JPH0811711B2 - Method for manufacturing sputtering target for transparent conductive film - Google Patents
Method for manufacturing sputtering target for transparent conductive filmInfo
- Publication number
- JPH0811711B2 JPH0811711B2 JP63117137A JP11713788A JPH0811711B2 JP H0811711 B2 JPH0811711 B2 JP H0811711B2 JP 63117137 A JP63117137 A JP 63117137A JP 11713788 A JP11713788 A JP 11713788A JP H0811711 B2 JPH0811711 B2 JP H0811711B2
- Authority
- JP
- Japan
- Prior art keywords
- ito
- target
- conductive film
- transparent conductive
- sputtering target
- 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)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明はLEディスプレイ，液晶ディスプレイ面発熱
体，タッチパネルなどの透明導電膜をスパッタリング法
で形成する際に用いられるスパッタリングターゲットに
関するものである。TECHNICAL FIELD The present invention relates to a sputtering target used when forming a transparent conductive film such as an LE display, a liquid crystal display surface heating element, and a touch panel by a sputtering method.
（従来の技術） 近年、薄膜化技術の発達に伴い表示素子分野などでは
透明導電膜が利用されてきている。現在、透明導電膜の
材質として酸化インジウム−酸化スズ（以下、ITOとい
う）が安定性，高光透過性など理由から多く用いられて
いる。また、ITOからなる透明導電膜の作製方法として
は蒸着法，インジウム−スズメタルターゲットを用いた
反応性スパッタ法,ITOターゲットを用いたスパッタリン
グ法が知られており、特に成膜コントロールの容易さか
らITOターゲットを用いたスパッタリング法が主流とな
っている。(Prior Art) In recent years, a transparent conductive film has been used in the field of display elements and the like with the development of thinning technology. At present, indium oxide-tin oxide (hereinafter referred to as ITO) is often used as a material for the transparent conductive film for reasons such as stability and high light transmittance. Further, as a method for producing a transparent conductive film made of ITO, a vapor deposition method, a reactive sputtering method using an indium-tin metal target, and a sputtering method using an ITO target are known. The sputtering method using an ITO target is the mainstream.
従来ITOターゲットは、ITO粉末を金型プレス法により
成型して得た成型体を焼成することにより得られてい
る。しかしながら、酸化インジウム及び酸化スズは1400
〜1450℃程度の温度から昇華するため、ITOターゲット
の製造時の焼成温度は1300〜1450℃に限定されてしま
い、また酸化インジウム及び酸化スズは難焼結性である
ことから、得られるITOターゲットの相対密度は70％未
満と低くなるという問題点がある。通常、相対密度の低
いターゲットは抵抗率が高い、抗折力が弱い熱伝導率が
低いため、この様なターゲットを用いてスパッタリング
を行った場合、異常放電が発生し、得られるITO透明導
電膜に悪影響を及ぼす。Conventionally, an ITO target has been obtained by firing a molded body obtained by molding ITO powder by a die pressing method. However, indium oxide and tin oxide are 1400
Since it sublimates from a temperature of approximately 1450 ° C, the firing temperature during manufacturing of the ITO target is limited to 1300-1450 ° C, and indium oxide and tin oxide are difficult to sinter, so the ITO target obtained is There is a problem that the relative density of is as low as less than 70%. Usually, a target with low relative density has high resistivity, weak transverse rupture strength, and low thermal conductivity, so when sputtering is performed using such a target, abnormal discharge occurs and the resulting ITO transparent conductive film is obtained. Adversely affect.
（発明が解決しようとする問題点） 本発明の目的は、相対密度の高いITOスパッタリング
ターゲットの製造方法を提供することにある。(Problems to be Solved by the Invention) An object of the present invention is to provide a method for manufacturing an ITO sputtering target having a high relative density.
（問題を解決するための手段） 本発明者らは上記問題点を解決するために鋭意検討を
行った結果、ITO成型体を冷間静水圧プレスにより圧密
化した後、焼成を行えば相対密度の高いターゲットが得
られることを見出だし本発明を完成するに至った。すな
わち本発明は、酸化インジウム−酸化スズを含有する粉
末を泥漿鋳込み成型により予備成型して得られた成形体
を冷間静水圧プレスにより圧密化し、次いで焼成するこ
とを特徴とする透明導電膜用スパッタリングターゲット
の製造方法である。(Means for Solving the Problem) As a result of intensive studies for solving the above-mentioned problems, the present inventors have found that the ITO molded body is consolidated by cold isostatic pressing and then fired to obtain a relative density. It has been found that a high target can be obtained, and the present invention has been completed. That is, the present invention is for a transparent conductive film, characterized in that a compact obtained by preforming a powder containing indium oxide-tin oxide by sludge casting molding is consolidated by cold isostatic pressing and then fired. It is a method of manufacturing a sputtering target.
本発明において用いられるITO粉末は市販の酸化イン
ジウム粉末と酸化スズ粉末を混合する方法や共沈法など
によって得ることができるが、通常酸化インジウムを70
重量％以上含有するITO粉末が用いられる。更に、スパ
ッタ後に得られる透明導電膜の導電性，光透過性を向上
させるためにこれらITO粉末に第三成分を添加した粉末
を用いても何ら差支えない。The ITO powder used in the present invention can be obtained by a method of mixing a commercially available indium oxide powder and a tin oxide powder or a coprecipitation method.
ITO powder containing at least wt% is used. Furthermore, there is no problem even if powders obtained by adding a third component to these ITO powders are used in order to improve the conductivity and light transmittance of the transparent conductive film obtained after sputtering.
予備成型の方法はITO粉末と溶媒，分散剤及びバイン
ダーを混合して得られたスラリーを、例えばセッコウ型
などの吸水性のある多孔質成形型に、常圧あるいは加圧
下で鋳込み成型する鋳込み成型法などの採用することが
できる。鋳込み成型法により所望形状、大きさのターゲ
ットを得ることができるので好ましい。また、鋳込み成
型法により予備成型を行う場合、スラリーを得るための
溶媒としては通常水が用いられ、分散剤としては例えば
ポリカルボン酸系のものなどが、バインダーとしてはア
クリルエマルジョン系のものなどが用いられるが、これ
らに限定はされない。また、このときのスラリー濃度と
しては75〜83％である。スラリー濃度が70％未満である
場合、ターゲットの作製中に割れが生じ易くなるおそれ
がある。The pre-molding method is a cast molding in which a slurry obtained by mixing ITO powder with a solvent, a dispersant and a binder is cast into a water-absorbing porous molding die such as a gypsum mold under normal pressure or pressure. The law can be adopted. It is preferable because a target having a desired shape and size can be obtained by the casting method. Further, when performing preforming by a casting method, water is usually used as a solvent for obtaining a slurry, a polycarboxylic acid type as a dispersant, and an acrylic emulsion type as a binder. Used, but not limited to. The slurry concentration at this time is 75 to 83%. If the slurry concentration is less than 70%, cracks may easily occur during the production of the target.
上記予備成型により得られたITO成型体を冷間静水圧
プレスにより圧密化し、焼成を行うことにより相対密度
の大きいITOターゲットが得られる。An ITO target having a large relative density can be obtained by consolidating the ITO molded body obtained by the above preliminary molding by cold isostatic pressing and firing it.
冷間静水圧プレスは３〜5ton/cm2で行う。該冷間静水
圧プレスを施すことにより、あらかじめITO成型体は圧
密化し、密度が大きくなるので、これを焼成することに
より相対密度の大きいITOターゲットを得ることができ
る。加圧が1ton/cm2未満の場合、焼成を行い得られるタ
ーゲットの相対密度が顕著に向上しないおそれがある。
また焼成は、1300〜1450℃で１時間以上行うことが好ま
しい。Cold isostatic pressing is performed at 3 to 5 ton / cm 2 . By performing the cold isostatic pressing, the ITO molded body is preliminarily consolidated and the density becomes large. Therefore, by firing this, an ITO target having a large relative density can be obtained. If the pressure is less than 1 ton / cm 2 , the relative density of the target obtained by firing may not be significantly improved.
The firing is preferably performed at 1300 to 1450 ° C for 1 hour or more.
以上の方法により得られたITOターゲットは相対密度
が70％以上と高いものとなり、ターゲット特性も良好な
ものとなる。The ITO target obtained by the above method has a high relative density of 70% or more, and has good target characteristics.
（実施例） 以下、実施例により本発明を更に詳しく説明するが、
本発明は何ら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.
The present invention is not limited to these.
実施例１ 市販の酸化インジウム粉末2250g、酸化スズ粉末250
g、ポリカルボン酸系分散剤（固形分40％）56.25g、ア
クリルエマルジョン系バインダー（固形分40％）56.25g
及び純水569gを10ナイロン製ポット中で直径15mmの鉄
芯入り樹脂ボールを用いて回転ボールミルにより16時間
混合し、スラリー濃度80％のITO粉末スラリーを得た。Example 1 2250 g of commercially available indium oxide powder, 250 of tin oxide powder
g, polycarboxylic acid type dispersant (solid content 40%) 56.25g, acrylic emulsion type binder (solid content 40%) 56.25g
Then, 569 g of pure water was mixed in a pot made of 10 nylon with a resin ball containing an iron core having a diameter of 15 mm for 16 hours by a rotary ball mill to obtain an ITO powder slurry having a slurry concentration of 80%.
得られたスラリーを充分脱泡した後、内寸法160×480
×10tのセッコウ型を用いた加圧鋳込み成型により予備
成型を行い、ITO成型体を得た。After thoroughly degassing the resulting slurry, the internal dimensions are 160 x 480
Pre-molding was performed by pressure casting using a gypsum mold of × 10 t to obtain an ITO molded body.
その後、得られた成型体を冷間静水圧プレスにて5ton
/cm2の圧力で圧密化し、脱バインダーを行い、1350℃で
５時間焼成しITO焼結体を得、これを放電加工及び平面
研削で加工し、127×381×6tのITOターゲットを得た。After that, the obtained molded body was subjected to 5 tons with a cold isostatic press.
It is consolidated at a pressure of / cm 2 , debindered, baked at 1350 ° C for 5 hours to obtain an ITO sintered body, which is processed by electrical discharge machining and surface grinding to obtain a 127 × 381 × 6 t ITO target. It was
得られたターゲットの相対密度は76.8％であった。ま
た、ターゲットの抵抗率，抗折力及び熱伝導率を測定し
た。その結果を表１に示す。The relative density of the obtained target was 76.8%. The resistivity, transverse rupture strength and thermal conductivity of the target were also measured. Table 1 shows the results.
比較例 市販の酸化インジウム粉末4950gと酸化スズ粉末550
g、ポリカルボン酸系分散剤（固形分40％）100g、アク
リルエマルジョン系バインダー（固形分40％）100gおよ
び純水2885gを10ナイロン製ポットで直径15mmの鉄心
入れ樹脂ボールを用いて回転ボールミルにより16時間混
合し、スラリー濃度65％のITO粉末スラリーを得た。Comparative Example 4950 g of commercially available indium oxide powder and 550 of tin oxide powder
g, polycarboxylic acid-based dispersant (solid content 40%) 100 g, acrylic emulsion-based binder (solid content 40%) 100 g and pure water 2885 g in a 10-nylon pot by using a rotating ball mill with an iron core resin ball with a diameter of 15 mm. The mixture was mixed for 16 hours to obtain an ITO powder slurry having a slurry concentration of 65%.
該スラリーを用いて実施例１と同様の条件で加圧鋳込
み成型を行ったところ、得られたITO予備成形体にはク
ラックが入った。When pressure casting was performed using the slurry under the same conditions as in Example 1, the resulting ITO preform had cracks.
このクラックが入ったITO予備成形体が冷間静水圧プ
レスにて5ton/cm2の圧力で圧密化し、脱バインダーを行
い、1350℃で５時間焼成したところ、焼結体は割れてし
まい目的とするターゲットを得ることができなかった。The cracked ITO preform was consolidated with a cold isostatic press at a pressure of 5 ton / cm 2 , debindered, and fired at 1350 ° C. for 5 hours. Could not get the target to.
（発明の効果） 以上述べたとおり、本発明によれば相対密度70％を越
えるITOターゲットを得ることができ、このターゲット
は抵抗率，抗折力及び熱伝導率にすぐれたものであり、
スパッタリング時に放電の安定性が良好となる。更に密
度が高いので、スパッタレートが高くなり、成膜の生産
性が高くなる。 (Effect of the invention) As described above, according to the present invention, an ITO target having a relative density of more than 70% can be obtained, and this target is excellent in resistivity, transverse rupture strength and thermal conductivity,
The stability of discharge becomes good during sputtering. Further, since the density is high, the sputter rate is high and the productivity of film formation is high.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭62−12009（ＪＰ，Ａ) 特開 昭60−65760（ＪＰ，Ａ) 特開 昭62−278004（ＪＰ，Ａ) 特開 昭59−136210（ＪＰ，Ａ) 特開 昭58−175620（ＪＰ，Ａ) 特開 昭50−89408（ＪＰ，Ａ) 素木洋一著「セラミックス製造プロセス ▲Ｉ▼」（1978年10月10日技報堂出版発 行）Ｐ．175−180，197，198 ─────────────────────────────────────────────────── ─── Continuation of front page (56) Reference JP 62-12009 (JP, A) JP 60-65760 (JP, A) JP 62-278004 (JP, A) JP 59- 136210 (JP, A) JP 58-175620 (JP, A) JP 50-89408 (JP, A) Yoichi Aoki, "Ceramics Manufacturing Process I" (October 10, 1978 Gihodo Publishing Publishing Line) P. 175-180, 197, 198
Claims (1)
酸化インジウム−酸化スズ含有粉末をスラリー濃度75〜
83％にて泥漿鋳込みにより予備成して得られた成型体
を、３〜5ton/cm2の冷間静水圧プレスにより圧密化し、
次いで焼成することを特徴とする透明導電膜用スパッタ
リングターゲットの製造方法。1. Indium oxide is contained in an amount of 70% by weight or more,
Indium oxide-tin oxide containing powder slurry concentration 75 ~
The molded body obtained by preforming by sludge casting at 83% was consolidated by a cold isostatic press of 3 to 5 ton / cm 2 ,
A method of manufacturing a sputtering target for a transparent conductive film, which is characterized by firing.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63117137A JPH0811711B2 (en) | 1988-05-16 | 1988-05-16 | Method for manufacturing sputtering target for transparent conductive film |
| DE68924095T DE68924095T2 (en) | 1988-05-16 | 1989-05-12 | Method for producing a sputtering target for producing an electrically conductive, transparent layer. |
| EP89108558A EP0342537B1 (en) | 1988-05-16 | 1989-05-12 | Process for the manufacture of a sputtering target for producing electroconductive transparent films |
| CA000599638A CA1337809C (en) | 1988-05-16 | 1989-05-15 | Sputtering target for producing electroconductive transparent films and process for manufacture thereof |
| KR1019890006539A KR940003786B1 (en) | 1988-05-16 | 1989-05-16 | Manufacturing method of sputtering target for transparent conductive film |
| US07/352,473 US5160675A (en) | 1988-05-16 | 1989-05-16 | Sputtering target for producing electroconductive transparent films and process for manufacture thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63117137A JPH0811711B2 (en) | 1988-05-16 | 1988-05-16 | Method for manufacturing sputtering target for transparent conductive film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01290551A JPH01290551A (en) | 1989-11-22 |
| JPH0811711B2 true JPH0811711B2 (en) | 1996-02-07 |
Family
ID=14704369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63117137A Expired - Fee Related JPH0811711B2 (en) | 1988-05-16 | 1988-05-16 | Method for manufacturing sputtering target for transparent conductive film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0811711B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03207858A (en) * | 1990-01-08 | 1991-09-11 | Nippon Mining Co Ltd | Production of ito sputtering target |
| JPH0779005B2 (en) * | 1990-06-19 | 1995-08-23 | 住友金属鉱山株式会社 | ITO sintered body and manufacturing method thereof |
| JP3184977B2 (en) * | 1990-07-12 | 2001-07-09 | 同和鉱業株式会社 | Method for producing ITO sputtering target material |
| GB2459917B (en) | 2008-05-12 | 2013-02-27 | Sinito Shenzhen Optoelectrical Advanced Materials Company Ltd | A process for the manufacture of a high density ITO sputtering target |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6065760A (en) * | 1983-09-21 | 1985-04-15 | 東ソー株式会社 | Manufacture of highly electroconductive tin oxide film material |
| JPS6212009A (en) * | 1985-07-09 | 1987-01-21 | 昭和電工株式会社 | Formation of indium oxide based low resistance transparent thin film |
-
1988
- 1988-05-16 JP JP63117137A patent/JPH0811711B2/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 素木洋一著「セラミックス製造プロセス▲Ｉ▼」（１９７８年１０月１０日技報堂出版発行）Ｐ．１７５−１８０，１９７，１９８ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01290551A (en) | 1989-11-22 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |