JPH0570942A - High density sintered target material for forming electric conductive transparent thin film by sputtering - Google Patents
High density sintered target material for forming electric conductive transparent thin film by sputteringInfo
- Publication number
- JPH0570942A JPH0570942A JP3259903A JP25990391A JPH0570942A JP H0570942 A JPH0570942 A JP H0570942A JP 3259903 A JP3259903 A JP 3259903A JP 25990391 A JP25990391 A JP 25990391A JP H0570942 A JPH0570942 A JP H0570942A
- Authority
- JP
- Japan
- Prior art keywords
- target material
- thin film
- sputtering
- sintered target
- transparent thin
- 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.)
- Withdrawn
Links
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Electric Cables (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、高密度と低い比抵抗
を有し、これによって高強度が確保され、かつスパッタ
リングによる速い成膜速度で、導電性の一段と良好な透
明導電性薄膜の安定的形成を可能ならしめる焼結ターゲ
ット材に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention has a high density and a low specific resistance, whereby high strength is secured, and at a high film-forming rate by sputtering, the conductivity of the transparent conductive thin film is further improved. The present invention relates to a sintered target material that enables the target formation.
【０００２】[0002]
【従来の技術】従来、一般に、透明導電性薄膜が、液晶
表示装置やＥＬ表示装置の透明電極、および帯電防止用
被膜などとして用いられ、さらにガスセンサーなどにも
適用されている。2. Description of the Related Art Conventionally, a transparent conductive thin film has been generally used as a transparent electrode of a liquid crystal display device or an EL display device, an antistatic coating film and the like, and further applied to a gas sensor and the like.
【０００３】また、上記透明導電性薄膜が、重量％で
（以下％は重量％を示す）、 酸化スズ（以下ＳｎＯ2 で示す）：５〜１５％、 を含有し、残りが酸化インジウム（以下Ｉｎ2 Ｏ3 で示
す）と不可避不純物からなる組成を有する焼結ターゲッ
ト材を用い、スパッタリングにより形成されることも知
られている。Further, the transparent conductive thin film contains, by weight (hereinafter,% represents weight%), tin oxide (hereinafter represented by SnO 2 ): 5 to 15%, and the remainder is indium oxide (hereinafter It is also known to be formed by sputtering using a sintered target material having a composition of In 2 O 3 ) and inevitable impurities.
【０００４】[0004]
【発明が解決しようとする課題】しかし、上記の従来焼
結ターゲット材は、焼結性に劣るために、通常の粉末冶
金法では６０％程度までの理論密度比しか確保すること
ができず、この結果強度不足が原因で成膜中に割れが発
生し易く、また理論密度比が低いことから、成膜速度が
遅く、かつスパッタ状態が不安定になるなどの問題点を
もつものである。However, since the above-mentioned conventional sintering target material is inferior in sinterability, it is possible to secure only a theoretical density ratio of up to about 60% by the usual powder metallurgy method. As a result, there are problems that cracks are likely to occur during film formation due to insufficient strength, and the theoretical density ratio is low, so that the film formation rate is slow and the sputtering state becomes unstable.
【０００５】[0005]
【課題を解決するための手段】そこで、本発明者等は、
上述のような観点から、上記の従来焼結ターゲット材に
着目し、これの高密度化をはかるべく研究を行なった結
果、上記のスパッタリングによる透明導電性薄膜の形成
に用いられている従来焼結ターゲット材に、酸化ジルコ
ニウム（以下ＺｒＯ2 で示す）および酸化イットリウム
（以下Ｙ2 Ｏ3 で示す）のうちの１種または２種を０．
０１〜５％の割合で含有させると、通常の粉末冶金法、
すなわち普通焼結だけで理論密度比で９０％以上に高密
度化するばかりでなく、比抵抗も低下するようになり、
この結果の焼結ターゲット材は、高強度と低い比抵抗を
もつようになることから、成膜中の割れがなくなり、か
つ速い成膜速度で安定して薄膜を形成することができ、
さらにＺｒＯ2 およびＹ2 Ｏ3 の作用で、形成された薄
膜の導電性が向上するようになるという研究結果を得た
のである。Therefore, the present inventors have
From the above viewpoints, we focused on the above-mentioned conventional sintering target material and conducted research to increase the density of the target material. As a result, the conventional sintering used for forming the transparent conductive thin film by the above-mentioned sputtering. One or two kinds of zirconium oxide (hereinafter referred to as ZrO 2 ) and yttrium oxide (hereinafter referred to as Y 2 O 3 ) were added to the target material at 0.
When it is contained at a rate of 01 to 5%, the usual powder metallurgy method,
That is to say, not only does the normal density increase the theoretical density ratio to 90% or more, but the specific resistance also decreases.
Since the resulting sintered target material has high strength and low specific resistance, cracks during film formation are eliminated, and a thin film can be stably formed at a high film formation rate.
Furthermore, they obtained the research result that the conductivity of the formed thin film is improved by the action of ZrO 2 and Y 2 O 3 .
【０００６】この発明は、上記の研究結果にもとづいて
なされたものであって、 ＳｎＯ2 ：５〜１５％、 ＺｒＯ2 およびＹ2 Ｏ3 のうちの１種または２種：０．
０１〜５％、 を含有し、残りがＩｎ2 Ｏ3 と不可避不純物からなる組
成、並びに、９０％以上の理論密度比、を有するスパッ
タリングによる透明導電性薄膜形成用高密度焼結ターゲ
ット材に特徴を有するものである。The present invention has been made based on the above-mentioned research results. SnO 2 : 5 to 15%, one or two of ZrO 2 and Y 2 O 3 : 0.
Characterized by a high-density sintered target material for forming a transparent conductive thin film by sputtering, which has a composition containing 01 to 5% and the balance of In 2 O 3 and unavoidable impurities, and a theoretical density ratio of 90% or more. Is to have.
【０００７】つぎに、この発明の高密度焼結ターゲット
材において、成分組成および理論密度比を上記の通りに
限定した理由を説明する。 Ａ 成分組成 （ａ） ＳｎＯ2 ＳｎＯ2 成分には、導電性を向上させる作用があるが、
その含有量が５％未満でも、また１５％を越えても所望
の良好な導電性を確保することができないことから、そ
の含有量を５〜１５％と定めた。Next, the reason why the component composition and the theoretical density ratio of the high density sintered target material of the present invention are limited as described above will be explained. Component A composition (a) SnO 2 SnO 2 component has the effect of improving conductivity,
If the content is less than 5% or more than 15%, the desired good conductivity cannot be ensured, so the content is defined as 5 to 15%.
【０００８】（ｂ） ＺｒＯ2 およびＹ2 Ｏ3 これらの成分には、上記の通り焼結性を向上させて高密
度化し、もって焼結ターゲット材の強度を高めると共
に、比抵抗を下げる作用があるが、その含有量が０．０
１％未満では前記作用に所望の効果が得られず、一方そ
の含有量が５％を越えるても所望の低い比抵抗を確保す
ることができないことから、その含有量を０．０１〜５
％と定めた。(B) ZrO 2 and Y 2 O 3 These components have the functions of improving the sinterability and increasing the density as described above, thereby increasing the strength of the sintered target material and reducing the specific resistance. However, its content is 0.0
If the content is less than 1%, the desired effect cannot be obtained, while if the content exceeds 5%, the desired low specific resistance cannot be secured.
Defined as%.
【０００９】なお、ＺｒＯ2 およびＹ2 Ｏ3 の単独含有
により共存含有した場合に上記作用により顕著な効果が
現われ、かつ０．２〜０．６％の範囲内の含有量で、強
度では最高値、比抵抗では最小値を示すものである。When both ZrO 2 and Y 2 O 3 are contained together, the above-mentioned effects have a remarkable effect, and when the content is within the range of 0.2 to 0.6%, the strength is the highest. The value and the specific resistance show the minimum value.
【００１０】Ｂ 理論密度比 上記の通りＺｒＯ2 およびＹ2 Ｏ3 の含有によって焼結
ターゲット材が高密度化し、９０％以上の理論密度比を
もつようになるものであり、したがって理論密度比が９
０％未満では所望の高強度を確保することができないこ
とから、その理論密度比を９０％以上と定めた。B Theoretical Density Ratio As described above, the inclusion of ZrO 2 and Y 2 O 3 densifies the sintered target material to have a theoretical density ratio of 90% or more. 9
If it is less than 0%, the desired high strength cannot be secured, so the theoretical density ratio was set to 90% or more.
【００１１】つぎに、この発明の焼結ターゲット材を実
施例により具体的に説明する。Next, the sintering target material of the present invention will be specifically described by way of examples.
【実施例】原料粉末として、０．２〜１０μｍ範囲内の
所定の平均粒径を有するＩｎ2 Ｏ3 粉末、ＳｎＯ2 粉
末、ＺｒＯ2粉末、およびＹ2 Ｏ3 粉末を用い、これら
原料粉末を表１〜３に示される配合組成に配合し、ボー
ルミルで５０時間粉砕混合した後、１ton ／cm2 の圧力
で直径：３０mm×厚さ：４mmの寸法をもった圧粉体にプ
レス成形し、この圧粉体を、大気中、１３００〜１５０
０℃の範囲内の所定の温度に３時間保持の条件で焼結す
ることにより実質的に配合組成と同一の成分組成を有す
る本発明焼結ターゲット材１〜２７および比較ターゲッ
ト材１〜４をそれぞれれ製造した。Example As the raw material powder, In 2 O 3 powder, SnO 2 powder, ZrO 2 powder, and Y 2 O 3 powder having a predetermined average particle size within the range of 0.2 to 10 μm were used. After blending with the blending composition shown in Tables 1 to 3 and pulverizing and mixing with a ball mill for 50 hours, it is pressed into a powder compact having a diameter of 30 mm and a thickness of 4 mm at a pressure of 1 ton / cm 2 , This green compact is placed in the atmosphere at 1300 to 150
The sintered target materials 1 to 27 of the present invention and the comparative target materials 1 to 4 having substantially the same composition as the compounded composition were obtained by sintering at a predetermined temperature within the range of 0 ° C. for 3 hours. Each was manufactured.
【００１２】[0012]
【表１】 [Table 1]
【００１３】[0013]
【表２】 [Table 2]
【００１４】[0014]
【表３】 [Table 3]
【００１５】この結果得られた各種の焼結ターゲット材
について、理論密度比、強度を評価する目的で抗折力、
および比抵抗を測定した。この測定結果を表１〜３に示
した。また、上記の各種焼結ターゲット材を用い、ＤＣ
マグネトロンスパッタリングにて、 雰囲気圧力：５×１０-3torr、 投入電力：４．２Ｗ／cm3 、 基材材質：スライドガラス（Ｂ２７０）、 基板温度：２５０℃、 時間：２０分、 の条件で薄膜を形成し、成膜速度と薄膜の比抵抗を測定
した。この測定結果も表１〜３に示した。With respect to the various sintered target materials obtained as a result, the transverse rupture strength was measured for the purpose of evaluating the theoretical density ratio and strength.
And the specific resistance was measured. The measurement results are shown in Tables 1 to 3. In addition, using the above various sintering target materials, DC
By magnetron sputtering, atmospheric pressure: 5 × 10 -3 torr, input power: 4.2 W / cm 3 , base material: slide glass (B270), substrate temperature: 250 ° C, time: 20 minutes, thin film Was formed, and the film formation rate and the specific resistance of the thin film were measured. The measurement results are also shown in Tables 1 to 3.
【００１６】[0016]
【発明の効果】表１〜３に示される結果から、本発明焼
結ターゲット材１〜２７は、いずれもＺｒＯ2 およびＹ
2 Ｏ3 を含有しない従来焼結ターゲット材に相当する比
較焼結ターゲット材１に比して、一段と高密度化し、相
対的に高い強度と速い成膜速度を示し、かつＺｒＯ2 お
よびＹ2 Ｏ3 の含有によってターゲット材および形成さ
れた薄膜も比抵抗が低下するようになるのに対して、比
較焼結ターゲット材２〜４に見られるように、ＺｒＯ2
および／またはＹ2 Ｏ3 の含有量がこの発明の範囲から
外れて高くなると比抵抗が高くなることが明らかであ
る。From the results shown in Tables 1 to 3, the sintered target materials 1 to 27 of the present invention are all ZrO 2 and Y.
Compared with the comparative sintered target material 1 corresponding to the conventional sintered target material which does not contain 2 O 3 , the density is further increased, and relatively high strength and high film formation rate are exhibited, and ZrO 2 and Y 2 O The target material and the formed thin film also have a lower specific resistance due to the inclusion of 3 , whereas ZrO 2 cannot be used as seen in the comparative sintered target materials 2 to 4.
It is clear that when the content of Y 2 O 3 and / or Y 2 O 3 is out of the range of the present invention, the resistivity becomes high.
【００１７】上述のように、この発明の高密度焼結ター
ゲット材は、高い強度と低い比抵抗を有するので、これ
を用いてのスパッタリングによる透明導電性薄膜の形成
に際しては、成膜中の割れ発生がなく、かつ速い成膜速
度で安定した薄膜形成ができ、さらに焼結ターゲット材
に含有するＺｒＯ2 およびＹ2 Ｏ3 が薄膜の導電性およ
び透明性の向上にも寄与するなど工業上有用な効果をも
たらすものである。As described above, the high-density sintered target material of the present invention has high strength and low specific resistance. Therefore, when forming a transparent conductive thin film by sputtering using this, cracking during film formation occurs. It is industrially useful, since it does not occur and a stable thin film can be formed at a high deposition rate, and ZrO 2 and Y 2 O 3 contained in the sintering target material contribute to the improvement of the conductivity and transparency of the thin film. It has a great effect.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 // Ｈ０１Ｂ 13/00 ５０３ Ｂ 7244−5Ｇ (72)発明者 杉原 忠 埼玉県大宮市北袋町１−297 三菱マテリ アル株式会社中央研究所内 (72)発明者 武下 拓夫 埼玉県大宮市北袋町１−297 三菱マテリ アル株式会社中央研究所内─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification number Internal reference number FI technical display location // H01B 13/00 503 B 7244-5G (72) Inventor Tadashi Sugihara 1 Kitabukuro-cho, Omiya-shi, Saitama Prefecture −297 Mitsubishi Materials Co., Ltd. Central Research Laboratory (72) Inventor Takuo Takeshita 1-297 Kitabukuro-cho, Omiya City, Saitama Prefecture 297 Mitsubishi Materiality Co., Ltd. Central Research Laboratory
Claims (1)
または２種：０．０１〜５％、を含有し、残りが酸化イ
ンジウムと不可避不純物からなる組成、並びに、 ９０％以上の理論密度比、を有することを特徴とするス
パッタリングによる透明導電性薄膜形成用高密度焼結タ
ーゲット材。1. By weight%, tin oxide: 5 to 15%, one or two kinds of zirconium oxide and yttrium oxide: 0.01 to 5%, and the balance is composed of indium oxide and inevitable impurities. And a theoretical density ratio of 90% or more, a high-density sintered target material for forming a transparent conductive thin film by sputtering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3259903A JPH0570942A (en) | 1991-09-11 | 1991-09-11 | High density sintered target material for forming electric conductive transparent thin film by sputtering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3259903A JPH0570942A (en) | 1991-09-11 | 1991-09-11 | High density sintered target material for forming electric conductive transparent thin film by sputtering |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0570942A true JPH0570942A (en) | 1993-03-23 |
Family
ID=17340538
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3259903A Withdrawn JPH0570942A (en) | 1991-09-11 | 1991-09-11 | High density sintered target material for forming electric conductive transparent thin film by sputtering |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0570942A (en) |
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| TWI557091B (en) * | 2011-12-07 | 2016-11-11 | 東曹股份有限公司 | Composite oxide sintered object and oxide transparent conductive film |
| CN103987678A (en) * | 2011-12-07 | 2014-08-13 | 东曹株式会社 | Complex oxide sintered body, sputtering target, transparent conductive oxide film, and method for producing same |
| WO2013084795A1 (en) * | 2011-12-07 | 2013-06-13 | 東ソー株式会社 | Complex oxide sintered body, sputtering target, transparent conductive oxide film, and method for producing same |
| WO2015136949A1 (en) * | 2014-03-11 | 2015-09-17 | 東ソー株式会社 | Sintered oxide and transparent conductive oxide film |
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