JPH05222410A - Production of high-purity ito sintered body - Google Patents
Production of high-purity ito sintered bodyInfo
- Publication number
- JPH05222410A JPH05222410A JP4061190A JP6119092A JPH05222410A JP H05222410 A JPH05222410 A JP H05222410A JP 4061190 A JP4061190 A JP 4061190A JP 6119092 A JP6119092 A JP 6119092A JP H05222410 A JPH05222410 A JP H05222410A
- Authority
- JP
- Japan
- Prior art keywords
- sintered body
- density
- relative density
- oxide powder
- temperature
- 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.)
- Granted
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ＩＴＯ焼結体の製造方
法に関し、さらに詳しくは、焼結性の良い粉末成形体を
つくり、これを焼成することによって、常圧下で高密度
なＩＴＯ焼結体を製造する製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an ITO sintered body, and more specifically, a powder compact having good sinterability is prepared and fired to obtain a high density ITO sintered body under normal pressure. The present invention relates to a manufacturing method for manufacturing a bound body.
【０００２】[0002]
【従来の技術】従来、ＩＴＯ焼結体は、透明導電膜を形
成するスパッタリングターゲット材や真空蒸着用のペレ
ットとして利用されている。この焼結体は、ＩＴＯが難
焼結性で高温域では解離を生ずる性質を有しているた
め、常圧焼結では相対密度６０〜７５％のものしか得ら
れないという問題があった。2. Description of the Related Art Conventionally, an ITO sintered body has been used as a sputtering target material for forming a transparent conductive film or a pellet for vacuum deposition. This sintered body has a problem that since ITO is difficult to sinter and has a property of causing dissociation in a high temperature range, only a relative density of 60 to 75% can be obtained by pressureless sintering.
【０００３】一方、焼結体の相対密度を上げると焼結体
の利用効率を高め得ることも知られており、特にスパッ
タ法では低抵抗膜が得られ、ターゲットの黒化までの時
間が延びることから高密度化の検討がなされている。こ
れらは特開平１−２９０５５１号公報に開示されている
ように成形体を仮焼後高圧でＣＩＰ処理をして成形体密
度を上げて焼成する方法や、特開平３−２０７８５８号
公報に開示されているように、焼成時に酸化雰囲気で加
圧して解離を抑える方法が知られているが、酸化雰囲気
で加圧しながら焼成する方法は、装置上の配慮が必要で
ある他、酸素を供給しなければならない等コスト上の問
題があった。On the other hand, it is also known that increasing the relative density of the sintered body can improve the utilization efficiency of the sintered body. In particular, a low resistance film can be obtained by the sputtering method, and the time until the blackening of the target is prolonged. Therefore, a study for increasing the density has been made. These are disclosed in Japanese Unexamined Patent Publication (Kokai) No. 3-207858 and a method in which a molded product is calcined and then subjected to CIP treatment at a high pressure to increase the density of the molded product, as disclosed in Japanese Unexamined Patent Publication No. 1-290551. As described above, there is known a method of suppressing dissociation by applying pressure in an oxidizing atmosphere at the time of baking, but the method of baking while applying pressure in an oxidizing atmosphere requires consideration of the apparatus and oxygen must be supplied. There was a cost problem such as having to do it.
【０００４】また、一般に高密度焼結体はホットプレス
法により製造されているが、この方法は、還元雰囲気下
で焼成を行うため得られた焼結体の一部が還元されると
いう欠点を有する他、大型の焼結品を製造するには装置
自体も大型化しなければならず実用的でない上、高価な
装置を用いなければならないという問題もあった。Generally, a high-density sintered body is manufactured by a hot pressing method, but this method has a drawback that a part of the obtained sintered body is reduced because firing is performed in a reducing atmosphere. Besides, in order to manufacture a large-sized sintered product, the apparatus itself must be upsized, which is not practical, and there is a problem that an expensive apparatus must be used.
【０００５】本発明者等は、先に特願平３−８３３０９
号「高密度ＩＴＯ焼結体の製造方法」において、焼結性
のよい微粉原料を用いた高密度の造粒粉を用いることに
より相対密度７５％以上の焼結体が得られる方法を提案
している。The present inventors have previously filed Japanese Patent Application No. 3-83309.
In "Production Method of High Density ITO Sintered Body", a method of obtaining a sintered body having a relative density of 75% or more by using a high-density granulated powder using a fine powder raw material having good sinterability is proposed. ing.
【０００６】[0006]
【発明が解決しようとする課題】上述のように従来法に
おいては、ホットプレスなど高価な装置を必要とした
り、成形後に成形体密度を高める為に、更に諸工程を要
したり、焼結工程の高圧化を図るためにコスト高となる
等の問題もあって新規な手段により、これらの問題を解
決することが望まれていた。As described above, in the conventional method, an expensive device such as a hot press is required, further steps are required to increase the density of the molded body after molding, and the sintering step is required. There is also a problem that the cost is increased in order to increase the pressure, and it has been desired to solve these problems by new means.
【０００７】[0007]
【課題を解決するための手段】本発明者等は斯かる課題
を解決するために鋭意研究したところ、焼結体密度８５
％以上のＩＴＯ焼結体を常圧焼結で得るには、焼結性に
優れたＩＴＯ粉末を用いて特定条件で焼結を行うことに
よって目的を達し得ることを見出し、本発明法を提出す
ることができたものである。Means for Solving the Problems The inventors of the present invention have made extensive studies to solve such problems and found that a sintered body density of 85
In order to obtain at least 10% of ITO sintered body by pressureless sintering, it was found that the object can be achieved by performing sintering under specific conditions using ITO powder having excellent sinterability, and submitted the method of the present invention. I was able to do it.
【０００８】すなわち本発明は、酸化インジウム粉と酸
化スズ粉との混合物を成形して焼成することによってＩ
ＴＯ焼結体を製造する方法において、成形体の相対密度
が４５％以上であるものを常圧下、昇温速度１００℃／
ｈｒ以上で昇温した後、１４００〜１７００℃の温度に
保持することによって相対密度が８５％以上である焼結
体と成すことを特徴とする高密度ＩＴＯ焼結体の製造方
法を提供するものである。That is, according to the present invention, a mixture of indium oxide powder and tin oxide powder is formed and fired.
In the method for producing a TO sintered body, a molded body having a relative density of 45% or more is heated under normal pressure at a heating rate of 100 ° C. /
A method for producing a high-density ITO sintered body, characterized by forming a sintered body having a relative density of 85% or more by holding the temperature at 1400 to 1700 ° C. after heating at a temperature of not less than hr. Is.
【０００９】[0009]
【作用】本発明法においては、焼結性に優れたＩＴＯ微
粉末を用いるが、主成分の酸化インジウム粉末としては
比表面積２０ｍ2 ／ｇ以上のものを８５〜１００ｗｔ％
の割合で使用し、残りの１５〜０ｗｔ％を酸化スズ粉末
が占めるように配合して、両者を均一に混合したものを
用い、次いで該混合粉を金型プレスあるいはＣＩＰ等を
用いて成形体密度が相対密度で４５％以上となるように
圧粉成形する。In the method of the present invention, ITO fine powder having excellent sinterability is used, and the main component of indium oxide powder is 85 to 100 wt% of a specific surface area of 20 m 2 / g or more.
Used in such a ratio that the tin oxide powder occupies the remaining 15 to 0 wt% and uniformly mixed both, and then the mixed powder is molded using a die press or CIP. The powder is compacted so that the relative density is 45% or more.
【００１０】混合粉の成形に際しては成形し易いように
有機バインダー等を添加したり、造粒等の操作を施して
も構わないが、成形体の密度については、所望の焼結体
密度を得るために４５％以上の相対密度となるようにす
ることが必要であり、これ以下の相対密度を持つ成形体
を使用したのでは焼結体密度８５％以上が得られないこ
とを確認した。At the time of molding the mixed powder, an organic binder or the like may be added or operations such as granulation may be performed so as to facilitate the molding, but with respect to the density of the molded body, a desired sintered body density is obtained. Therefore, it is necessary to set the relative density to 45% or more, and it was confirmed that a sintered body density of 85% or more cannot be obtained by using a molded body having a relative density of less than this.
【００１１】次いで得られた成形体を大気中で焼成して
焼結体を製造するが、焼成パターンとして昇温は１００
℃／ｈｒ以上で行い、１４００〜１７００℃の温度に所
定時間保持することを特徴とするものである。この場合
の高温保持時間は焼結体の相対密度が８５％以上となる
ことが保証される限り特に制限はないが、通常１〜２０
ｈｒ好ましくは２〜１０ｈｒである。尚、大型の成形体
を焼成する場合には、低温域での強度が弱いために急速
昇温では割れやクラックが発生することもあるため、低
温域では昇温速度を抑えても構わない。Next, the obtained molded body is fired in the atmosphere to produce a sintered body, and the firing pattern has a temperature rise of 100.
C./hr or more, and the temperature is maintained at 1400 to 1700.degree. C. for a predetermined time. The high temperature holding time in this case is not particularly limited as long as the relative density of the sintered body is guaranteed to be 85% or more, but is usually 1 to 20.
hr is preferably 2 to 10 hr. When a large-sized compact is fired, cracks or cracks may occur during rapid temperature increase due to weak strength in the low temperature range, so the temperature increase rate may be suppressed in the low temperature range.
【００１２】先ず、昇温によって強度が割れ等に耐える
ようにした後、１０００℃以上の温度域では、１００℃
／ｈｒ以上の昇温速度、望ましくは１２０℃／ｈｒ以上
の昇温速度で１４００℃以上の温度に迄昇温し、所定の
温度に保持した後冷却して焼結体を得るが、成形時に有
機バインダー等を添加した場合は、脱バインダー等の処
理を１０００℃以下で行うことは構わない。First, after the strength is set to withstand cracking and the like by raising the temperature, 100 ° C. in the temperature range of 1000 ° C. or higher.
The temperature is raised to 1400 ° C. or higher at a temperature rising rate of / hr or more, preferably 120 ° C./hr or more, and the temperature is maintained at a predetermined temperature and then cooled to obtain a sintered body. When an organic binder or the like is added, treatment such as debinding may be performed at 1000 ° C or lower.
【００１３】上述のような製造方法で、所望の高密度Ｉ
ＴＯ焼結体が得られる理由としては、以下のような反応
機構が考えられる。すなわちＩＴＯの焼結においては、
Ｉｎ2 Ｏ3 とＳｎＯ2 は共に焼成温度域での蒸気圧が高
く、気相拡散により焼結が進行していると考えられる
が、反面、ＩＴＯの解離や異常粒成長により焼結が阻害
される。１０００℃以上では、ＩＴＯの気相での拡散が
大きく、この温度域で温度分布にむらが生じると異常粒
成長が起き、焼結体密度は上がらない。従って１０００
℃以上の温度域では焼結温度まで比較的速い速度で昇温
することにより異常粒の成長を抑えることができる。With the manufacturing method as described above, the desired high density I
The following reaction mechanism can be considered as a reason for obtaining the TO sintered body. That is, in the sintering of ITO,
Both In 2 O 3 and SnO 2 have a high vapor pressure in the firing temperature range, and it is considered that sintering progresses due to vapor phase diffusion, but on the other hand, the dissociation of ITO and abnormal grain growth hinder the sintering. It At 1000 ° C. or higher, the diffusion of ITO in the gas phase is large, and if uneven temperature distribution occurs in this temperature range, abnormal grain growth occurs and the sintered body density does not rise. Therefore 1000
In the temperature range of ℃ or higher, abnormal grain growth can be suppressed by raising the temperature to the sintering temperature at a relatively fast rate.
【００１４】またＩＴＯの解離により焼結が阻害される
が、これは成形体密度が低く、焼結によって成形体のも
つ空げきが充分に塞がれない場合、気相となったＩＴＯ
は焼成物の系外に蒸気として抜けた空孔が残ることによ
る。従って成形体密度を相対密度で４５％以上としたも
のを用いて、焼成時に表面が焼結し、ＩＴＯの蒸発が少
なくなるようにすることで焼結体密度が上がるように対
処している。Further, the dissociation of ITO hinders the sintering, but this is because the density of the molded body is low, and when the voids of the molded body cannot be sufficiently closed by the sintering, the ITO in the vapor phase is formed.
Is due to the holes left as vapor outside the system of the fired product. Therefore, by using a compact having a relative density of 45% or more, the surface is sintered during firing so that the evaporation of ITO is reduced, so that the sintered density is increased.
【００１５】以下、実施例により詳細に説明する。A detailed description will be given below with reference to embodiments.
【００１６】[0016]
【実施例１】比表面積３０ｍ2 ／ｇの酸化インジウム粉
９０ｗｔ％と、比表面積４ｍ2 ／ｇの酸化スズ粉１０ｗ
ｔ％との混合粉にＰＶＡ５ｗｔ％水溶液を混合粉の全量
基準で１０ｗｔ％を添加した粉体を金型プレスを用いて
φ１”×５ｍｍのペレットを作成した。得られたペレッ
トを乾燥後、昇温速度１２０℃／ｈｒで昇温させて、大
気圧下、１５００℃の温度で２時間焼成を行い、所望の
焼結体を得た。得られた焼結体の焼結体密度および焼成
重量減を表１に示した。Example 1 90 wt% of indium oxide powder having a specific surface area of 30 m 2 / g and 10 w of tin oxide powder having a specific surface area of 4 m 2 / g
A powder obtained by adding 10 wt% of PVA 5 wt% aqueous solution to the mixed powder with t% based on the total amount of the mixed powder was made into a pellet of φ1 ″ × 5 mm by using a mold press. The temperature was raised at a temperature rate of 120 ° C./hr, and firing was performed under atmospheric pressure at a temperature of 1500 ° C. for 2 hours to obtain a desired sintered body.Sintered body density and firing weight of the obtained sintered body The decrease is shown in Table 1.
【００１７】尚、焼成重量減は成形体（乾燥後）と焼結
体との重量より算出した。The reduction in firing weight was calculated from the weights of the molded body (after drying) and the sintered body.
【００１８】[0018]
【実施例２】比表面積３０ｍ2 ／ｇの酸化インジウム粉
９５ｗｔ％と、比表面積４ｍ2 ／ｇの酸化スズ粉５ｗｔ
％との混合粉にＰＶＡ５ｗｔ％水溶液を混合粉の全量基
準で１０ｗｔ％添加した粉末を金型プレスにより４８０
×１７０×１０ｍｍの成形体に成形したところ、この成
形体の相対密度は５３％であった。次いでこの成形体を
電気炉中で、脱脂パターンを含む昇温パターンで１００
０℃まで昇温せしめた後、更に１８０℃／ｈｒの昇温速
度で１５５０℃まで昇温して５時間保持して焼成を行っ
た。得られた焼結体の相対密度９３％で、焼成重量減は
２．９％であった。Example 2 95 wt% of indium oxide powder having a specific surface area of 30 m 2 / g and 5 wt% tin oxide powder having a specific surface area of 4 m 2 / g
% Powder of PVA added to 10% by weight based on the total amount of the mixed powder to 480% by a die press.
When molded into a molded body of × 170 × 10 mm, the relative density of this molded body was 53%. Next, this molded body is heated in an electric furnace at 100 ° C. in a heating pattern including a degreasing pattern.
After the temperature was raised to 0 ° C., the temperature was further raised to 1550 ° C. at a heating rate of 180 ° C./hr, and the temperature was maintained for 5 hours for firing. The relative density of the obtained sintered body was 93%, and the weight reduction by firing was 2.9%.
【００１９】[0019]
【実施例３】実施例２に示す造粒粉を用いて作製した成
形体を用い、成形圧力を制御して成形体の相対密度を４
８％とした。この成形体を実施例２と同様な工程で焼成
体としたものは、焼結体の相対密度８６％で、焼成重量
減は３．５％であった。[Embodiment 3] A molded body produced by using the granulated powder shown in Example 2 was used, and the relative density of the molded body was controlled to 4 by controlling the molding pressure.
8%. When this molded body was made into a fired body in the same process as in Example 2, the relative density of the sintered body was 86%, and the weight loss on firing was 3.5%.
【００２０】[0020]
【比較例１】実施例１に示す造粒粉を用いて作製したペ
レット体を用い、電気炉中での昇温速度を６０℃／ｈｒ
とした以外は、実施例１に示す工程と同様の条件で焼成
した。得られた焼結体の相対密度は８２％で、焼成重量
減は４．７％であった。[Comparative Example 1] A pellet body produced by using the granulated powder shown in Example 1 was used, and the temperature rising rate in an electric furnace was 60 ° C / hr.
Other than the above, firing was performed under the same conditions as in the process shown in Example 1. The relative density of the obtained sintered body was 82%, and the weight reduction by firing was 4.7%.
【００２１】[0021]
【比較例２】実施例２に示す造粒粉を用いて、作製した
成形体を、成形圧力を制御して成形体の相対密度を４３
％とし、次いでこの成形体を電気炉中で焼成した。この
場合、昇温は１０００℃迄脱脂パターンを含む昇温速度
で比較的ゆるやかに昇温した後、１０００℃以上からは
昇温速度１００℃／ｈｒで１５５０℃まで昇温して５時
間保持した後冷却した。得られた焼結体の相対密度は７
５％であり、焼成重量減は４．２％であった。[Comparative Example 2] A molded product produced by using the granulated powder shown in Example 2 has a relative density of 43 which is controlled by controlling the molding pressure.
%, And then the molded body was fired in an electric furnace. In this case, the temperature was raised up to 1000 ° C. at a relatively slow rate including the degreasing pattern, and from 1000 ° C. or higher, the temperature was raised to 1550 ° C. at a rate of 100 ° C./hr and held for 5 hours. After cooling. The relative density of the obtained sintered body is 7
It was 5%, and the weight loss on burning was 4.2%.
【００２２】表１の結果から成形体の相対密度が４５％
以下のものを用いる場合と、昇温速度が１００℃／ｈｒ
以下の場合には、焼結体の相対密度が８５％以下となり
高密度化が図れないことが確認できた。From the results shown in Table 1, the relative density of the molded body was 45%.
When using the following, the temperature rising rate is 100 ° C / hr
In the following cases, it was confirmed that the relative density of the sintered body was 85% or less and the density could not be increased.
【００２３】[0023]
【表１】 [Table 1]
【００２４】[0024]
【発明の効果】上述のように従来、高密度なＩＴＯ焼結
体を得るには高価な装置や割高な焼成条件が必要である
と考えられていたが、本発明法によれば、成形体の相対
密度が４５％以上となるように予め制御することによっ
て一般的な常圧焼結を行うことにより高密度ＩＴＯが得
られるので、通常の大気炉を用いて、安価な焼結体を製
造できるという効果がある。As described above, conventionally, it was considered that an expensive apparatus and expensive firing conditions were required to obtain a high density ITO sintered body, but according to the method of the present invention, a molded body is obtained. Since high density ITO can be obtained by performing general atmospheric pressure sintering by controlling in advance so that the relative density of the above is 45% or more, an inexpensive sintered body can be manufactured using a normal atmospheric furnace. There is an effect that you can.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 戸田 尚 東京都千代田区丸の内１丁目８番２号 同 和鉱業株式会社内 (72)発明者 阿部 正春 東京都千代田区丸の内１丁目８番２号 同 和鉱業株式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Nao Toda 1-8-2 Marunouchi, Chiyoda-ku, Tokyo Dowa Mining Co., Ltd. (72) Masaharu Abe 1-2-8 Marunouchi, Chiyoda-ku, Tokyo Within Wa Mining Co., Ltd.
Claims (1)
物を成形して焼成することによってＩＴＯ焼結体を製造
する方法において、圧粉成形により相対密度が４５％以
上の成形体を製造した後、該成形体を常圧下、昇温速度
１００℃／ｈｒ以上で高温保持温度まで昇温し、次いで
１４００〜１７００℃の高温に所定時間保持することに
よって相対密度が８５％以上である焼結体と成すことを
特徴とする高密度ＩＴＯ焼結体の製造方法。1. A method for producing an ITO sintered body by shaping a mixture of indium oxide powder and tin oxide powder and firing the mixture, after producing a compact having a relative density of 45% or more by compacting. A sintered body having a relative density of 85% or more by raising the temperature of the formed body to a high temperature holding temperature at a temperature rising rate of 100 ° C./hr or more under normal pressure, and then holding at a high temperature of 1400 to 1700 ° C. for a predetermined time. A method for manufacturing a high-density ITO sintered body, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4061190A JP2794679B2 (en) | 1992-02-17 | 1992-02-17 | Method for producing high-density ITO sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4061190A JP2794679B2 (en) | 1992-02-17 | 1992-02-17 | Method for producing high-density ITO sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05222410A true JPH05222410A (en) | 1993-08-31 |
| JP2794679B2 JP2794679B2 (en) | 1998-09-10 |
Family
ID=13164003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4061190A Expired - Lifetime JP2794679B2 (en) | 1992-02-17 | 1992-02-17 | Method for producing high-density ITO sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2794679B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06299344A (en) * | 1993-04-13 | 1994-10-25 | Mitsui Mining & Smelting Co Ltd | Production of ito target for sputtering |
| US6051166A (en) * | 1995-12-06 | 2000-04-18 | Sumitomo Chemical Corporation, Limited | Indium oxide-tin oxide powders and method for producing the same |
| WO2010018707A1 (en) * | 2008-08-11 | 2010-02-18 | 出光興産株式会社 | Gallium oxide-tin oxide based oxide sintered body and oxide film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02297812A (en) * | 1989-02-28 | 1990-12-10 | Tosoh Corp | Sintered body of oxide, manufacture thereof, and target using same |
| JPH0328156A (en) * | 1989-06-22 | 1991-02-06 | Tosoh Corp | Production of oxide sintered material |
-
1992
- 1992-02-17 JP JP4061190A patent/JP2794679B2/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02297812A (en) * | 1989-02-28 | 1990-12-10 | Tosoh Corp | Sintered body of oxide, manufacture thereof, and target using same |
| JPH0328156A (en) * | 1989-06-22 | 1991-02-06 | Tosoh Corp | Production of oxide sintered material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06299344A (en) * | 1993-04-13 | 1994-10-25 | Mitsui Mining & Smelting Co Ltd | Production of ito target for sputtering |
| US6051166A (en) * | 1995-12-06 | 2000-04-18 | Sumitomo Chemical Corporation, Limited | Indium oxide-tin oxide powders and method for producing the same |
| WO2010018707A1 (en) * | 2008-08-11 | 2010-02-18 | 出光興産株式会社 | Gallium oxide-tin oxide based oxide sintered body and oxide film |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2794679B2 (en) | 1998-09-10 |
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