JP3591610B2 - ITO sintered body for forming transparent conductive film - Google Patents
ITO sintered body for forming transparent conductive film Download PDFInfo
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- JP3591610B2 JP3591610B2 JP27199395A JP27199395A JP3591610B2 JP 3591610 B2 JP3591610 B2 JP 3591610B2 JP 27199395 A JP27199395 A JP 27199395A JP 27199395 A JP27199395 A JP 27199395A JP 3591610 B2 JP3591610 B2 JP 3591610B2
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- 230000015572 biosynthetic process Effects 0.000 claims description 12
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 239000010408 film Substances 0.000 description 47
- 239000000843 powder Substances 0.000 description 14
- 239000000203 mixture Substances 0.000 description 13
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 8
- 239000001301 oxygen Substances 0.000 description 8
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- 238000004544 sputter deposition Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 239000011812 mixed powder Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004973 liquid crystal related substance Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000550 scanning electron microscopy energy dispersive X-ray spectroscopy Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
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Description
【０００１】
【発明の属する技術分野】
本発明は、透明導電膜形成用ＩＴＯ焼結体に関し、特に低温基板、すなわち２００℃以下から室温までの基板温度において低抵抗な透明導電膜を形成するための ＩＴＯ焼結体に関するものである。
【０００２】
【従来の技術】
近年、液晶を中心とする表示デバイスの発展に伴い、透明導電膜の需要が増加している。その透明導電膜には、低い抵抗性と高い透明性を備えているインジウム・スズ酸化物膜（以下ＩＴＯ膜と称する）が最適とされている。
ＩＴＯ膜を得る方法としては酸化インジウム粉末と酸化スズ粉末からなる混合粉末を成形、焼結することによりインジウム・スズ酸化物焼結体（以下ＩＴＯ焼結体と称する）を作製し、それをターゲットとしてＩＴＯ膜を形成する。ＩＴＯ膜の形成方法には、スパッタリング法、真空蒸着法、ＣＶＤ法等があるが、中でもスパッタリング法は、大面積を成膜することが可能でかつ低抵抗膜を再現性良く得られるとの利点から、現在、ＩＴＯ膜を形成する方法の主流になっている。スパッタリング法はターゲットを不活性ガスイオンによりスパッタリングし、３００℃程度に加熱した基板上に成膜する方法である。このようにして得られたＩ ＴＯ膜は、比抵抗が２．０×１０−４Ω・ｃｍ程度になることが知られている。
【０００３】
【発明が解決しようとする課題】
しかし、最近は液晶のカラー化、表示素子の微細化、アクティブマトリックス方式の採用、薄膜トランジスタの導入に伴い、加熱可能温度が２００℃以下のフィルム等の樹脂製基板上に低抵抗のＩＴＯ膜を形成させることが要望され、成膜に用いるターゲットも低温成膜可能なターゲットとする必要が生じてきた。
従来のターゲットの抵抗率は、成膜温度２００℃で５×１０−４Ω・ｃｍが限界であるが、目的とする液晶用電極として使用するには、成膜温度２００℃で４×１０−４Ω・ｃｍより低い抵抗率が必要とされている。
したがって、本発明は低温成膜によっても低抵抗なＩＴＯ膜が得られる透明導電膜形成用ＩＴＯ焼結体を得ることを目的とする。
【０００３】
【課題を解決するための手段】
本発明者等は前記目的を解決するため、種々検討を行った結果、ＩＴＯ焼結体として、Ｉｎ２Ｏ３を主成分とする主相と主相に比べＳｎＯ２が多い第２相からなる組織 とし、各相の組成を新規に規定することにより、低温成膜によっても低抵抗な膜が得られるターゲットとすることができることを知見した。
すなわち、本発明の透明導電膜形成用ターゲットは、実質的にＩｎ、Ｓｎ、およびＯからなるＩＴＯ焼結体であり、主相とｍｏｌ比でＩｎ：Ｓｎ＝１．６：１〜３．０：１ からなる第２相とを有することを特徴とする透明導電膜形成用ＩＴＯ焼結体である。ただし、主相、第２相以外の相、例えば第３相としてＩｎ：Ｓｎ＝１．６：１よ りもＳｎが多い相も、面積比にて第２相より少なければ一部含んでも良い。
本発明において、主相はｍｏｌ比でＩｎ：Ｓｎ＝１０：１〜８６：１とするのが望ましく 、Ｉｎ：Ｓｎ＝１０：１〜２２：１とするのがさらに望ましい。また、主相の格子定数は１．０１２１ｎｍ以上とするのが望ましく、１．０１２１〜１．０１４０とするのがさらに望ましい。さらに、主相と第２相との面積比は主相：第２相＝９９．９：０．１〜７５：２５ であることが望ましく、さらには第２相／第３相＞１であることが望ましい。
【０００４】
本発明透明導電膜形成用ＩＴＯ焼結体において、第２相の組成をｍｏｌ比でＩｎ：Ｓｎ＝１．６：１〜３．０：１としたのは、低温成膜によっても低抵抗な透明導電膜を得るためである。第２相の組成がＩｎ／Ｓｎ＜１．６になるとＳｎ量が過剰となり 低抵抗な膜が得られない。また、第２相の組成がＩｎ／Ｓｎ＞３．０の場合はＳｎ 量が不足し、ＩＴＯ膜中に酸素欠陥が生じないために充分な低抵抗性が発現しない。なお、主相、第２相以外の第３相（例えば、Ｉｎ／Ｓｎ＜１．６である相）が 焼結体中に存在したとしても、第２相より少なければ膜特性に与える影響は少なく、許容される。
【０００５】
また、本発明において、主相はｍｏｌ比でＩｎ：Ｓｎ＝１０：１〜８６：１とするのが望ましく、Ｉｎ：Ｓｎ＝１０：１〜２２：１とするのが特に望ましい。主相の組成がＩｎ／Ｓｎ＜１０になるとＳｎ量が過剰となり低抵抗な膜が得られにくく、主相の組成がＩｎ／Ｓｎ＞２２の場合はＳｎ量が不足し、ＩＴＯ膜中に酸素欠陥が生じないために充分な低抵抗性が発現しにくい。
さらに、本発明において、主相の格子定数が１．０１２１ｎｍ未満であると酸素欠陥が生じにくく充分な低抵抗性が発現しにくいので１．０１２１ｎｍ以上であることが望ましく、１．０１２１〜１．０１４０ｎｍとするのがさらに望ましい。
【０００６】
また、主相と第２相との面積比は、主相：第２相＝９９．９：０．１〜７５：２５であるこ とが望ましく、（主相／第２相）＞（９９．９／０．１）の場合はＳｎ量が不足し、（ 主相／第２相）＜（７５／２５）場合はＳｎ量が過剰となり、低温成膜において低抵抗な膜が得られにくい。
本発明において、各相の組成はＳＥＭ−ＥＤＸ分析（Ｓｃａｎｎｉｎｇ ｅｌｅｃｔｒｏｎ ｍｉｃｒｏｓｃｏｐｙ−Ｅｎｅｒｇｙ ｄｉｓｐｅｒｓｉｖｅ Ｘｒａｙ ｓｐｅｃｔｒｏｍｅｔｅｒ）によってＩｎとＳｎの組成分析を行うことにより、また、相の面積比はＳＥＭ組織写真の、ライトグレーを主相とし 、ダークグレーを第２相とし面積比を求めることにより確認することができる。主相の格子定数はＸ線回折装置（例えば、リガク ＲＩＮＴ１０００）により確認することが できる。
【０００７】
本発明のターゲットを作製するに際しては、例えば、Ｉｎ２Ｏ３粉末とＳｎＯ２粉末と を所定の割合で均一に混合し、混合粉末やあるいは固溶体粉末あるいは共沈粉末等の複合粉末を用いてもよい。また、複合粉末を主成分とし、Ｉｎ２Ｏ３粉末およびＳｎＯ２粉末の一種または二種を混合した混合粉末を用いることもできる。
前記の混合粉末を一軸加圧あるいは静水圧プレス等にて成形し、得られた成形体を酸素濃度が２５ｖｏｌ％以上の雰囲気で１３００℃〜１７００℃の温度で加熱保持する。
【０００８】
本発明において、焼結雰囲気を酸素雰囲気中とするのは Ｉｎ２Ｏ３やＳｎＯ２の分解を抑えるために必要だからであるが、酸素濃度は２５％以上、より好ましくは５０％以上が望ましい。加圧酸素雰囲気中であれば更に望ましい。焼結温度は、１３００℃未満では相対密度８５％以上の焼結体が得られず、一方１７００℃を越えると酸化スズ、酸化インジウムの分解により密度低下が生ずるので１２００〜１７００℃とするのが望ましい。また、ＩＴＯ焼結体を、主相とＩｎ：Ｓｎ＝１．６：１〜３．０：１からなる第２相とを有する焼結体とするために、１０００℃以上での昇温速度を０．５℃／ｍｉｎ以上に、さらに冷却時の降温速度を０．５℃／ｍｉｎ以上にするのが好ましい。昇温速度を０．５℃／ｍｉｎより小さくするとＳｎの分解により相対密度８５％以上の焼結体が得られにくい。降温速度を０．５℃／ｍｉｎより小さくするとＩｎ／Ｓｎ＜１．６になり易 くなる。
【０００９】
【発明の実施の形態】
（実施例１）
平均粒径５０ｎｍのＩｎ２Ｏ３粉末と、平均粒径１５０ｎｍのＳｎＯ２粉末とを、所定の比率になるように配合しボールミルによって２４時間混合した。
成形は、これらの粉末にポリビニルアルコール（ＰＶＡ）を１％添加して造粒 し、これを冷間静水圧プレスで成形圧力３０００ｋｇ／ｃｍ２で成形した。この成形体を１５５０℃、１気圧、７０％の酸素雰囲気中で５時間保持し焼結した。試料Ｎｏ．１〜１３、１８〜２０については、１０００℃以上での昇温速度２℃／ｍｉｎ、冷却時の降温速度２℃／ｍｉｎの焼結条件で焼結を行った。Ｎｏ．１４〜１７、２１については、冷却時の降温速度０．２℃／ｍｉｎの条件で焼結を行った。
得られた焼結体の各相の組成と面積比、格子定数を測定し表１、２に示す。さらに得られた焼結体を研削により直径１００ｍｍ、厚さ５ｍｍの形状に加工したターゲットを用いて成膜した時の成膜温度２００℃でのＩＴＯ膜の抵抗率を表１，２に示す 。なお、Ｎｏ．１〜１３，１８〜２０は本発明であり、Ｎｏ．１４〜１７，２１は比較例である。
表１のＮｏ．１、Ｎｏ．８、Ｎｏ．１５のＩＴＯ焼結体のミクロ組織を鏡面加工後のＳＥＭに て観察したＳＥＭ組織写真を図１、図２、図３に示す。
また、表１、２のＮｏ．１、８、１１、１４、１５の試料について、成膜時の基板温度を変化 させた場合のＩＴＯ膜の抵抗率（μΩ・ｃｍ）を表３に示す。
なお、成膜条件は次の通りである。
スパッタ方式 ＤＣマグネトロンスパッタリング
ターゲット−基板間距離 ６０ｍｍ
スパッタ電力 １．０Ｗ／ｃｍ２
スパッタガス組成 ９９％アルゴン＋１％酸素の混合ガス
スパッタガス圧 １Ｐａ
膜厚 １５０ｎｍ
基板 コーニング＃７０５９ガラス
【００１０】
表１より、第２相の組成をｍｏｌ比でＩｎ：Ｓｎ＝１．６：１〜３．０：１とすることにより、低温成膜によっても低抵抗な透明導電膜が得られること、また主相の組成がｍｏｌ比でＩｎ：Ｓｎ＝１０：１〜２２：１の場合特に低抵抗なＩＴＯ膜が得られることがわかる。
また、表２より、第３相の面積比が第２相より大きくなると、第２相による低抵抗の効果は発現しないことがわかる。なお、Ｎｏ．１８〜２１の試料に含有された第 ３相は、Ｉｎ：Ｓｎ＝１．５：１の相であった。
さらに、表３に示すように、本発明のターゲットの試料Ｎｏ．１ないし試料Ｎｏ．８，１１は比較例のＮｏ．１４に較べ、特に、２００℃以下の低温成膜において低い抵抗値を示 した。
【００１１】
【表１】
【表２】
【表３】
本発明透明導電膜形成用ＩＴＯ焼結体をターゲットとすれば、低温でのスパッタリングによっても低い抵抗値のＩＴＯ膜が得ることが可能である。
【図面の簡単な説明】
【図１】本発明ＩＴＯ焼結体である試料Ｎｏ．１のミクロ金属組織写真である。
【図２】本発明ＩＴＯ焼結体である試料Ｎｏ．８のミクロ金属組織写真である。
【図３】比較例ＩＴＯ焼結体である試料Ｎｏ．１５のミクロ金属組織写真である。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to an ITO sintered body for forming a transparent conductive film, and more particularly to an ITO sintered body for forming a low-resistance transparent conductive film at a low-temperature substrate, that is, at a substrate temperature from 200 ° C. or lower to room temperature.
[0002]
[Prior art]
In recent years, with the development of display devices centering on liquid crystals, the demand for transparent conductive films has been increasing. As the transparent conductive film, an indium tin oxide film (hereinafter, referred to as an ITO film) having low resistance and high transparency is optimized.
As a method for obtaining an ITO film, a mixed powder comprising an indium oxide powder and a tin oxide powder is molded and sintered to produce an indium tin oxide sintered body (hereinafter referred to as an ITO sintered body), which is then used as a target. To form an ITO film. Methods of forming the ITO film include a sputtering method, a vacuum evaporation method, and a CVD method. Among them, the sputtering method has an advantage that a large-area film can be formed and a low-resistance film can be obtained with good reproducibility. Therefore, the method of forming an ITO film is currently the mainstream. The sputtering method is a method in which a target is sputtered with inert gas ions to form a film on a substrate heated to about 300 ° C. It is known that the ITO film thus obtained has a specific resistance of about 2.0 × 10 −4 Ω · cm.
[0003]
[Problems to be solved by the invention]
However, recently, with the development of color liquid crystal, miniaturization of display elements, adoption of active matrix method, and introduction of thin film transistors, low-resistance ITO film is formed on a resin substrate such as a film whose heating temperature is 200 ° C or less. Therefore, it has become necessary to use a target capable of forming a film at a low temperature.
The limit of the resistivity of the conventional target is 5 × 10 −4 Ω · cm at a film formation temperature of 200 ° C., but 4 × 10 −4 Ω at a film formation temperature of 200 ° C. to be used as a target liquid crystal electrode. -Resistivity lower than cm is required.
Therefore, an object of the present invention is to obtain an ITO sintered body for forming a transparent conductive film, which can obtain a low-resistance ITO film even by low-temperature film formation.
[0003]
[Means for Solving the Problems]
The present inventors have conducted various studies in order to solve the above-mentioned object. As a result, the ITO sintered body has a main phase mainly composed of In2O3 and a second phase having more SnO2 than the main phase. It has been found that by newly defining the phase composition, it is possible to obtain a target capable of obtaining a low-resistance film even by low-temperature film formation.
That is, the transparent conductive film forming target of the present invention is an ITO sintered body substantially composed of In, Sn, and O, and has a molar ratio of In: Sn = 1.6: 1 to 3.0 to the main phase. 1: a second phase comprising: a sintered body for forming a transparent conductive film; However, a phase other than the main phase and the second phase, for example, a phase having more Sn than In: Sn = 1.6: 1 as the third phase may partially include the phase if the area ratio is smaller than the second phase. .
In the present invention, the molar ratio of the main phase is preferably In: Sn = 10: 1 to 86: 1, and more preferably In: Sn = 10: 1 to 22: 1. The lattice constant of the main phase is desirably 1.0121 nm or more, and more desirably 1.0121 to 1.0140. Further, the area ratio between the main phase and the second phase is desirably main phase: second phase = 99.9: 0.1 to 75:25, and more preferably, second phase / third phase> 1. It is desirable.
[0004]
In the ITO sintered body for forming a transparent conductive film of the present invention, the composition of the second phase is set to be In: Sn = 1.6: 1 to 3.0: 1 by mol ratio because of low resistance even by low-temperature film formation. This is for obtaining a transparent conductive film. If the composition of the second phase becomes In / Sn <1.6, the amount of Sn becomes excessive and a low-resistance film cannot be obtained. Further, when the composition of the second phase is In / Sn> 3.0, the Sn content is insufficient, and oxygen deficiency does not occur in the ITO film, so that sufficient low resistance is not exhibited. Even if a third phase other than the main phase and the second phase (for example, a phase satisfying In / Sn <1.6) is present in the sintered body, the influence on the film properties is not so large as being smaller than the second phase. Less and acceptable.
[0005]
In the present invention, the main phase preferably has a molar ratio of In: Sn = 10: 1 to 86: 1, particularly preferably In: Sn = 10: 1 to 22: 1. When the composition of the main phase is In / Sn <10, the amount of Sn becomes excessive and it is difficult to obtain a low-resistance film. When the composition of the main phase is In / Sn> 22, the amount of Sn becomes insufficient, and oxygen is contained in the ITO film. Sufficient low resistance is hardly developed because no defect occurs.
Furthermore, in the present invention, if the lattice constant of the main phase is less than 1.0121 nm, oxygen vacancies hardly occur and sufficient low resistance is hardly exhibited, so that the lattice constant is desirably 1.0121 nm or more. More preferably, it is set to 0140 nm.
[0006]
The area ratio between the main phase and the second phase is preferably main phase: second phase = 99.9: 0.1 to 75:25, and (main phase / second phase)> (99. In the case of (9 / 0.1), the amount of Sn is insufficient, and in the case of (main phase / second phase) <(75/25), the amount of Sn becomes excessive, and it is difficult to obtain a low-resistance film in low-temperature film formation.
In the present invention, the composition of each phase is determined by performing a composition analysis of In and Sn by SEM-EDX analysis (Scanning electron microscopy-Energy dispersive Xray spectrometer). It can be confirmed by determining the area ratio by using dark gray as the second phase as the main phase. The lattice constant of the main phase can be confirmed by an X-ray diffractometer (for example, Rigaku RINT1000).
[0007]
In producing the target of the present invention, for example, In2O3 powder and SnO2 powder may be uniformly mixed at a predetermined ratio, and a mixed powder or a composite powder such as a solid solution powder or a coprecipitated powder may be used. Alternatively, a mixed powder containing a composite powder as a main component and a mixture of one or two of In2O3 powder and SnO2 powder can be used.
The mixed powder is molded by a uniaxial press or hydrostatic press or the like, and the obtained molded body is heated and held at a temperature of 1300 ° C. to 1700 ° C. in an atmosphere having an oxygen concentration of 25 vol% or more.
[0008]
In the present invention, the sintering atmosphere is set to an oxygen atmosphere because it is necessary to suppress the decomposition of In2O3 and SnO2, and the oxygen concentration is preferably 25% or more, more preferably 50% or more. It is more desirable to be in a pressurized oxygen atmosphere. When the sintering temperature is lower than 1300 ° C., a sintered body having a relative density of 85% or more cannot be obtained. On the other hand, when the sintering temperature exceeds 1700 ° C., the density decreases due to decomposition of tin oxide and indium oxide. desirable. Further, in order to make the ITO sintered body a sintered body having a main phase and a second phase composed of In: Sn = 1.6: 1 to 3.0: 1, the temperature rising rate at 1000 ° C. or higher is used. Is preferably 0.5 ° C./min or more, and the cooling rate during cooling is 0.5 ° C./min or more. If the heating rate is lower than 0.5 ° C./min, it is difficult to obtain a sintered body having a relative density of 85% or more due to decomposition of Sn. If the cooling rate is lower than 0.5 ° C./min, In / Sn <1.6 tends to be satisfied.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
(Example 1)
In2O3 powder having an average particle diameter of 50 nm and SnO2 powder having an average particle diameter of 150 nm were blended so as to have a predetermined ratio, and mixed by a ball mill for 24 hours.
Molding was performed by adding 1% of polyvinyl alcohol (PVA) to these powders, granulating the powders, and pressing them with a cold isostatic press at a molding pressure of 3000 kg / cm 2. The compact was sintered at 1550 ° C., 1 atm and 70% oxygen atmosphere for 5 hours. Sample No. About 1-13 and 18-20, sintering was carried out under the sintering conditions of a heating rate of 2 ° C./min above 1000 ° C. and a cooling rate of 2 ° C./min during cooling. No. About 14-17 and 21, sintering was performed on the conditions of 0.2 degree-C / min of the temperature fall rate at the time of cooling.
The composition, area ratio, and lattice constant of each phase of the obtained sintered body were measured, and the results are shown in Tables 1 and 2. Further, Tables 1 and 2 show the resistivity of the ITO film at a film formation temperature of 200 ° C. when the obtained sintered body was formed using a target processed into a shape having a diameter of 100 mm and a thickness of 5 mm by grinding. In addition, No. Nos. 1 to 13 and 18 to 20 are the present invention. 14 to 17, 21 are comparative examples.
No. 1 in Table 1. 1, No. 8, No. FIGS. 1, 2 and 3 show SEM micrographs of the microstructures of the 15 ITO sintered bodies observed by SEM after mirror finishing.
Also, in Tables 1 and 2, Table 3 shows the resistivity (μΩ · cm) of the ITO films of the samples 1, 8, 11, 14, and 15 when the substrate temperature during film formation was changed.
The film forming conditions are as follows.
Sputtering method DC magnetron sputtering target-substrate distance 60mm
Sputtering power 1.0W / cm2
Sputter gas composition 99% argon + 1% oxygen mixed gas Sputter gas pressure 1Pa
150nm thickness
Substrate Corning # 7059 glass [0010]
From Table 1, it can be seen that by setting the composition of the second phase to In: Sn = 1.6: 1 to 3.0: 1 in a molar ratio, a transparent conductive film having low resistance can be obtained even by low-temperature film formation. It can be seen that a particularly low-resistance ITO film can be obtained when the composition of the main phase is In: Sn = 10: 1 to 22: 1 in molar ratio.
Also, from Table 2, it can be seen that when the area ratio of the third phase is larger than that of the second phase, the effect of low resistance by the second phase is not exhibited. In addition, No. The third phase contained in the samples 18 to 21 was a phase of In: Sn = 1.5: 1.
Further, as shown in Table 3, the sample No. of the target of the present invention was used. 1 to Sample No. Nos. 8 and 11 are Nos. Of Comparative Examples. As compared with No. 14, the resistance was particularly low in film formation at a low temperature of 200 ° C. or lower.
[0011]
[Table 1]
[Table 2]
[Table 3]
By using the ITO sintered body for forming a transparent conductive film of the present invention as a target, an ITO film having a low resistance value can be obtained even by sputtering at a low temperature.
[Brief description of the drawings]
FIG. 1 shows a sample No. which is an ITO sintered body of the present invention. 1 is a photograph of a micro metal structure.
FIG. 2 shows a sample No. which is an ITO sintered body of the present invention. 8 is a micro metallographic photograph of FIG.
FIG. 3 shows a sample No. which is a comparative example ITO sintered body. It is a micro metal structure photograph of No. 15.
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27199395A JP3591610B2 (en) | 1994-11-10 | 1995-09-26 | ITO sintered body for forming transparent conductive film |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6-301459 | 1994-11-10 | ||
| JP30145994 | 1994-11-10 | ||
| JP27199395A JP3591610B2 (en) | 1994-11-10 | 1995-09-26 | ITO sintered body for forming transparent conductive film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08188871A JPH08188871A (en) | 1996-07-23 |
| JP3591610B2 true JP3591610B2 (en) | 2004-11-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| JP27199395A Expired - Fee Related JP3591610B2 (en) | 1994-11-10 | 1995-09-26 | ITO sintered body for forming transparent conductive film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003264307A (en) * | 2002-03-11 | 2003-09-19 | Sharp Corp | Thin film solar cell and its manufacturing method |
| US20100127611A1 (en) * | 2007-05-22 | 2010-05-27 | Masaaki Imura | Transparent electrode |
| WO2016174877A1 (en) * | 2015-04-30 | 2016-11-03 | 三井金属鉱業株式会社 | Ito sputtering target material |
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