP (1) JP2000061917A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2004090051A1 (en) * 2003-04-09 2006-07-06 株式会社ホソカワ粉体技術研究所 Powder coating production method and powder coating obtained by the production method
JP2008255480A (en) * 2007-03-09 2008-10-23 Mitsubishi Materials Corp Vapor deposition material and manufacturing method therefor
GB2482544A (en) * 2010-08-06 2012-02-08 Advanced Tech Materials Making high density indium tin oxide sputtering targets
WO2016117688A1 (en) * 2015-01-23 2016-07-28 Toto株式会社 Cast molded body and method for producing same
CN111006514A (en) * 2019-12-20 2020-04-14 广州市尤特新材料有限公司 Sintering method of burning bearing plate and planar ceramic target material

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2004090051A1 (en) * 2003-04-09 2006-07-06 株式会社ホソカワ粉体技術研究所 Powder coating production method and powder coating obtained by the production method
JP4489019B2 (en) * 2003-04-09 2010-06-23 ホソカワミクロン株式会社 Method for producing powder coating
JP2008255480A (en) * 2007-03-09 2008-10-23 Mitsubishi Materials Corp Vapor deposition material and manufacturing method therefor
GB2482544A (en) * 2010-08-06 2012-02-08 Advanced Tech Materials Making high density indium tin oxide sputtering targets
WO2016117688A1 (en) * 2015-01-23 2016-07-28 Toto株式会社 Cast molded body and method for producing same
CN111006514A (en) * 2019-12-20 2020-04-14 广州市尤特新材料有限公司 Sintering method of burning bearing plate and planar ceramic target material

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