JP2000040429A - Manufacturing of zinc oxide transparent conductive film - Google Patents
Manufacturing of zinc oxide transparent conductive filmInfo
- Publication number
- JP2000040429A JP2000040429A JP20874398A JP20874398A JP2000040429A JP 2000040429 A JP2000040429 A JP 2000040429A JP 20874398 A JP20874398 A JP 20874398A JP 20874398 A JP20874398 A JP 20874398A JP 2000040429 A JP2000040429 A JP 2000040429A
- Authority
- JP
- Japan
- Prior art keywords
- zinc oxide
- target
- transparent conductive
- conductive film
- substrate
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、スパッタリング法
による酸化亜鉛系透明導電膜の製造方法の改良に関す
る。The present invention relates to an improvement in a method for producing a zinc oxide-based transparent conductive film by a sputtering method.
【０００２】[0002]
【従来の技術】透明導電膜は可視光領域で高い透過率と
高い導電性を有し、液晶表示素子や太陽電池、その他各
種受光素子の電極として、また、自動車および建築用の
熱線反射膜、帯電防止膜、冷凍ショーケースなどの各種
の防曇用の透明発熱体として広範に利用されている。2. Description of the Related Art A transparent conductive film has a high transmittance and a high conductivity in a visible light region, and is used as an electrode of a liquid crystal display element, a solar cell, other various light receiving elements, a heat ray reflective film for automobiles and buildings, It is widely used as a transparent heating element for various antifogging applications such as antistatic films and frozen showcases.
【０００３】従来、透明導電膜としては、ガラス基板上
に堆積させたアンチモンやフッ素をドーパントとして含
む酸化錫（ＳｎＯ2）や、錫をドーパントとして含む酸
化インジウム（Ｉｎ2Ｏ3）などが知られている。特に錫
をドーパントとして含む酸化インジウム膜はＩＴＯ膜と
称され、低抵抗膜が容易に得られることからよく用いら
れている。Conventionally, as a transparent conductive film, tin oxide (SnO 2 ) containing antimony or fluorine as a dopant deposited on a glass substrate, indium oxide (In 2 O 3 ) containing tin as a dopant, and the like are known. ing. In particular, an indium oxide film containing tin as a dopant is called an ITO film, and is often used because a low-resistance film can be easily obtained.
【０００４】しかし、ＩＴＯは、原料が希少金属である
インジウムであるため高価であり、この膜を用いたとき
低コスト化には限界がある。またインジウムの資源埋蔵
量は少なく、亜鉛鉱等の副産物として得られるため、大
幅な生産量の増大や安定供給は困難である。However, ITO is expensive because the raw material is indium, which is a rare metal, and there is a limit to the cost reduction when this film is used. In addition, since indium reserves are small and can be obtained as a by-product such as zinc ore, it is difficult to greatly increase the production amount and supply it stably.
【０００５】一方、酸化亜鉛（ＺｎＯ）を主成分とする
酸化亜鉛系透明導電膜は、主原料である亜鉛が極めて低
価格であり、かつ埋蔵量、生産量ともに極めて多く、資
源枯渇や安定供給の点で心配がない。酸化亜鉛系透明導
電膜は、現在主に太陽電池用透明導電膜として利用され
ており、その製造方法にはスパッタリング法が用いられ
ている。On the other hand, a zinc oxide-based transparent conductive film containing zinc oxide (ZnO) as a main component has an extremely low price of zinc as a main raw material, has a very large reserve and production amount, and is depleted of resources and stable supply. Don't worry about it. BACKGROUND ART Zinc oxide-based transparent conductive films are currently mainly used as transparent conductive films for solar cells, and a sputtering method is used as a manufacturing method thereof.
【０００６】スパッタリング法は、蒸気圧の低い材料の
成膜や精密な膜厚制御を必要とする際に有効な手法であ
り、操作が非常に簡便であるため工業的に広範に利用さ
れている。[0006] The sputtering method is an effective technique when film formation of a material having a low vapor pressure or precise control of the film thickness is required. Since the operation is very simple, it is widely used industrially. .
【０００７】スパッタリング法は、一般に、約１０Ｐａ
以下のガス圧のもとで、陽極となる基板と陰極となるタ
ーゲットの間にグロー放電を起こしてアルゴンプラズマ
を発生させ、プラズマ中のアルゴン陽イオンを陰極のタ
ーゲットに衝突させ、これによってはじきとばされるタ
ーゲット成分の粒子を基板上に堆積させて膜を形成する
方法である。アルゴンプラズマの発生させる方法として
は、高周波プラズマを用いる高周波スパッタリング法と
直流プラズマを用いる直流スパッタリング法がある。[0007] Sputtering is generally performed at about 10 Pa
Under the following gas pressure, a glow discharge is generated between the substrate serving as the anode and the target serving as the cathode to generate argon plasma, and argon cations in the plasma collide with the cathode target. In this method, particles of a target component to be deposited are deposited on a substrate to form a film. As a method for generating argon plasma, there are a high-frequency sputtering method using high-frequency plasma and a direct-current sputtering method using direct-current plasma.
【０００８】スパッタリング法で酸化亜鉛系透明導電膜
を作製する場合、ＩＴＯの透明導電膜と比較して、低抵
抗の膜を安定に製造することが難しく、工業化には障害
となっていた。When a zinc oxide-based transparent conductive film is produced by a sputtering method, it is difficult to stably produce a low-resistance film as compared with an ITO transparent conductive film, which has been an obstacle to industrialization.
【０００９】[0009]
【発明が解決しようとする課題】本発明は上記の問題点
を克服するために提案されたもので、安定に低抵抗の酸
化亜鉛系透明導電膜を、スパッタリング法で製造する方
法を提供することを目的とする。SUMMARY OF THE INVENTION The present invention has been proposed to overcome the above problems, and provides a method for stably producing a low-resistance transparent conductive film of zinc oxide by sputtering. With the goal.
【００１０】[0010]
【課題を解決するための手段】上記の目的を達成するた
めに本発明による酸化亜鉛透明導電膜の製造方法は、以
下のようにしたものである。Means for Solving the Problems To achieve the above object, a method for producing a zinc oxide transparent conductive film according to the present invention is as follows.
【００１１】即ち、本発明の酸化亜鉛透明導電膜の製造
方法は、チャンバー内に設けたカソードに酸化亜鉛系材
料からなるターゲットを取り付け、ターゲットに対向し
て基板を取り付け、チャンバー内に希薄なＡｒガスを導
入し、該ターゲットを陰極とし、基板を陽極としてター
ゲットと基板間にグロー放電を起こし、Ａｒ陽イオンが
ターゲットに衝突することによって供給される酸化亜鉛
系材料の粒子を基板上に堆積させて基板上に酸化亜鉛系
透明導電膜を形成させる、スパッタリング法による酸化
亜鉛系透明導電膜の製造方法において、前記直流プラズ
マを発生させる前に予めチャンバー内の到達真空度を５
×１０-5Ｐａ以下の高真空にすることを特徴とする。That is, according to the method for producing a zinc oxide transparent conductive film of the present invention, a target made of a zinc oxide-based material is attached to a cathode provided in a chamber, a substrate is attached to face the target, and a dilute Ar gas is placed in the chamber. A gas is introduced, a glow discharge is caused between the target and the substrate using the target as a cathode and the substrate as an anode, and particles of the zinc oxide-based material supplied by the Ar cations colliding with the target are deposited on the substrate. Forming a zinc oxide-based transparent conductive film on a substrate by sputtering, in the method for producing a zinc oxide-based transparent conductive film by a sputtering method.
It is characterized by a high vacuum of × 10 -5 Pa or less.
【００１２】前記酸化亜鉛系材料のターゲットには、酸
化亜鉛を主成分とし、さらに、Ａｌ、Ｇａ、Ｉｎ、Ｂ、
Ｙ、Ｓｉ、Ｚｒ、Ｔｉのうちの少なくとも１種類が添加
されているものを用いることができる。The target of the zinc oxide-based material contains zinc oxide as a main component, and further contains Al, Ga, In, B,
A material to which at least one of Y, Si, Zr, and Ti is added can be used.
【００１３】上記のスパッタリング法には、直流マグネ
トロンスパッタリング法、即ち、プラズマ中に磁界をか
けて低ガス圧においても安定なプラズマを発生させてス
パッタリング効率を高めたスパッタリング法も含まれ
る。The above-mentioned sputtering method includes a direct current magnetron sputtering method, that is, a sputtering method in which a magnetic field is applied to the plasma to generate a stable plasma even at a low gas pressure to increase the sputtering efficiency.
【００１４】[0014]
【発明の実施の形態】ガス圧、成膜ガスの種類、ターゲ
ット基板間距離、成膜パワーを一定にして、到達真空度
を変化させた発明者の実験によると、膜の比抵抗は到達
真空度に大きく依存する。この比抵抗は到達真空度が悪
いほど高く、特に到達真空度が５．０×１０-5Ｐａ以上
の高真空では顕著である。この原因は次のように説明で
きる。到達真空度が悪い状態でスパッタ成膜を行うと、
残留ガス中の酸素量が多いため、膜中に取り込まれる酸
素量が多くなり、膜の比抵抗を悪化させてしまうのであ
る。比抵抗を悪化させない到達真空度の最高値は、発明
者の実験によると、５．０×１０-5Ｐａであった。DESCRIPTION OF THE PREFERRED EMBODIMENTS According to an experiment conducted by the inventor in which the ultimate vacuum degree was changed while keeping the gas pressure, the kind of the deposition gas, the distance between target substrates and the deposition power constant, the specific resistance of the film was found to be the ultimate vacuum. Depends greatly on the degree. This specific resistance is higher as the ultimate vacuum degree is worse, and is particularly remarkable in a high vacuum where the ultimate vacuum degree is 5.0 × 10 −5 Pa or more. The cause can be explained as follows. When performing sputter film formation in a state where the ultimate vacuum degree is poor,
Since the amount of oxygen in the residual gas is large, the amount of oxygen taken into the film increases, and the specific resistance of the film deteriorates. According to an experiment performed by the inventor, the highest value of the ultimate vacuum degree that does not deteriorate the specific resistance was 5.0 × 10 −5 Pa.
【００１５】従って、本発明で提案した到達真空度、即
ち５．０×１０-5Ｐａ以下においてスパッタリング成膜
を実施すれば、比抵抗の低い酸化亜鉛系透明導電膜が安
定に製造できる。Therefore, if the sputtering film formation is performed at the ultimate vacuum degree proposed in the present invention, that is, 5.0 × 10 −5 Pa or less, a zinc oxide-based transparent conductive film having a low specific resistance can be stably manufactured.
【００１６】[0016]
【実施例】以下、本発明の実施例を示し、本発明をより
具体的に説明する。大きさが６インチφ×５ｍｍｔのＺ
ｎＯ焼結体のターゲットを直流マグネトロンスパッタリ
ング装置の非磁性体ターゲット用カソードにとりつけ
た。ターゲットと基板の間の距離は７０ｍｍとし、純度
９９．９９９９％のＡｒガスを導入し０．５Ｐａのガス
圧にしてＤＣ２００Ｗでスパッタリングを実施した。The present invention will be described more specifically with reference to the following examples. Z of size 6 inches φ x 5mmt
The target of the nO sintered body was attached to a cathode for a nonmagnetic target of a DC magnetron sputtering apparatus. The distance between the target and the substrate was 70 mm, Ar gas having a purity of 99.9999% was introduced, the gas pressure was set to 0.5 Pa, and sputtering was performed at 200 W DC.
【００１７】本発明に従った条件を含む種々の条件にお
いて直流プラズマを発生させてスパッタリングを開始
し、膜厚５００ｎｍの膜を製造し比抵抗を四端針法で測
定した。５ａｔ％Ｇａ添加ＺｎＯ焼結体ターゲットを使
用してスパッタリングした場合の膜の比抵抗と到達真空
度との関係についての実験結果を表１に示す。Under various conditions including the conditions according to the present invention, DC plasma was generated to start sputtering, a film having a thickness of 500 nm was manufactured, and the specific resistance was measured by a four-point probe method. Table 1 shows the experimental results on the relationship between the specific resistance of the film and the ultimate vacuum when sputtering is performed using a 5 at% Ga-added ZnO sintered body target.
【００１８】[0018]
【表１】 ―――――――――――――――――――――――――― 到達真空度(Pa) 膜の比抵抗(Ωcm) 備 考 ―――――――――――――――――――――――――― 2.0×10-5 6.1×10-4 実施例１ 4.0×10-5 6.1×10-4 実施例２ 5.0×10-5 6.2×10-4 実施例３ 6.0×10-5 6.9×10-4 比較例１ 8.0×10-5 7.2×10-4 比較例２ 1.0×10-4 7.5×10-4 比較例３ 2.0×10-4 1.0×10-3 比較例４ 4.0×10-4 1.3×10-3 比較例５ 6.0×10-4 1.7×10-3 比較例６ 1.0×10-3 2.4×10-3 比較例７ ――――――――――――――――――――――――――[Table 1] ―――――――――――――――――――――――― Ultimate vacuum (Pa) Specific resistance of film (Ωcm) Remarks ――――――――――――――――――――― 2.0 × 10 -5 6.1 × 10 -4 Example 1 4.0 × 10 -5 6.1 × 10 -4 Example 2 5.0 × 10 -5 6.2 × 10 -4 Example 3 6.0 × 10 -5 6.9 × 10 -4 Comparative Example 1 8.0 × 10 -5 7.2 × 10 -4 Comparative Example 2 1.0 × 10 -4 7.5 × 10 -4 Comparative Example 3 2.0 × 10 -4 1.0 × 10 -3 Comparative Example 4 4.0 × 10 -4 1.3 × 10 -3 Comparative Example 5 6.0 × 10 -4 1.7 × 10 -3 Comparative Example 6 1.0 × 10 -3 2.4 × 10 -3 Comparative Example 7 ――――――――――――――――――――――――――
【００１９】同様に３ａｔ％のＡｌを添加したＺｎＯ焼
結体ターゲットを用いた場合の膜の比抵抗と到達真空度
との関係についての実験結果を表２に示す。Similarly, Table 2 shows the experimental results on the relationship between the specific resistance of the film and the ultimate vacuum when a ZnO sintered target to which 3 at% of Al was added was used.
【００２０】[0020]
【表２】 ―――――――――――――――――――――――――― 到達真空度(Pa) 膜の比抵抗(Ωcm) 備 考 ―――――――――――――――――――――――――― 2.0×10-5 6.3×10-4 実施例４ 4.0×10-5 6.4×10-4 実施例５ 5.0×10-5 6.4×10-4 実施例６ 6.0×10-5 7.1×10-4 比較例８ 8.0×10-5 7.5×10-4 比較例９ 1.0×10-4 7.7×10-4 比較例１０ 2.0×10-4 1.2×10-3 比較例１１ 4.0×10-4 1.8×10-3 比較例１２ 6.0×10-4 2.0×10-3 比較例１３ 1.0×10-3 3.1×10-3 比較例１４ ――――――――――――――――――――――――――[Table 2] ―――――――――――――――――――――――― Ultimate vacuum (Pa) Film specific resistance (Ωcm) Remarks ――――― ――――――――――――――――――――― 2.0 × 10 -5 6.3 × 10 -4 Example 4 4.0 × 10 -5 6.4 × 10 -4 Example 5 5.0 × 10 -5 6.4 × 10 -4 Example 6 6.0 × 10 -5 7.1 × 10 -4 Comparative Example 8 8.0 × 10 -5 7.5 × 10 -4 Comparative Example 9 1.0 × 10 -4 7.7 × 10 -4 Comparative Example 10 2.0 × 10 -4 1.2 × 10 -3 Comparative Example 11 4.0 × 10 -4 1.8 × 10 -3 Comparative Example 12 6.0 × 10 -4 2.0 × 10 -3 Comparative Example 13 1.0 × 10 -3 3.1 × 10 -3 Comparative Example 14 ――――――――――――――――――――――――――
【００２１】次に、５ａｔ％のＢを添加したＺｎＯ焼結
体ターゲットを用いた場合の膜の比抵抗と到達真空度と
の関係についての実験結果を表３に示す。Next, Table 3 shows experimental results on the relationship between the specific resistance of the film and the ultimate vacuum when a ZnO sintered body target containing 5 at% of B was used.
【００２２】[0022]
【表３】 ―――――――――――――――――――――――――― 到達真空度(Pa) 膜の比抵抗(Ωcm) 備 考 ―――――――――――――――――――――――――― 2.0×10-5 9.4×10-4 実施例７ 4.0×10-5 9.4×10-4 実施例８ 5.0×10-5 9.6×10-4 実施例９ 6.0×10-5 1.0×10-3 比較例１５ 8.0×10-5 2.0×10-3 比較例１６ 1.0×10-4 3.5×10-3 比較例１７ 2.0×10-4 5.0×10-3 比較例１８ 4.0×10-4 8.3×10-3 比較例１９ 6.0×10-4 1.2×10-2 比較例２０ ――――――――――――――――――――――――――[Table 3] ―――――――――――――――――――――――― Ultimate vacuum (Pa) Film specific resistance (Ωcm) Remarks ――――― ――――――――――――――――――――― 2.0 × 10 -5 9.4 × 10 -4 Example 7 4.0 × 10 -5 9.4 × 10 -4 Example 8 5.0 × 10 -5 9.6 × 10 -4 Example 9 6.0 × 10 -5 1.0 × 10 -3 Comparative Example 15 8.0 × 10 -5 2.0 × 10 -3 Comparative Example 16 1.0 × 10 -4 3.5 × 10 -3 Comparative Example 17 2.0 × 10 -4 5.0 × 10 -3 Comparative Example 18 4.0 × 10 -4 8.3 × 10 -3 Comparative Example 19 6.0 × 10 -4 1.2 × 10 -2 Comparative Example 20 ―――――――――――― ――――――――――――――
【００２３】以上の表に示すように、本発明に従った到
達真空度でスパッタ成膜を行うと、低抵抗の膜を作製す
ることができる。As shown in the above table, when a film is formed by sputtering at an ultimate degree of vacuum according to the present invention, a film having a low resistance can be produced.
【００２４】作製した膜の結晶性をＸＲＤで測定し、ま
た膜表面をＳＥＭで観察した。その結果、上記比較例に
従って作製した膜は、いずれも表面の凹凸が激しく結晶
性が悪かった。これに対し、本発明に従った実施例で作
製した膜表面はいずれも非常になめらかで良好であり、
結晶性が良好であった。The crystallinity of the prepared film was measured by XRD, and the film surface was observed by SEM. As a result, the films prepared according to the above comparative examples all had severe irregularities on the surface and were poor in crystallinity. On the other hand, the film surfaces prepared in the examples according to the present invention are all very smooth and good,
The crystallinity was good.
【００２５】[0025]
【発明の効果】本発明によれば、低抵抗の酸化亜鉛系透
明導電膜を安定に製造できる。従って、高価なＩＴＯ膜
にかわる安価な膜が電子部品に適用できるため、電子部
品のコスト低減にも結びつく。これらのことから、本発
明は工業的に極めて価値が高い。According to the present invention, a zinc oxide-based transparent conductive film having a low resistance can be stably manufactured. Therefore, an inexpensive film in place of the expensive ITO film can be applied to the electronic component, which leads to a reduction in the cost of the electronic component. For these reasons, the present invention is extremely valuable industrially.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｈ０１Ｌ 21/285 Ｈ０１Ｌ 21/285 Ｓ ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) H01L 21/285 H01L 21/285 S
Claims (2)
鉛系材料からなるターゲットを取り付け、該ターゲット
に対向して基板を取り付け、該チャンバー内に希薄なＡ
ｒガスを導入し、該ターゲットを陰極とし、該基板を陽
極として該ターゲットと該基板間にグロー放電を起こ
し、Ａｒ陽イオンが該ターゲットに衝突することによっ
て供給される酸化亜鉛系材料の粒子を該基板上に堆積さ
せて該基板上に酸化亜鉛系透明導電膜を形成させる、ス
パッタリング法による酸化亜鉛系透明導電膜の製造方法
において、前記直流プラズマを発生させる前に予めチャ
ンバー内の到達真空度を５×１０-5Ｐａ以下の高真空に
することを特徴とする酸化亜鉛透明導電膜の製造方法。1. A target made of a zinc oxide-based material is attached to a cathode provided in a chamber, and a substrate is attached to the target so as to face the target.
r gas is introduced, the target is used as a cathode, the substrate is used as an anode, a glow discharge is caused between the target and the substrate, and particles of the zinc oxide-based material supplied by the collision of Ar cations with the target are generated. Forming a zinc oxide-based transparent conductive film on the substrate by depositing the film on the substrate; forming a zinc oxide-based transparent conductive film by a sputtering method; A high vacuum of 5 × 10 −5 Pa or less.
し、さらに、Ａｌ、Ｇａ、Ｉｎ、Ｂ、Ｙ、Ｓｉ、Ｚｒ、
Ｔｉのうちの少なくとも１種類が添加されている酸化亜
鉛系材料であることを特徴とする請求項１記載の酸化亜
鉛系透明導電膜の製造方法。2. The method according to claim 1, wherein the target is mainly composed of zinc oxide, and further includes Al, Ga, In, B, Y, Si, Zr,
The method for producing a zinc oxide-based transparent conductive film according to claim 1, wherein the zinc oxide-based material is a zinc oxide-based material to which at least one of Ti is added.
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