JP2756586B2 - Manufacturing method of oxide sintered body - Google Patents
Manufacturing method of oxide sintered bodyInfo
- Publication number
- JP2756586B2 JP2756586B2 JP1158164A JP15816489A JP2756586B2 JP 2756586 B2 JP2756586 B2 JP 2756586B2 JP 1158164 A JP1158164 A JP 1158164A JP 15816489 A JP15816489 A JP 15816489A JP 2756586 B2 JP2756586 B2 JP 2756586B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- indium
- particle size
- sintered body
- based oxide
- 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.)
- Expired - Fee Related
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Physical Vapour Deposition (AREA)
- Conductive Materials (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、インジウム系酸化物の焼結体の製造方法に
関するものである。Description: TECHNICAL FIELD The present invention relates to a method for producing a sintered body of an indium-based oxide.
更に詳しくは、スパッタリングターゲット材料等のイ
ンジウム系酸化物の焼結材料を製造する方法に関するも
のであり、光エレクトロニクス分野で有用な材料を提供
する手法に関するものである。More specifically, the present invention relates to a method for producing a sintered material of an indium-based oxide such as a sputtering target material, and to a method for providing a material useful in the field of optoelectronics.
［従来の技術］ インジウム酸化物は化合物半導体の一つであり、透明
性と導電性を有する酸化物の一つである。[Related Art] Indium oxide is one of compound semiconductors and one of oxides having transparency and conductivity.
特に、インジウム酸化物にスズの酸化物を微量添加し
た複合酸化物は、ITO（Indium Tin Oxide）として良く
知られており、このものから得た透明導電膜や光選択透
過膜等は光エレクトロニクス分野で巾広く用いられてい
る。In particular, a composite oxide obtained by adding a trace amount of tin oxide to indium oxide is well known as ITO (Indium Tin Oxide), and a transparent conductive film or a light selective transmission film obtained from the compound oxide is used in the field of optoelectronics. Widely used in
インジウム系酸化物等を光エレクトロニクス材料とし
て用いる場合、一般にガラスや透明フィルム上にインジ
ウム系酸化物を被覆したものが用いられている。インジ
ウム系酸化物の被覆法として、最も広く実施されている
手法の一つは、インジウム系酸化物をターゲット材料と
して用いるスパッタリングターゲット法である。インジ
ウム系酸化物ターゲット材料の製造法は、インジウム系
酸化物粉末を成型し、その後、焼結する方法が一般に実
施されている方法である。しかしながら、インジウム系
酸化物は一般に難焼結性で、高密度でかつ強固な焼結体
を得ることが困難であるといわれており、通常の成型・
焼結法では、相対密度で高々70％までの焼結体しか得ら
れない。When an indium-based oxide or the like is used as an optoelectronic material, a glass or transparent film coated with an indium-based oxide is generally used. One of the most widely practiced methods for coating an indium-based oxide is a sputtering target method using an indium-based oxide as a target material. The method for producing an indium-based oxide target material is a method in which an indium-based oxide powder is molded and then sintered. However, indium-based oxides are generally difficult to sinter, and it is said that it is difficult to obtain a high-density and strong sintered body.
In the sintering method, only a sintered body having a relative density of up to 70% can be obtained.
［発明が解決しようとする問題点］ 本発明の目的は、高密度でかつ強固なインジウム系酸
化物焼結体の製造方法を提供することである。[Problems to be Solved by the Invention] An object of the present invention is to provide a method for producing a high-density and strong indium-based oxide sintered body.
［問題点を解決するための手段］ 本発明者等は、スパッタリングターゲット材料等のイ
ンジウム系酸化物焼結体の製造法を鋭意検討した結果、
特定の粒径及び分散性をもつインジウム系酸化物を用い
ることにより、高密度でかつ強固なインジウム系酸化物
の焼結体が得られることを見出し本発明を完成した。[Means for Solving the Problems] The present inventors have conducted intensive studies on a method for producing an indium-based oxide sintered body such as a sputtering target material.
The inventors have found that a high-density and strong sintered body of indium-based oxide can be obtained by using an indium-based oxide having a specific particle size and dispersibility, and completed the present invention.
なお、本発明で述べる高密度焼結体とは、少なくとも
相対密度が70％以上で内部にひびや割れのない強固な焼
結体を意味する。The high-density sintered body described in the present invention means a strong sintered body having a relative density of at least 70% and having no cracks or cracks inside.
本発明に用いるインジウム系酸化物とは、インジウム
酸化物、又は、インジウム酸化物を主成分とする酸化物
を意味する。このようなインジウム系酸化物は、化合物
半導体として公知のものであり、例えば、インジウム酸
化物に酸化スズ、及び／又は他の酸化物、又は、ハロゲ
ン系酸化物を添加した酸化物を意味する。The indium-based oxide used in the present invention means indium oxide or an oxide containing indium oxide as a main component. Such an indium-based oxide is known as a compound semiconductor, and means, for example, an oxide obtained by adding tin oxide and / or another oxide or a halogen-based oxide to indium oxide.
本発明のインジウム系酸化物焼結体の製造方法に於い
ては、平均粒径が１μｍ以下で、かつ１μｍ以上の粒径
をもつ粉末が20wt％以上で、粒度分布より求めた表面積
が2m2/g以上のインジウム系酸化物を原料として用いる
ことが必須である。In the method for producing an indium-based oxide sintered body of the present invention, the powder having an average particle size of 1 μm or less and having a particle size of 1 μm or more is 20 wt% or more, and the surface area determined from the particle size distribution is 2 m 2. It is essential to use an indium-based oxide of / g or more as a raw material.
本発明で用いるインジウム系酸化物粉末の一次粒径の
平均粒径は１μｍ以下であることが、高密度な焼結体を
得るために必要であり、平均粒径が１μｍを越えると、
高密度な焼結体を得ることはできない。又、１μｍ以上
の粒径をもつ粉末が20wt％以上であることは、緻密でか
つ強固な焼結体を得るために必要である。本発明者等の
検討によれば、緻密でかつ強固な焼結体を得るために
は、粉末の粒度分布はある程度巾を持つことが必要であ
り、特に、１μｍ以上の粒径をもつ粉末が20wt％以上存
在することが必要であることが判った。１μｍ以上の粒
径を持つ粉末が20wt％未満の場合は、得られる焼結体に
ひびや割れが発生するようになる。In order to obtain a high-density sintered body, it is necessary that the average particle diameter of the primary particle diameter of the indium-based oxide powder used in the present invention is 1 μm or less.
High-density sintered bodies cannot be obtained. It is necessary that the powder having a particle size of 1 μm or more be 20 wt% or more in order to obtain a dense and strong sintered body. According to the study of the present inventors, in order to obtain a dense and strong sintered body, the particle size distribution of the powder needs to have a certain width, and in particular, a powder having a particle size of 1 μm or more is required. It turned out that it is necessary to be present at 20 wt% or more. If the powder having a particle size of 1 μm or more is less than 20% by weight, cracks and cracks are generated in the obtained sintered body.
さらに、本発明のインジウム系酸化物焼結体の製造方
法に於いては、用いる粉末は、粒度分布より求めた表面
積が、2m2/g以上であることが必要であり、表面積が2m2
/g未満の場合は、高密度な焼結体を得ることが困難であ
る。Furthermore, in the manufacturing method of the indium-based oxide sintered body of the present invention, using the powder, the surface area determined from particle size distribution, must be at 2m 2 / g or more, a surface area of 2m 2
If it is less than / g, it is difficult to obtain a high-density sintered body.
尚、粉末の粒径、平均粒径、粒度分布の測定は電子顕
微鏡を用いた通常の方法で行なった。The measurement of the particle size, average particle size, and particle size distribution of the powder was performed by an ordinary method using an electron microscope.
本発明に用いるインジウム系酸化物粉末は、上記した
条件を満たせば、どのような方法で得たインジウム系酸
化物粉末も用いることができる。As the indium-based oxide powder used in the present invention, an indium-based oxide powder obtained by any method can be used as long as the above conditions are satisfied.
なお、上記条件を満たす粉末の調製法を幾つか例示す
れば、例えば、あらかじめ粉末合成時に粒径制御を行な
うか、あるいは、合成後の粉末を分級、粉砕、凝集等の
粉末処理技術により、粒度調製を行うなどの手段をあげ
ることができる。Some examples of methods for preparing powders satisfying the above conditions include, for example, controlling the particle size at the time of powder synthesis in advance, or classifying, synthesizing, pulverizing, and agglomerating the powder after synthesis using a powder processing technique such as agglomeration. Means such as preparation can be given.
例えば、比較的粒度の大きな粉末と、粒度の小さな粉
末を混合することにより、上記条件を満たすような混合
粉末を調製することができる。又、沈殿法等の微粒子合
成技術により、0.5μｍ以下の微粒子を合成し、この粉
末を湿式粉砕処理によりより細かい粒子に変化させた後
に、乾式粉砕や熱処理により、逆に粒子を凝集させ、よ
り大きな粒子に成長させた粉末を添加するような手法を
用いることにより調製することもできる。For example, by mixing a powder having a relatively large particle size and a powder having a small particle size, a mixed powder satisfying the above conditions can be prepared. Also, by a fine particle synthesis technique such as precipitation method, to synthesize fine particles of 0.5μm or less, after changing this powder into finer particles by wet pulverization, dry pulverization or heat treatment to conversely aggregate the particles, It can also be prepared by using a technique such as adding powder grown into large particles.
本発明は、上記のような特徴をもつ粉末を用いてこれ
を成型・焼結してインジウム系酸化物焼結体を製造す
る。According to the present invention, an indium-based oxide sintered body is manufactured by molding and sintering a powder having the above characteristics.
この際の成型法としては特に限定されないが、公知の
金型成型法やスリップキャスト成型法を用いることがで
きる。又、必要に応じ、CIP（Cold Isotherm Press）処
理などを施すことも可能である。又、上記成型体の焼結
は、真空中、酸素中、空気中、不活性ガス雰囲気中等任
意の雰囲気を選定して行なうことができるが、一般的に
は空気中1200〜1500℃程度の温度で実施する。The molding method at this time is not particularly limited, but a known mold molding method or slip cast molding method can be used. If necessary, CIP (Cold Isotherm Press) processing or the like can be performed. Further, the sintering of the molded body can be performed by selecting an arbitrary atmosphere such as in vacuum, in oxygen, in air, in an inert gas atmosphere, etc., and generally, in air at a temperature of about 1200 to 1500 ° C. It is carried out in.
［発明の効果］ 本発明により、高密度でかつ強固なインジウム系酸化
物焼結体を得ることができる。[Effect of the Invention] According to the present invention, a high-density and strong indium-based oxide sintered body can be obtained.
本発明により得られた焼結体は、例えば、インジウム
系酸化物ターゲット材料として用いることができ、光エ
レクトロニクス関連の素子や部品を作成するための材料
として用いることができる。The sintered body obtained by the present invention can be used, for example, as an indium-based oxide target material, and can be used as a material for producing optoelectronics-related elements and components.
［実施例］ 以下、実施例で本発明を詳述するが、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 detail with reference to examples, but the present invention is not limited thereto.
実施例１ In2 O395wt％、SnO25wt％の組成となるように混合
し、下記の粉末特性を持つ粉末Ａを調製した。粉末Ａ
は、平均粒径0.3μｍで１μｍ以上の粒径をもつ粉末の
割合は約5wt％であり、又粒度分布から求めた表面積は4
m2/gであった。Example 1 Powder A having the following powder characteristics was prepared by mixing so that a composition of In 2 O 3 95 wt% and SnO 2 5 wt% was obtained. Powder A
Is that the ratio of powder having an average particle size of 0.3 μm and a particle size of 1 μm or more is about 5 wt%, and the surface area determined from the particle size distribution is 4%.
m 2 / g.
一方、粉末Ｂは、平均粒径2.2μｍで１μｍ以上の粒
径をもつ粉末の割合は約90wt％であり、粒度分布から求
めた表面積は0.6m2/gであった。On the other hand, in powder B, the ratio of powder having an average particle size of 2.2 μm and a particle size of 1 μm or more was about 90 wt%, and the surface area determined from the particle size distribution was 0.6 m 2 / g.
さらに、上記粉末Ａと粉末Ｂを重量比で6:4の割合で
混合し、軽く湿式粉砕した粉末Ｃを調製した。粉末Ｃの
平均粒径は0.6μｍ、１μｍ以上の粒径を持つ粉末の割
合は約35wt％であり、又粒度分布から求めた表面積は3m
2/gであった。Further, the powder A and the powder B were mixed at a weight ratio of 6: 4 to prepare a powder C which was lightly wet-pulverized. The average particle size of powder C is 0.6 μm, the ratio of powder having a particle size of 1 μm or more is about 35 wt%, and the surface area determined from the particle size distribution is 3 m
2 / g.
この粉末を夫々150mmφの金型に充填し、油圧プレス
を行いその後CIP処理を施した。このようにして得られ
た成型体を、1350℃で５時間焼結した。Each of the powders was filled into a 150 mmφ mold, subjected to a hydraulic press, and then subjected to a CIP treatment. The molded body thus obtained was sintered at 1350 ° C. for 5 hours.
本発明の条件を満たす粉末Ｃを用いて成型し大気中で
焼結した焼結体は、相対密度90％の焼結密度を示し、又
この焼結体には、ひびや割れは発生しなかった。一方、
粉末Ａを用いて得た焼結体は、相対密度68％であり、又
粉末Ｂを用いて得た焼結体は、相対密度88％という高密
度を示したが一部に割れが発生した。A sintered body molded using powder C satisfying the conditions of the present invention and sintered in the atmosphere shows a sintered density of 90% relative density, and no crack or crack is generated in this sintered body. Was. on the other hand,
The sintered body obtained using the powder A had a relative density of 68%, and the sintered body obtained using the powder B showed a high density of 88% relative density, but some cracks occurred. .
実施例２ 実施例１の粉末Ａを乾式粉砕し、さらに1100℃で熱処
理を施し粉末Ｄを得た。粉末Ｄは平均粒径1.3μｍで１
μｍ以上の粉末の割合は60wt％、粒度分布より求めた表
面積は1.2m2/gであった。Example 2 Powder A of Example 1 was dry-pulverized and heat-treated at 1100 ° C to obtain powder D. Powder D has an average particle size of 1.3 μm and is 1
The proportion of powder having a particle size of μm or more was 60 wt%, and the surface area determined from the particle size distribution was 1.2 m 2 / g.
この粉末Ｄと、実施例１の粉末Ａを1:1の割合で混合
し、軽く湿式粉砕を行ない粉末Ｅを得た。粉末Ｅは、平
均粒径0.5μｍ、１μｍ以上の粉末の割合は25wt％、粒
度分布より求めた表面積は、3m2/gであった。This powder D and powder A of Example 1 were mixed at a ratio of 1: 1 and lightly wet-pulverized to obtain powder E. Powder E had an average particle size of 0.5 μm, a proportion of powder having a particle size of 1 μm or more was 25 wt%, and a surface area determined from the particle size distribution was 3 m 2 / g.
この粉末Ｅに、水を加え、分散剤（ヘキスト社製「Ａ
−40」…ポリカルボン酸アンモニウム塩系）、結合剤
（中京樹脂社製「WE−518」…アクリル系エマルジョ
ン）を夫々微量（約0.5wt％）添加し、撹拌してスラリ
ーを調製した。このスラリー濃度は75wt％であった。こ
の、スラリーを300mmφ、厚み10mmφの吸水性の石膏型
に流しこみ、スリップキャスト成型した。石膏型への着
肉後着肉体を取り出し、乾燥して相対密度45％の成型体
を得た。この成型体を大気中1400℃で３時間焼結したと
ころ、相対密度85％で、ひびや割れのない強固な焼結体
が得られた。Water is added to the powder E, and a dispersant ("A" manufactured by Hoechst)
-40 ": a polycarboxylic acid ammonium salt) and a binder (" WE-518 ", an acrylic emulsion manufactured by Chukyo Resin Co., Ltd.) were added in small amounts (about 0.5 wt%), and stirred to prepare a slurry. The slurry concentration was 75% by weight. This slurry was poured into a water-absorbing gypsum mold having a diameter of 300 mm and a thickness of 10 mm, and was subjected to slip casting. After the inlay on the gypsum mold, the inlaid body was taken out and dried to obtain a molded body having a relative density of 45%. When this molded body was sintered in the atmosphere at 1400 ° C. for 3 hours, a strong sintered body having a relative density of 85% and no cracks or cracks was obtained.
Claims (1)
の粒径をもつ粉末が20wt％以上で、粒度分布より求めた
表面積が、2m2/g以上のインジウム系酸化物を原料とし
て用いて、成型、焼結することを特徴とするインジウム
系酸化物の焼結体の製造方法1. An indium oxide having an average particle diameter of 1 μm or less, a powder having a particle diameter of 1 μm or more, 20 wt% or more, and a surface area determined from a particle size distribution of 2 m 2 / g or more is used as a raw material. For producing a sintered body of an indium-based oxide, characterized by being molded and sintered
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1158164A JP2756586B2 (en) | 1989-06-22 | 1989-06-22 | Manufacturing method of oxide sintered body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1158164A JP2756586B2 (en) | 1989-06-22 | 1989-06-22 | Manufacturing method of oxide sintered body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0328156A JPH0328156A (en) | 1991-02-06 |
| JP2756586B2 true JP2756586B2 (en) | 1998-05-25 |
Family
ID=15665670
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1158164A Expired - Fee Related JP2756586B2 (en) | 1989-06-22 | 1989-06-22 | Manufacturing method of oxide sintered body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2756586B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2794679B2 (en) * | 1992-02-17 | 1998-09-10 | 同和鉱業株式会社 | Method for producing high-density ITO sintered body |
-
1989
- 1989-06-22 JP JP1158164A patent/JP2756586B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0328156A (en) | 1991-02-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5071800A (en) | Oxide powder, sintered body, process for preparation thereof and targe composed thereof | |
| WO1994018138A1 (en) | Method of manufacturing an ito sintered body, and article produced thereby | |
| KR101155358B1 (en) | Composite oxide sinter, process for producing amorphous composite oxide film, amorphous composite oxide film, process for producing crystalline composite oxide film, and crystalline composite oxide film | |
| JPH0971860A (en) | Target and manufacturing method thereof | |
| TWI401211B (en) | Indium oxide powder and method for producing same | |
| JPH0754132A (en) | ITO sintered body and sputtering target | |
| JP2756586B2 (en) | Manufacturing method of oxide sintered body | |
| JPH03126655A (en) | Indium oxide-tin oxide sintered body and method for producing the same | |
| JP4724330B2 (en) | Tin-antimony oxide sintered compact target and method for producing the same | |
| CN112624619A (en) | Quartz nanocrystalline microcrystalline glass synthesized by desert aeolian sand and synthetic method thereof | |
| JP5720726B2 (en) | Zinc oxide sintered body and method for producing the same | |
| TW201925501A (en) | IZO target and manufacturing method of the same in which the film resistance of a sputtered film is not easily affected by the oxygen concentration at the time of sputtering | |
| JP4508079B2 (en) | Manufacturing method of sputtering target | |
| WO2023167030A1 (en) | Opaque quartz glass and production method therefor | |
| JP2984581B2 (en) | Member composed of indium-tin oxide and method for producing the same | |
| JP2663636B2 (en) | Molding method of oxide powder | |
| CN1113831C (en) | In-situ synthesis process for preparing complex-phase TiN/O'-sialon material | |
| JPH0474860A (en) | Ito sputtering target material and its production | |
| JPWO2019187269A1 (en) | Oxide sintered body, sputtering target and transparent conductive film | |
| JPH09124364A (en) | Ito sintered compact for forming transparent electroconductive film and its production | |
| JPH01290551A (en) | Production of target for sputtering to be used for production of transparent electroconductive film | |
| JPH02149424A (en) | White color conductive material and its production | |
| JPS59207883A (en) | Manufacture of aluminum nitride sintered body | |
| CN120923249A (en) | Preparation method of glass-coated silicon nitride ceramic powder and silicon nitride ceramic | |
| KR19990055001A (en) | Method for manufacturing silica radome using slip casting method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |