JPH10330169A - Production of ceramic sintered compact - Google Patents
Production of ceramic sintered compactInfo
- Publication number
- JPH10330169A JPH10330169A JP9139678A JP13967897A JPH10330169A JP H10330169 A JPH10330169 A JP H10330169A JP 9139678 A JP9139678 A JP 9139678A JP 13967897 A JP13967897 A JP 13967897A JP H10330169 A JPH10330169 A JP H10330169A
- Authority
- JP
- Japan
- Prior art keywords
- ceramic sintered
- producing
- sintered body
- degreasing
- oxygen
- 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
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、スパッタリングタ
ーゲットに好適なセラミックス焼結体の製造方法に関す
るものである。The present invention relates to a method for producing a ceramic sintered body suitable for a sputtering target.
【０００２】[0002]
【従来の技術】種々の分野で薄膜を形成するために、セ
ラミックス焼結体からなるスパッタリングターゲットが
利用されている。例えば、ＩＴＯ（Ｉｎｄｉｕｍ Ｔｉ
ｎ Ｏｘｉｄｅ）薄膜は、高導電性、高透過率といった
特徴を有し、更に微細加工も行えることから、フラット
パネル用表示電極、太陽電池窓材、帯電防止膜等の広範
囲な分野に渡って用いられている。特に液晶表示装置を
始めとしたフラットパネルディスプレイ分野では大型化
及び高精細化が進んでおり、その表示用電極であるＩＴ
Ｏ薄膜に対する需要も急速に高まっている。2. Description of the Related Art Sputtering targets made of ceramic sintered bodies have been used to form thin films in various fields. For example, ITO (Indium Ti
n Oxide) thin films have characteristics such as high conductivity and high transmittance, and can be finely processed. Therefore, they are used in a wide range of fields such as display electrodes for flat panels, solar cell window materials, and antistatic films. Have been. In particular, in the field of flat panel displays such as liquid crystal display devices, the size and definition are increasing, and the display electrodes IT
The demand for O thin films is also growing rapidly.
【０００３】しかしながらＩＴＯを始めとするセラミッ
クス焼結体の製品価格は比較的高価であり、その応用範
囲が拡大するにつれて、市場からは低価格化の要求が高
まっている。低価格化を達成するための一つの方法とし
て、セラミックス焼結体の製造歩留まりを向上すること
が考えられる。[0003] However, the price of ceramics sintered products such as ITO is relatively expensive, and as the range of application thereof expands, demands for lower prices are increasing from the market. As one method for achieving a reduction in cost, it is conceivable to improve the production yield of ceramic sintered bodies.
【０００４】一般にセラミックス焼結体は、原料粉末を
成形した後、焼結することにより製造されるが、粉末を
成形する際に成形性を向上させるため、ポリビニルアル
コールまたはパラフィン等のバインダーが使用される。
この場合、焼結前に成形体からバインダーを取り除くた
めの脱脂処理を行う必要がある。この脱脂処理における
成形体の割れは、歩留まり低下の要因の一つであり、成
形体サイズが大きくなるのにともない顕著となる。[0004] In general, a ceramic sintered body is manufactured by molding a raw material powder and then sintering. In order to improve the moldability when molding the powder, a binder such as polyvinyl alcohol or paraffin is used. You.
In this case, it is necessary to perform a degreasing treatment for removing the binder from the compact before sintering. Cracking of the molded article in this degreasing treatment is one of the factors that reduce the yield, and becomes more significant as the molded article size increases.
【０００５】[0005]
【発明が解決しようとする課題】本発明の課題は、製造
歩留まりの高いセラミックス焼結体の製造方法を提供す
ることにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a ceramic sintered body having a high production yield.
【０００６】[0006]
【課題を解決するための手段】本発明者等は、成形体の
脱脂時に発生する割れの発生原因について解析を行い、
１）成形体に加えられる温度が不均一になると、成形体
の局部的な収縮が起こり割れが生じる、２）バインダー
が急激に蒸発または燃焼した場合は、その衝撃により成
形体に割れが生じる、３）脱脂終了後、炉内温度を低下
させるときの降温速度が早いと熱衝撃により成形体に割
れが生じる、等の知見を得た。Means for Solving the Problems The present inventors have analyzed the causes of cracks that occur during degreasing of molded articles,
1) When the temperature applied to the molded article becomes non-uniform, local shrinkage of the molded article occurs to cause cracks. 2) When the binder is rapidly evaporated or burned, the impact causes cracks in the molded article. 3) It has been found that after the degreasing is completed, if the temperature drop rate when the furnace temperature is lowered is high, cracks may occur in the molded body due to thermal shock.
【０００７】そこで、以上の知見を元に成形体の脱脂工
程における昇温速度、脱脂温度、保持時間、降温速度に
着目して更に実験を行った結果、ある条件を満たす昇温
速度、降温速度に設定して脱脂を行うと脱脂時に発生す
る成形体の割れの発生率が著しく減少し、セラミックス
焼結体の製造歩留まりが向上することを見いだし、本発
明を完成した。Therefore, based on the above findings, further experiments were conducted focusing on the heating rate, the degreasing temperature, the holding time, and the cooling rate in the degreasing step of the molded body. As a result, the heating rate and the cooling rate satisfying certain conditions were obtained. When degreasing is performed by setting to, the occurrence rate of cracks in the molded body during degreasing is significantly reduced, and it has been found that the production yield of ceramic sintered bodies is improved, and the present invention has been completed.
【０００８】即ち本発明は、原料粉末にバインダーを添
加した後、成形、脱脂、焼結を行うセラミックス焼結体
の製造方法において、脱脂工程における昇降温速度を２
［℃／時間］以下にすることを特徴とするセラミックス
焼結体の製造方法に関するものである。That is, according to the present invention, in a method for producing a ceramic sintered body in which a binder is added to a raw material powder, followed by molding, degreasing, and sintering, the rate of temperature rise and fall in the degreasing step is 2
The present invention relates to a method for producing a ceramic sintered body, wherein the temperature is not more than [° C./hour].
【０００９】以下、本発明を詳細に説明する。Hereinafter, the present invention will be described in detail.
【００１０】本発明のセラミックス焼結体とは、特に限
定することはできないが、例えば、実質的に亜鉛、アル
ミニウムおよび酸素からなる焼結体（ＺＡＯ）、実質的
にストロンチウム、チタンおよび酸素からなる焼結体
（ＳＴＯ）、実質的にストロンチウム、バリウム、チタ
ンおよび酸素からなる焼結体（ＢＳＴ）、実質的にスト
ロンチウム、ビスマス、タンタルおよび酸素からなる焼
結体（ＳＢＴ）、実質的にインジウム、スズおよび酸素
からなる焼結体（ＩＴＯ）等をあげることができる。Although the ceramic sintered body of the present invention is not particularly limited, for example, a sintered body (ZAO) substantially consisting of zinc, aluminum and oxygen, and substantially consisting of strontium, titanium and oxygen A sintered body (STO), a sintered body substantially composed of strontium, barium, titanium and oxygen (BST), a sintered body substantially composed of strontium, bismuth, tantalum and oxygen (SBT), substantially indium; A sintered body (ITO) composed of tin and oxygen can be used.
【００１１】本発明によるセラミックス焼結体は、特定
のゆっくりした（２［℃／時間］以下）昇温速度および
降温速度を有する脱脂工程を経ることにより得られる。The ceramic sintered body according to the present invention can be obtained through a degreasing step having a specific slow (less than 2 [° C./hour]) heating rate and a cooling rate.
【００１２】本発明における成形体は、例えば、所望す
るセラミックス焼結体の原料粉末の混合粉末、または仮
焼粉末、または固溶体粉末等にバインダーを添加した粉
末を成形することにより得ることができる。The compact in the present invention can be obtained, for example, by molding a powder obtained by adding a binder to a mixed powder of raw material powder of a desired ceramic sintered body, a calcined powder, a solid solution powder or the like.
【００１３】例えばＺＡＯを得るための成形体は、酸化
亜鉛および酸化アルミニウムの混合粉末より、ＳＴＯを
得るための成形体は、炭酸ストロンチウムおよび酸化チ
タンの混合粉末の仮焼により得られた粉末より、ＢＳＴ
を得るための成形体は、炭酸ストロンチウム、炭酸バリ
ウムおよび酸化チタンの混合粉末の仮焼により得られた
粉末より、ＳＢＴを得るための成形体は、酸化ビスマ
ス、酸化チタンおよび炭酸ストロンチウムの混合粉末の
仮焼により得られた粉末より、ＩＴＯを得るための成形
体は酸化インジウムおよび酸化スズの混合粉末または酸
化インジウム酸化スズ固溶体粉末に、ポリビニルアルコ
ールまたはパラフィン等のバインダーを添加した粉末よ
り成形することができる。ＩＴＯの場合、酸化スズの量
はスパッタリングにより得られるＩＴＯ薄膜の比抵抗値
が低下するように５〜１５［ｗｔ．％］とすることが望
ましい。For example, a compact for obtaining ZAO is formed from a mixed powder of zinc oxide and aluminum oxide, and a compact for obtaining STO is formed from a powder obtained by calcining a mixed powder of strontium carbonate and titanium oxide. BST
The molded body for obtaining SBT was formed from a powder obtained by calcining a mixed powder of strontium carbonate, barium carbonate and titanium oxide, and the molded body for obtaining SBT was formed of a mixed powder of bismuth oxide, titanium oxide and strontium carbonate. From the powder obtained by calcination, a molded body for obtaining ITO can be formed from a powder obtained by adding a binder such as polyvinyl alcohol or paraffin to a mixed powder of indium oxide and tin oxide or a solid solution powder of indium oxide and tin oxide. it can. In the case of ITO, the amount of tin oxide is 5 to 15 wt.% So that the specific resistance of the ITO thin film obtained by sputtering decreases. %].
【００１４】これら混合粉末、仮焼粉末または固溶粉末
に対して、必要に応じて粉砕あるいは圧密処理を施した
後、ポリビニルアルコールまたはパラフィン等のバイン
ダーを添加し、プレス法あるいは鋳込み法等の成型方法
により成型して成形体を作製する。These mixed powders, calcined powders or solid solution powders are subjected to pulverization or consolidation treatment as required, and then a binder such as polyvinyl alcohol or paraffin is added thereto, and the mixture is molded by a pressing method or a casting method. A molded article is produced by molding according to the method.
【００１５】プレス成形により成形体を製造する場合に
は、粉末に０．５〜５．０［ｗｔ．％］のバインダーを
添加した後、該バインダー添加粉末を所定の大きさの金
型に充填し、プレス機を用いて１００〜１０００ｋｇ／
ｃｍ2の圧力でプレスを行い成形体とする。In the case of producing a compact by press molding, 0.5 to 5.0 [wt. %], The binder-added powder is filled in a mold of a predetermined size, and 100 to 1000 kg /
Pressing is performed at a pressure of cm 2 to obtain a molded body.
【００１６】一方、鋳込み成形により成形体を製造する
場合には粉末を水、バインダーおよび分散材と共に混合
してスラリー化し、こうして得られた５０〜５０００セ
ンチポイズの粘度を持つスラリーを鋳込み成形用の型の
中へ注入して成形体を作製する。On the other hand, when a molded article is produced by casting, the powder is mixed with water, a binder and a dispersant to form a slurry, and the slurry having a viscosity of 50 to 5000 centipoise is cast into a mold for casting. To form a molded body.
【００１７】次に、得られた成形体の各エッジ部に対し
て、焼結時のエッジ部からの割れの発生を防止するた
め、０．２ｍｍ以上のＲ加工を施すことが好ましい。Next, in order to prevent the occurrence of cracks from the edges during sintering, it is preferable to subject each edge of the obtained molded body to a rounding process of 0.2 mm or more.
【００１８】次に、得られた成形体は必要に応じて冷間
等方圧プレス（ＣＩＰ）による圧密化処理を行う。この
際ＣＩＰの圧力は十分な圧密効果を得るため１ｔｏｎ／
ｃｍ2以上であることが望ましい。Next, the obtained molded body is subjected to a consolidation treatment by a cold isostatic press (CIP) as required. At this time, the pressure of the CIP is 1 ton / ton to obtain a sufficient consolidation effect.
cm 2 or more.
【００１９】このようにして得られた、成形体に対して
脱脂処理を行うが、脱脂時の昇温速度および降温速度を
２［℃／時間］以下とする。その理由は、２［℃／時
間］以上では、充分な歩留まり向上効果が得られないた
めである。The molded body thus obtained is subjected to a degreasing treatment, and the temperature rising rate and the temperature decreasing rate during the degreasing are set to 2 [° C./hour] or less. The reason is that at a rate of 2 [° C./hour] or more, a sufficient yield improvement effect cannot be obtained.
【００２０】また、脱脂温度は４００〜５００［℃］と
するのが好ましい。その理由は、４００［℃］未満で
は、充分な脱脂効果が得られずバインダーの残留が起こ
り、５００［℃］を越えると脱脂工程では必要のない原
料粉末の反応が生じたり、不必要にエネルギーと時間を
浪費するからである。Further, the degreasing temperature is preferably set to 400 to 500 [° C.]. The reason is that if the temperature is lower than 400 [° C.], a sufficient degreasing effect cannot be obtained and the binder remains, and if the temperature exceeds 500 [° C.], a reaction of the raw material powder which is unnecessary in the degreasing step occurs, or unnecessary energy is consumed. And waste time.
【００２１】このようにして得られた成形体に対して焼
結炉内で焼結を行う。焼結雰囲気は特に限定されるもの
ではない。焼結温度および時間は、使用する粉末によっ
て異なるが、例えばＩＴＯの場合、充分な密度上昇効果
を得るために１４００℃以上、３時間以上とすることが
望ましい。The compact obtained in this way is sintered in a sintering furnace. The sintering atmosphere is not particularly limited. The sintering temperature and time vary depending on the powder used. For example, in the case of ITO, the sintering temperature is preferably 1400 ° C. or more and 3 hours or more in order to obtain a sufficient density increasing effect.
【００２２】以上の方法により作製された焼結体のクラ
ック発生率は低下し、製造歩留まりが向上する。The crack generation rate of the sintered body manufactured by the above method is reduced, and the production yield is improved.
【００２３】このようにして得られた焼結体は、所望の
形状に研削加工してスパッタリングターゲットとする。
得られた加工済みの焼結体は、インジウム半田等を用い
て無酸素銅等からなるバッキングプレートにボンディン
グすることにより容易にターゲット化することができ、
ターゲットの製造歩留まりが向上する。The sintered body thus obtained is ground into a desired shape to form a sputtering target.
The processed sintered body obtained can be easily targeted by bonding to a backing plate made of oxygen-free copper or the like using indium solder or the like,
The production yield of the target is improved.
【００２４】[0024]
【実施例】以下、本発明を実施例をもって更に詳細に説
明するが、本発明はこれらに限定されるものではない。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited thereto.
【００２５】実施例１ ＺｎＯを９８．０［ｗｔ．％］、Ａｌ2Ｏ3を２．０［ｗ
ｔ．％］の割合で混合した混合粉末を原料粉末として用
いた。この原料粉末に２．０［ｗｔ．％］のパラフィン
ワックスをバインダーとして添加した後、１２０［℃］
で加熱処理し、パラフィンワックスを融解させた。この
バインダー入り粉末を７３０×３２０［ｍｍ］の金型に
入れ、３００［ｋｇ／ｃｍ2］の圧力でプレスして成形
体２０枚を作製した。これらの成形体のエッジ部に対し
て、０．３［ｍｍ］のＲ加工を施した後、３［ｔｏｎ／
ｃｍ2］の圧力でＣＩＰ処理を施した。次にこれら２０
枚の成形体を電気炉にいれて大気雰囲気中で脱脂を行っ
た。脱脂条件は、昇温速度１．５［℃／時間］、脱脂温
度４００［℃］、保持時間３［時間］、降温速度１．５
［℃／時間］とした。脱脂工程においては、１枚の割れ
も発生しなかった。Example 1 98.0 [wt. %] And Al 2 O 3 at 2.0 [w
t. %] Was used as the raw material powder. 2.0 [wt. %] Of paraffin wax as a binder, and then added at 120 [° C].
And the paraffin wax was melted. The binder-containing powder was placed in a 730 × 320 [mm] mold and pressed at a pressure of 300 [kg / cm 2 ] to produce 20 molded bodies. After performing an R process of 0.3 [mm] on the edge of these molded bodies, 3 [ton /
cm 2 ]. Next, these 20
The sheets were placed in an electric furnace and degreased in an air atmosphere. The degreasing conditions include a heating rate of 1.5 ° C./hour, a degreasing temperature of 400 ° C., a holding time of 3 hours, and a cooling rate of 1.5.
[° C./hour]. In the degreasing step, one crack did not occur.
【００２６】次にこれら２０枚の成形体を電気炉にいれ
て大気雰囲気中で焼結を行った。焼結条件は、昇温速度
２５［℃／時間］、焼結温度１３００［℃］、保持時間
３［時間］、降温速度２５［℃／時間］とした。焼結工
程においても割れは発生せず、歩留まりは２０／２０＝
１００％であった。Next, these 20 compacts were placed in an electric furnace and sintered in an air atmosphere. The sintering conditions were as follows: a heating rate of 25 [° C./hour], a sintering temperature of 1300 [° C.], a holding time of 3 [hours], and a cooling rate of 25 [° C./hour]. No cracks occurred even in the sintering process, and the yield was 20/20 =
100%.
【００２７】比較例１ 実施例１と同様の粉末を用い、実施例１と同様のプレス
条件でプレスして成形体２０枚を作製し、実施例１と同
様のエッジ部の加工およびＣＩＰ処理を行った。次にこ
れら２０枚の成形体を電気炉に入れ、大気雰囲気下で脱
脂を行った。脱脂条件は、昇温速度１０［℃／時間］、
脱脂温度３００［℃］、保持時間３［時間］、降温速度
１０［℃／時間］とした。脱脂工程において、６枚の割
れが発生した。Comparative Example 1 Using the same powder as in Example 1, pressing was performed under the same pressing conditions as in Example 1 to produce 20 compacts, and the same edge processing and CIP processing as in Example 1 were performed. went. Next, these 20 compacts were placed in an electric furnace and degreased in an air atmosphere. The degreasing conditions include a heating rate of 10 [° C./hour],
The degreasing temperature was 300 [° C.], the retention time was 3 [hours], and the temperature decreasing rate was 10 [° C./hour]. In the degreasing step, six cracks occurred.
【００２８】割れの発生しなかった成形体１４枚を実施
例１と同じ条件で焼結した。焼結工程においては、割れ
は発生しなかったものの、製造歩留まりは１４／２０＝
７０％であった。Fourteen compacts without cracks were sintered under the same conditions as in Example 1. In the sintering process, no cracks occurred, but the production yield was 14/20 =
70%.
【００２９】実施例２ ＳｒＣＯ3を６４．９［ｗｔ．％］、ＴｉＯ2を３５．１
［ｗｔ．％］の割合で混合した混合粉末を１１００
［℃］で３時間仮焼しＳＴＯの原料粉末を得た。この原
料粉末に２．０［ｗｔ．％］のパラフィンワックスをバ
インダーとして添加した後、１２０［℃］で加熱処理
し、パラフィンワックスを融解させた。このバインダー
入り粉末を４５０［ｍｍφ］の金型に入れ、３００［ｋ
ｇ／ｃｍ2］の圧力でプレスして成形体２０枚を作製し
た。これらの成形体のエッジ部に対して、０．３［ｍ
ｍ］のＲ加工を施した後、３［ｔｏｎ／ｃｍ2］の圧力
でＣＩＰ処理を施した。次にこれら２０枚の成形体を電
気炉にいれて大気雰囲気中で脱脂を行った。脱脂条件
は、昇温速度１．５［℃／時間］、脱脂温度４００
［℃］、保持時間３［時間］、降温速度１．５［℃／時
間］とした。脱脂工程においては、１枚の割れも発生し
なかった。Example 2 SrCO 3 was added at 64.9 [wt. %], 35.1% TiO 2
[Wt. %] Is mixed with 1100
Calcination was performed at [° C.] for 3 hours to obtain STO raw material powder. 2.0 [wt. %] Of paraffin wax as a binder, and then heat-treated at 120 ° C. to melt the paraffin wax. This binder-containing powder is put into a 450 [mmφ] mold and 300 [k].
g / cm 2 ] to produce 20 compacts. 0.3 [m
m], and then a CIP treatment at a pressure of 3 [ton / cm 2 ]. Next, these 20 compacts were placed in an electric furnace and degreased in an air atmosphere. Degreasing conditions were as follows: heating rate 1.5 [° C./hour], degreasing temperature 400
[° C.], a retention time of 3 [hours], and a temperature decrease rate of 1.5 [° C./hour]. In the degreasing step, one crack did not occur.
【００３０】次にこれら２０枚の成形体を電気炉にいれ
て大気雰囲気中で焼結を行った。焼結条件は、昇温速度
２５［℃／時間］、焼結温度１４００［℃］、保持時間
３［時間］、降温速度２５［℃／時間］とした。焼結工
程においても割れは発生せず、歩留まりは２０／２０＝
１００％であった。Next, these 20 compacts were placed in an electric furnace and sintered in an air atmosphere. The sintering conditions were a heating rate of 25 [° C./hour], a sintering temperature of 1400 [° C.], a holding time of 3 [hours], and a cooling rate of 25 [° C./hour]. No cracks occurred even in the sintering process, and the yield was 20/20 =
100%.
【００３１】比較例２ 実施例２と同様の粉末を用い、実施例２と同様のプレス
条件でプレスして成形体２０枚を作製し、実施例２と同
様のエッジ部の加工およびＣＩＰ処理を行った。次にこ
れら２０枚の成形体を電気炉に入れて大気雰囲気下で脱
脂を行った。脱脂条件は、昇温速度５［℃／時間］、脱
脂温度４００［℃］、保持時間３［時間］、降温速度５
［℃／時間］とした。脱脂工程において、６枚の割れが
発生した。COMPARATIVE EXAMPLE 2 Using the same powder as in Example 2, pressing was performed under the same pressing conditions as in Example 2 to produce 20 compacts, and the same edge processing and CIP processing as in Example 2 were performed. went. Next, these 20 compacts were placed in an electric furnace and degreased in an air atmosphere. Degreasing conditions include a temperature rising rate of 5 ° C./hour, a degreasing temperature of 400 ° C., a holding time of 3 hours, and a temperature decreasing rate of 5 ° C.
[° C./hour]. In the degreasing step, six cracks occurred.
【００３２】割れの発生しなかった成形体１４枚を実施
例２と同じ条件で焼結した。焼結工程においては、割れ
は発生しなかったものの、製造歩留まりは１４／２０＝
７０％であった。Fourteen compacts without cracks were sintered under the same conditions as in Example 2. In the sintering process, no cracks occurred, but the production yield was 14/20 =
70%.
【００３３】実施例３ ＢａＣＯ3を３９．１［ｗｔ．％］、ＳｒＣＯ3を２９．
２［ｗｔ．％］およびＴｉＯ2を３１．７［ｗｔ．％］
の割合で混合した混合粉末を１１００［℃］で３時間仮
焼しＢＳＴの原料粉末を得た。この原料粉末に２．０
［ｗｔ．％］のパラフィンワックスをバインダーとして
添加した後、１２０［℃］で加熱処理し、パラフィンワ
ックスを融解させた。このバインダー入り粉末を４５０
［ｍｍφ」の金型に入れ、３００［ｋｇ／ｃｍ2］の圧
力でプレスして成形体２０枚を作製した。これらの成形
体のエッジ部に対して、０．３［ｍｍ］のＲ加工を施し
た後、３［ｔｏｎ／ｃｍ2］の圧力でＣＩＰ処理を施し
た。次にこれら２０枚の成形体を電気炉にいれて大気雰
囲気下で脱脂を行った。脱脂条件は、昇温速度１．５
［℃／時間］、脱脂温度４００［℃］、保持時間３［時
間］、降温速度１．５［℃／時間］とした。脱脂工程に
おいては、１枚の割れも発生しなかった。Example 3 BaCO 3 was added in an amount of 39.1 [wt. %] And SrCO 3 at 29.
2 [wt. %] And TiO 2 at 31.7 [wt. %]
Was calcined at 1100 [° C.] for 3 hours to obtain BST raw material powder. 2.0%
[Wt. %] Of paraffin wax as a binder, and then heat-treated at 120 ° C. to melt the paraffin wax. This binder-containing powder is mixed with 450
It was placed in a [mmφ] mold and pressed at a pressure of 300 [kg / cm 2 ] to produce 20 molded bodies. The edge portions of these molded bodies were subjected to an R process of 0.3 [mm], and then subjected to a CIP process at a pressure of 3 [ton / cm 2 ]. Next, these 20 sheets were placed in an electric furnace and degreased in an air atmosphere. The degreasing condition is a heating rate of 1.5
[° C./hour], degreasing temperature 400 [° C.], holding time 3 [hours], and cooling rate 1.5 [° C./hour]. In the degreasing step, one crack did not occur.
【００３４】次にこれら２０枚の成形体を電気炉にいれ
て大気雰囲気中で焼結を行った。焼結条件は、昇温速度
２５［℃／時間］、焼結温度１４００［℃］、保持時間
３［時間］、降温速度２５［℃／時間］とした。焼結工
程においても割れは発生せず、歩留まりは２０／２０＝
１００％であった。Next, these 20 compacts were placed in an electric furnace and sintered in an air atmosphere. The sintering conditions were a heating rate of 25 [° C./hour], a sintering temperature of 1400 [° C.], a holding time of 3 [hours], and a cooling rate of 25 [° C./hour]. No cracks occurred even in the sintering process, and the yield was 20/20 =
100%.
【００３５】比較例３ 実施例３と同様の粉末を用い、実施例３と同様のプレス
条件でプレスして成形体２０枚を作製し、実施例３と同
様のエッジ部の加工およびＣＩＰ処理を行った。次にこ
れら２０枚の成形体を電気炉に入れて大気雰囲気下で脱
脂を行った。脱脂条件は、昇温速度５［℃／時間］、脱
脂温度４００［℃］、保持時間３［時間］、降温速度５
［℃／時間］とした。脱脂工程において、８枚の割れが
発生した。Comparative Example 3 The same powder as in Example 3 was pressed under the same pressing conditions as in Example 3 to produce 20 compacts, and the same edge processing and CIP processing as in Example 3 were performed. went. Next, these 20 compacts were placed in an electric furnace and degreased in an air atmosphere. Degreasing conditions include a temperature rising rate of 5 ° C./hour, a degreasing temperature of 400 ° C., a holding time of 3 hours, and a temperature decreasing rate of 5 ° C.
[° C./hour]. In the degreasing step, eight cracks occurred.
【００３６】割れの発生しなかった成形体１４枚を実施
例３と同じ条件で焼結した。焼結工程においては、割れ
は発生しなかったものの、製造歩留まりは１２／２０＝
６０％であった。Fourteen compacts without cracks were sintered under the same conditions as in Example 3. No cracking occurred in the sintering process, but the manufacturing yield was 12/20 =
60%.
【００３７】実施例４ Ｂｉ2Ｏ3を４４．２［ｗｔ．％］、ＳｒＣＯ3を１４．
０［ｗｔ．％］およびＴａ2Ｏ5を４１．８［ｗｔ．％］
の割合で混合した混合粉末を９００［℃］で３時間仮焼
し量論組成のＳＢＴの原料粉末を得た。この量論組成粉
末に過剰のＢｉを添加するために、Ｂｉ2Ｏ3を１５．６
［ｗｔ．％］添加して混合し、原料粉末を得た。この原
料粉末に１．０［ｗｔ．％］のパラフィンワックスをバ
インダーとして添加した後、１２０［℃］で加熱処理
し、パラフィンワックスを融解させた。このバインダー
入り粉末を４５０［ｍｍφ］の金型に入れ、３００
［ｋｇ／ｃｍ2］の圧力でプレスして成形体２０枚を作
製した。これらの成形体のエッジ部に対して、０．３
［ｍｍ］のＲ加工を施した後、３［ｔｏｎ／ｃｍ2］の
圧力でＣＩＰ処理を施した。次にこれら２０枚の成形体
を電気炉にいれて大気雰囲気下で脱脂を行った。脱脂条
件は、昇温速度１．５［℃／時間］、脱脂温度４００
［℃］、保持時間３［時間］、降温速度１．５［℃／時
間］とした。脱脂工程においては、１枚の割れも発生し
なかった。Example 4 Bi 2 O 3 was added to 44.2 [wt. %] And SrCO 3 .
0 [wt. %] And Ta 2 O 5 of 41.8 [wt. %]
Was calcined at 900 [° C.] for 3 hours to obtain SBT raw material powder having a stoichiometric composition. To add excess Bi to this stoichiometric powder, Bi 2 O 3 is added to 15.6.
[Wt. %] And mixed to obtain a raw material powder. 1.0 [wt. %] Of paraffin wax as a binder, and then heat-treated at 120 ° C. to melt the paraffin wax. This binder-containing powder is put into a 450 [mmφ]
Pressing was performed at a pressure of [kg / cm 2 ] to produce 20 molded bodies. 0.3 to the edge of these compacts
After performing [mm] R processing, CIP processing was performed at a pressure of 3 [ton / cm 2 ]. Next, these 20 sheets were placed in an electric furnace and degreased in an air atmosphere. Degreasing conditions were as follows: heating rate 1.5 [° C./hour], degreasing temperature 400
[° C.], a retention time of 3 [hours], and a temperature decrease rate of 1.5 [° C./hour]. In the degreasing step, one crack did not occur.
【００３８】次にこれら２０枚の成形体を電気炉にいれ
て大気雰囲気中で焼結を行った。焼結条件は、昇温速度
２５［℃／時間］、焼結温度９７０［℃］、保持時間３
［時間］、降温速度２５［℃／時間］とした。焼結工程
においても割れは発生せず、歩留まりは２０／２０＝１
００％であった。Next, these 20 compacts were placed in an electric furnace and sintered in an air atmosphere. The sintering conditions were as follows: heating rate 25 [° C./hour], sintering temperature 970 [° C.], holding time 3
[Time], and the temperature drop rate was 25 [° C./hour]. No cracks occurred even in the sintering process, and the yield was 20/20 = 1.
00%.
【００３９】比較例４ 実施例４と同様の粉末を用い、実施例４と同様のプレス
条件でプレスして成形体２０枚を作製し、実施例４と同
様のエッジ部の加工およびＣＩＰ処理を行った。次にこ
れら２０枚の成形体を電気炉に入れて大気雰囲気下で脱
脂を行った。脱脂条件は、昇温速度５［℃／時間］、脱
脂温度４００［℃］、保持時間３［時間］、降温速度５
［℃／時間］とした。脱脂工程において、１０枚の割れ
が発生した。Comparative Example 4 The same powder as in Example 4 was pressed under the same pressing conditions as in Example 4 to produce 20 compacts, and the same edge processing and CIP processing as in Example 4 were performed. went. Next, these 20 compacts were placed in an electric furnace and degreased in an air atmosphere. Degreasing conditions include a temperature rising rate of 5 ° C./hour, a degreasing temperature of 400 ° C., a holding time of 3 hours, and a temperature decreasing rate of 5 ° C.
[° C./hour]. In the degreasing step, ten cracks occurred.
【００４０】割れの発生しなかった成形体１０枚を実施
例４と同じ条件で焼結した。焼結工程においては、割れ
は発生しなかったものの、製造歩留まりは１０／２０＝
５０％であった。Ten compacts without cracks were sintered under the same conditions as in Example 4. No cracking occurred in the sintering process, but the production yield was 10/20 =
It was 50%.
【００４１】実施例５ ＳｎＯ2換算で１０ｗｔ．％の錫を含有した、酸化イン
ジウムと酸化錫の混合粉末を原料粉末として用いた。こ
の混合粉末に２．０［ｗｔ．％］のポリビニルアルコー
ルを添加、混合した後、７３０×３２０［ｍｍ］の金型
に入れ、３００［ｋｇ／ｃｍ2］の圧力でプレスして成
形体２０枚を作製した。これらの成形体のエッジ部に対
して、０．３［ｍｍ］のＲ加工を施した後、３［ｔｏｎ
／ｃｍ2］の圧力でＣＩＰ処理を施した。次にこれら２
０枚の成形体を酸素雰囲気焼結炉内に設置して脱脂を行
った。脱脂条件は、昇温速度１［℃／時間］、脱脂温度
４５０［℃］、保持時間２［時間］、降温速度２［℃／
時間］とした。脱脂工程においては、１枚の割れも発生
しなかった。[0041] Example 5 SnO 2 10wt at the exchange. % Of tin, and a mixed powder of indium oxide and tin oxide was used as a raw material powder. 2.0 [wt. %] Of polyvinyl alcohol was added and mixed, and then placed in a 730 × 320 [mm] mold and pressed at a pressure of 300 [kg / cm 2 ] to produce 20 molded bodies. After performing an R process of 0.3 [mm] on the edge portion of these molded bodies, 3 [ton]
/ Cm 2 ]. Then these two
Zero sheets were placed in an oxygen atmosphere sintering furnace to perform degreasing. The degreasing conditions were as follows: temperature rising rate 1 [° C./hour], degreasing temperature 450 [° C.], holding time 2 [hours], temperature decreasing rate 2 [° C. /
Time]. In the degreasing step, one crack did not occur.
【００４２】次にこれら２０枚の成形体を電気炉にいれ
て純酸素雰囲気中で焼結を行った。焼結条件は、昇温速
度２５［℃／時間］、焼結温度１５００［℃］、保持時
間３［時間］、降温速度２５［℃／時間］とした。焼結
工程においても割れは発生せず、歩留まりは２０／２０
＝１００％であった。Next, these 20 compacts were placed in an electric furnace and sintered in a pure oxygen atmosphere. The sintering conditions were a heating rate of 25 [° C./hour], a sintering temperature of 1500 [° C.], a holding time of 3 [hours], and a cooling rate of 25 [° C./hour]. No cracks occurred even in the sintering process, and the yield was 20/20.
= 100%.
【００４３】次に、これら成形体を純酸素雰囲気炉内に
設置して焼結した。焼結工程においても割れは発生せ
ず、歩留まりは２０／２０＝１００％であった。Next, these compacts were placed in a pure oxygen atmosphere furnace and sintered. No cracks occurred in the sintering step, and the yield was 20/20 = 100%.
【００４４】比較例５ 実施例５と同様の粉末を用い、実施例５と同様のプレス
条件でプレスして成形体２０枚を作製し、実施例５と同
様のエッジ部の加工およびＣＩＰ処理を行った。次にこ
れら２０枚の成形体を酸素雰囲気焼結炉内に設置して脱
脂を行った。脱脂条件は、昇温速度１０［℃／時間］、
脱脂温度４５０［℃］、保持時間２［時間］、降温速度
１０［℃／時間］とした。脱脂工程において、８枚の割
れが発生した。Comparative Example 5 The same powder as in Example 5 was pressed under the same pressing conditions as in Example 5 to produce 20 compacts, and the same edge processing and CIP processing as in Example 5 were performed. went. Next, these 20 compacts were placed in an oxygen atmosphere sintering furnace to perform degreasing. The degreasing conditions include a heating rate of 10 [° C./hour],
The degreasing temperature was 450 [° C], the holding time was 2 [hours], and the temperature decreasing rate was 10 [° C / hour]. In the degreasing step, eight cracks occurred.
【００４５】割れの発生しなかった成形体１２枚を実施
例５と同じ条件で焼結した。焼結工程においては、割れ
は発生しなかったものの、製造歩留まりは１２／２０＝
６０％であった。Twelve compacts without cracks were sintered under the same conditions as in Example 5. No cracking occurred in the sintering process, but the manufacturing yield was 12/20 =
60%.
【００４６】[0046]
【発明の効果】本発明の方法によりセラミックス焼結体
を製造することにより、脱脂工程における成形体の割れ
が発生せず、製造歩留まりを大幅に向上させることがで
きる。By producing a ceramic sintered body by the method of the present invention, cracking of the molded body in the degreasing step does not occur, and the production yield can be greatly improved.
Claims (13)
形、脱脂、焼結するセラミックス焼結体の製造方法にお
いて、前記脱脂工程における昇降温速度を２［℃／時
間］以下にすることを特徴とするセラミックス焼結体の
製造方法。1. A method for producing a ceramic sintered body in which a binder is added to a raw material powder, and then molded, degreased, and sintered, wherein the rate of temperature rise and fall in the degreasing step is 2 ° C./hour or less. Of manufacturing a ceramic sintered body.
る請求項１に記載のセラミックス焼結体の製造方法。2. The method for producing a ceramic sintered body according to claim 1, wherein the temperature raising / lowering rate is 0.5 to 2 [° C./hour].
求項１または請求項２に記載のセラミックス焼結体の製
造方法。3. The method for producing a ceramic sintered body according to claim 1, wherein the degreasing is performed in the air or in an oxidizing atmosphere.
ラフィンである、請求項１〜３のいずれかの請求項に記
載のセラッミクス焼結体の製造方法。4. The method for producing a ceramics sintered body according to claim 1, wherein the binder is polyvinyl alcohol or paraffin.
請求項４に記載のセラミックス焼結体の製造方法。5. A degreasing temperature of 400 to 500 ° C.
A method for producing a ceramic sintered body according to claim 4.
び酸素からなる、請求項１〜５のいずれかの請求項に記
載のセラミックス焼結体の製造方法。6. The method for producing a ceramic sintered body according to claim 1, wherein the molded body substantially consists of zinc, aluminum and oxygen.
および酸素からなる、請求項１〜５のいずれかの請求項
に記載のセラミックス焼結体の製造方法。7. The method for producing a ceramic sintered body according to claim 1, wherein the molded body is substantially composed of strontium, titanium, and oxygen.
ム、チタンおよび酸素からなる、請求項１〜５のいずれ
かの請求項に記載のセラミックス焼結体の製造方法。8. The method for producing a ceramic sintered body according to claim 1, wherein the molded body substantially comprises strontium, barium, titanium and oxygen.
ス、タンタルおよび酸素からなる、請求項１〜５のいず
れかの請求項に記載のセラミックス焼結体の製造方法。9. The method for producing a ceramic sintered body according to claim 1, wherein the molded body substantially comprises strontium, bismuth, tantalum, and oxygen.
び酸素からなる、請求項１〜５のいずれかの請求項に記
載のセラミックス焼結体の製造方法。10. The method for producing a ceramic sintered body according to claim 1, wherein the molded body is substantially made of indium, tin and oxygen.
スズ粉末の混合粉を成形したものであることを特徴とす
る請求項１０に記載のセラミックス焼結体の製造方法11. The method for producing a ceramic sintered body according to claim 10, wherein the molded body is formed by molding a mixed powder of indium oxide powder and tin oxide powder.
溶粉末を形成したものであることを特徴とする請求項１
０に記載のセラミックス焼結体の製造方法。12. The molded body formed from indium oxide-tin oxide solid solution powder.
0. The method for producing a ceramic sintered body according to 0.
ｔ．％］である、請求項１０〜１２のいずれかの請求項
に記載のセラミックス焼結体の製造方法。13. The tin oxide content in the molded product is 5 to 15 [w
t. %], The method for producing a ceramic sintered body according to any one of claims 10 to 12.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9139678A JPH10330169A (en) | 1997-05-29 | 1997-05-29 | Production of ceramic sintered compact |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9139678A JPH10330169A (en) | 1997-05-29 | 1997-05-29 | Production of ceramic sintered compact |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH10330169A true JPH10330169A (en) | 1998-12-15 |
Family
ID=15250883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9139678A Pending JPH10330169A (en) | 1997-05-29 | 1997-05-29 | Production of ceramic sintered compact |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH10330169A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004359982A (en) * | 2003-06-03 | 2004-12-24 | Nikko Materials Co Ltd | Ito sputtering target and method for manufacturing the same |
| JP2007211265A (en) * | 2006-02-07 | 2007-08-23 | Mitsui Mining & Smelting Co Ltd | Ito sintered body and ito sputtering target |
| KR101099472B1 (en) * | 2006-03-14 | 2011-12-28 | 미쓰이 긴조꾸 고교 가부시키가이샤 | Ito sintered body, sputtering target, and method for manufacturing sputtering target material |
| US20120024699A1 (en) * | 2010-07-28 | 2012-02-02 | Hon Hai Precision Industry Co., Ltd. | Composite target material and method for producing the same |
| US8419400B2 (en) | 2005-02-01 | 2013-04-16 | Tosoh Corporation | Sintered body, sputtering target and molding die, and process for producing sintered body employing the same |
| JP2014234340A (en) * | 2013-06-05 | 2014-12-15 | 信越化学工業株式会社 | Defatting method of ceramic molded body |
-
1997
- 1997-05-29 JP JP9139678A patent/JPH10330169A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004359982A (en) * | 2003-06-03 | 2004-12-24 | Nikko Materials Co Ltd | Ito sputtering target and method for manufacturing the same |
| JP4642327B2 (en) * | 2003-06-03 | 2011-03-02 | Ｊｘ日鉱日石金属株式会社 | ITO sputtering target and manufacturing method thereof |
| US8419400B2 (en) | 2005-02-01 | 2013-04-16 | Tosoh Corporation | Sintered body, sputtering target and molding die, and process for producing sintered body employing the same |
| JP2014129231A (en) * | 2005-02-01 | 2014-07-10 | Tosoh Corp | Sintered compact and sputtering target |
| US9920420B2 (en) | 2005-02-01 | 2018-03-20 | Tosoh Corporation | Sintered body, sputtering target and molding die, and process for producing sintered body employing the same |
| JP2007211265A (en) * | 2006-02-07 | 2007-08-23 | Mitsui Mining & Smelting Co Ltd | Ito sintered body and ito sputtering target |
| KR101157123B1 (en) | 2006-02-07 | 2012-06-22 | 미쓰이 긴조꾸 고교 가부시키가이샤 | Ito sintered body and ito sputtering target |
| KR101099472B1 (en) * | 2006-03-14 | 2011-12-28 | 미쓰이 긴조꾸 고교 가부시키가이샤 | Ito sintered body, sputtering target, and method for manufacturing sputtering target material |
| US20120024699A1 (en) * | 2010-07-28 | 2012-02-02 | Hon Hai Precision Industry Co., Ltd. | Composite target material and method for producing the same |
| US8535601B2 (en) * | 2010-07-28 | 2013-09-17 | Hong Fu Jin Precision Industry (Shenzhen) Co., Ltd. | Composite target material and method for producing the same |
| JP2014234340A (en) * | 2013-06-05 | 2014-12-15 | 信越化学工業株式会社 | Defatting method of ceramic molded body |
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