JP4432206B2 - Method for forming laminated film - Google Patents
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- JP4432206B2 JP4432206B2 JP2000146892A JP2000146892A JP4432206B2 JP 4432206 B2 JP4432206 B2 JP 4432206B2 JP 2000146892 A JP2000146892 A JP 2000146892A JP 2000146892 A JP2000146892 A JP 2000146892A JP 4432206 B2 JP4432206 B2 JP 4432206B2
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Description
【０００１】
【発明の属する技術分野】
本発明は、基板上に金属酸化物薄膜と金属薄膜とが交互に多層に積層された積層膜に係り、特に、プラズマディスプレイパネル（ＰＤＰ）の前面に配置される透明導電性薄膜や熱線反射膜として有用な低抵抗で導電性に優れた積層膜をスパッタリング法により形成する方法に関する。
【０００２】
【従来の技術】
ＰＤＰの前面板には、反射防止性能（即ち、可視光高透過性（可視光低反射性））、熱線反射（近赤外カット）性能、電磁波シールド性能等に優れることが要求され、従来、このような要求性能のうち、熱線反射性と電磁波シールド性とを兼備するものとして、ＰＥＴフィルム上にＩＴＯ（スズインジウム酸化物）等の金属酸化物薄膜とＡｇ等の金属薄膜とを交互に多層積層形成したフィルムが提供されている。
【０００３】
この積層膜の形成方法としては、スパッタリング法、イオンプレーティング法、ＣＶＤ法等、各種の方法があるが、膜厚制御が容易な点からスパッタリング法が最も好適とされている。なお、スパッタリング法による金属薄膜の形成は、アルゴン（Ａｒ）雰囲気にて行われ、金属酸化物薄膜をスパッタリング法により形成する場合には、雰囲気ガス中に酸素（Ｏ２）を導入し、Ａｒ／Ｏ２雰囲気で行われる。
【０００４】
【発明が解決しようとする課題】
しかしながら、金属酸化物薄膜と金属薄膜との積層膜では、金属薄膜が酸化を受け易く、酸化劣化により金属薄膜の抵抗値が高くなり、結果として得られる積層膜の導電性が損なわれるという欠点がある。
【０００５】
本発明は、このような金属薄膜の抵抗値の悪化を防止して表面抵抗値が低く導電性に優れた積層膜を提供することを目的とする。
【０００６】
【課題を解決するための手段】
本発明の積層膜の形成方法は、スパッタリング法により、基板上に金属酸化物薄膜と金属薄膜とを積層形成する積層膜の形成方法において、金属薄膜の成膜後、金属酸化物薄膜の成膜に先立ち、該金属薄膜を酸素ガス雰囲気に晒すことにより、或いは、金属薄膜の成膜後、金属酸化物薄膜の成膜に先立ち、該金属薄膜の表面を酸素プラズマで処理することにより、該金属薄膜の金属酸化物薄膜との界面に、膜厚０．５〜５ｎｍの、該金属薄膜を構成する金属の酸化物層が形成されている積層膜を形成することを特徴とする。
【０００７】
本発明者らは、従来の積層膜において、金属薄膜の抵抗値が高くなる原因について検討した結果、従来の積層膜では、金属酸化物薄膜中の活性酸素（不安定酸素）が金属薄膜との界面へ移動し、金属薄膜が酸化を受けること、また、大気中の水分等により金属薄膜が腐食すること、そして、この結果、金属薄膜の抵抗値が悪化する可能性が高いことを知見した。
【０００８】
そこで、本発明者らは、金属酸化物薄膜から金属薄膜への酸素の移動、大気中の水分等の影響を低減するべく、更に検討を重ねた結果、金属薄膜の金属酸化物薄膜との界面に該金属薄膜を構成する金属の酸化物層を形成することにより、この酸化物層がバリヤー層となって、隣接する金属酸化物薄膜からの酸素の移動や大気中の水分等による酸化劣化から、金属薄膜を保護することができることを見出した。
【０００９】
本発明はこのような知見により完成されたものであり、本発明によれば、金属薄膜の酸化による抵抗値の悪化を防止して、表面抵抗値の低い高導電性積層膜を得ることができる。
【００１０】
この酸化物層は、金属薄膜の基板側と反対側の面に形成されていることが好ましい。
【００１１】
本発明においては、特に、金属酸化物薄膜と金属薄膜とを交互に多層に積層形成した積層膜に有効であり、金属酸化物薄膜としてはＩＴＯ、酸化インジウム、酸化スズ、酸化亜鉛、酸化チタン及び酸化ケイ素よりなる群から選ばれる１種の金属酸化物又は２種以上の複合金属酸化物の薄膜が挙げられる。その他金属酸化物膜としては、例えば酸化亜鉛膜にＺｎ２＋よりイオン半径の小さいＡｌ，Ｓｉ，Ｂ，Ｔｉ，Ｓｎ，Ｍｇ，Ｃｒ，Ｆ，Ｇａ等をドープさせた膜も同様に使用することができる。ドープ量としては通常原子比で１０％以下が好ましい。また、金属薄膜としては、Ａｇ，Ａｕ，Ｐｔ，Ｃｕ，Ａｌ，Ｃｒ，Ｔｉ，Ｚｎ，Ｓｎ，Ｎｉ，Ｃｏ，Ｈｆ，Ｎｂ，Ｔａ，Ｗ，Ｚｒ，Ｐｂ，Ｐｄ及びＩｎよりなる群から選ばれる１種の金属又は２種以上の合金の薄膜が挙げられる。特に、金属酸化物薄膜がＩＴＯであり、金属薄膜がＡｇ薄膜である積層膜が好適であり、このような本発明により、好ましくは表面抵抗値３．５Ω／□以下の透明導電性薄膜が提供される。
【００１２】
【発明の実施の形態】
以下に図面を参照して本発明の積層膜の実施の形態を詳細に説明する。
【００１３】
図１は本発明の積層膜の実施の形態を示す断面図である。
【００１４】
この積層膜は、基板１上に金属酸化物薄膜２と金属薄膜３とが交互に積層形成された積層膜であって、金属薄膜３と金属酸化物薄膜２との界面のうち、基板１とは反対側の面にこの金属薄膜３を構成する金属の酸化物よりなる層４が形成されたものである。
【００１５】
本発明において、金属酸化物薄膜２及び金属薄膜３の種類及びその膜厚、積層数としては特に制限はないが、金属酸化物薄膜２としては、例えば、ＩＴＯ、酸化インジウム、酸化スズ、酸化亜鉛、酸化チタン及び酸化ケイ素よりなる群から選ばれる１種の金属酸化物又は２種以上の複合金属酸化物の薄膜が挙げられ、金属薄膜３としては例えば、Ａｇ，Ａｕ，Ｐｔ，Ｃｕ，Ａｌ，Ｃｒ，Ｔｉ，Ｚｎ，Ｓｎ，Ｎｉ，Ｃｏ，Ｈｆ，Ｎｂ，Ｔａ，Ｗ，Ｚｒ，Ｐｂ，Ｐｄ及びＩｎよりなる群から選ばれる１種の金属又は２種以上の合金の薄膜が挙げられる。
【００１６】
金属酸化物薄膜２の膜厚は通常２０〜２００ｎｍの範囲で適宜設定され、金属薄膜３の膜厚は通常５〜２０ｎｍの範囲で適宜決定される。
【００１７】
金属薄膜３の上面に形成される酸化物層４は、その膜厚が過度に厚いと、得られる積層膜の表面抵抗値が高くなり、過度に薄いとバリヤー層としての機能を有効に得ることができず、金属薄膜３の酸化劣化で抵抗値が悪化する。従って、この酸化物層４の膜厚は０．５〜５ｎｍとする。
【００１８】
なお、このような積層膜を形成する基板１としては、用途に応じて各種の材質、厚みのものが用いられるが、ＰＤＰ等の前面板としての用途においては、ポリエステル、ポリエチレンテレフタレート（ＰＥＴ）、ポリブチレンテレフタレート、ポリメチルメタアクリレート（ＰＭＭＡ）、アクリル、ポリカーボネート（ＰＣ）、ポリスチレン、トリアセテート、ポリビニルアルコール、ポリ塩化ビニル、ポリ塩化ビニリデン、ポリエチレン、エチレン−酢酸ビニル共重合体、ポリウレタン、セロファン等、好ましくはＰＥＴ、ＰＣ、ＰＭＭＡの透明フィルムであって、通常の場合、１μｍ〜１０ｍｍ程度の厚さのものが用いられるが、ガラス基板であっても良い。
【００１９】
このような本発明の積層膜は、スパッタリング法により金属酸化物薄膜２と金属薄膜３とを交互に積層形成するに当たり、金属薄膜３を成膜した後、金属酸化物薄膜２の成膜に先立ち、金属薄膜３を酸素ガス雰囲気に晒すことにより、或いは金属薄膜３の表面を酸素プラズマ処理することにより形成することができる。
【００２０】
金属薄膜３を酸素ガス雰囲気に晒す時には基板を加熱してもよい。プラズマ処理の方法としては、Ａｒ等の不活性ガスにＯ２を混入させた系またはＯ２のみの系にてプラズマを発生し、被処理物の表面で反応（酸化）を起こすことができる方法であればいかなる手法も採用できる。電圧の印加方法は直流、交流、マイクロ波等が考えられる。
【００２１】
本発明の積層膜の形成方法において、その他の成膜条件については、特に制限はなく、常法に従って積層膜の形成を行うことができる。
【００２２】
即ち、例えば、スパッタリング装置の真空槽内に金属ターゲットと金属酸化物ターゲットをセットすると共に基板を配置し、真空槽内を真空引きした後、ＡｒガスとＯ２ガスを導入して圧力０．１〜１．０Ｐａ程度に調整すると共に金属酸化物ターゲットに電圧を印加して、金属酸化物薄膜を形成する。その際の雰囲気ガスのＯ２濃度、即ち、ＡｒガスとＯ２との合計に対するＯ２の体積割合は１〜１０ｖｏｌ％とするのが好ましい。
【００２３】
次いで、雰囲気ガスの置換により、系内を０．１〜１．０Ｐａ程度のＡｒガス雰囲気として金属ターゲットに電圧を印加して、金属薄膜を形成する。その後、雰囲気ガスの置換により系内を１〜５Ｐａ程度のＯ２ガス雰囲気として金属薄膜を酸素ガスに晒して金属薄膜表面に酸化物層を形成する。その後、必要に応じて、上記金属酸化物薄膜の成膜、金属薄膜の成膜及び酸化物層の形成を繰り返し行って、積層膜を形成する。
【００２４】
【実施例】
以下に実施例及び比較例を挙げて本発明をより具体的に説明する。
【００２５】
実施例１
マグネトロンＤＣスパッタリング装置のターゲットとしてＩＴＯとＡｇをセットし、基板として厚さ１８８μｍのＰＥＴフィルムを用いて積層膜の形成を行った。
【００２６】
まず、真空槽をターボ分子ポンプで１×１０−４Ｐａ以下まで排気した後、Ａｒガス２００ｃｃ／ｍｉｎとＯ２ガス６ｃｃ／ｍｉｎとを真空系内に導入し、圧力が０．５Ｐａとなるように調整した。この状態でＩＴＯターゲットに電圧を印加して基板上にＩＴＯ薄膜を成膜した。次に、真空槽内のガスを全てＡｒガスとなるように置換して圧力を０．５Ｐａに調整し、その後Ａｇターゲットに電圧を印加してＡｇ薄膜を成膜した。真空槽内のガスを全てＯ２ガスとなるように置換して圧力を１００Ｐａに調整し、１分間保持することにより、Ａｇ薄膜の表面に酸化物層を形成した。この時基板加熱は行わなかった。その後、再び上記と同様のＡｒ／Ｏ２ガス雰囲気でＩＴＯ薄膜を成膜して、基板上に、膜厚３０ｎｍのＩＴＯ薄膜／膜厚１５ｎｍのＡｇ薄膜／膜厚５ｎｍのＡｇ２Ｏ層／膜厚３０ｎｍのＩＴＯ薄膜の積層膜を形成した。
【００２７】
この積層膜を６０℃、９０％ＲＨの湿熱雰囲気に４８時間晒す耐候性試験を行い、試験前後の表面抵抗値を調べ、結果を表１に示した。
【００２８】
比較例１
実施例１において、酸化物層を形成しなかったこと以外は同様にして積層膜を形成し、同様に耐候性試験前後の表面抵抗値を調べ、結果を表１に示した。
【００２９】
表１より、酸化物層を形成することにより、抵抗値が低く導電性に優れ、その耐候性にも優れた積層膜を形成することができることがわかる。
【００３０】
【表１】
なお、実施例１の方法で、同様に雰囲気ガスの切り換えを行って、ＩＴＯ，Ａｇ７層、バリア３層の積層膜を形成し、電磁波シールド性熱線カットフィルムとしてＰＤＰの前面に配置して使用したところ、長期に亘り良好な特性を得ることができた。
【００３２】
【発明の効果】
以上詳述した通り、本発明によれば、金属薄膜と金属酸化物薄膜との多層積層膜であって、表面抵抗値が低く、ＰＤＰの前面板の電磁波シールド性熱線カットフィルム等として有用な高特性積層膜が提供される。
【図面の簡単な説明】
【図１】 本発明の積層膜の実施の形態を示す断面図である。
【符号の説明】
１ 基板
２ 金属酸化物薄膜
３ 金属薄膜
４ 酸化物層[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a laminated film in which metal oxide thin films and metal thin films are alternately laminated on a substrate, and in particular, a transparent conductive thin film or heat ray reflective film disposed on the front surface of a plasma display panel (PDP). The present invention relates to a method for forming a laminated film having a low resistance and excellent conductivity that is useful as a sputtering method.
[0002]
[Prior art]
The front plate of the PDP is required to have excellent antireflection performance (that is, high visible light transmittance (visible light low reflectivity)), heat ray reflection (near infrared cut) performance, electromagnetic wave shielding performance, etc. Among such required performances, as a combination of heat ray reflectivity and electromagnetic shielding properties, a metal oxide thin film such as ITO (tin indium oxide) and a metal thin film such as Ag are alternately laminated on a PET film. A laminated film is provided.
[0003]
As a method for forming this laminated film, there are various methods such as a sputtering method, an ion plating method, a CVD method and the like, but the sputtering method is most preferable from the viewpoint of easy film thickness control. The formation of the metal thin film by the sputtering method is performed in an argon (Ar) atmosphere. When the metal oxide thin film is formed by the sputtering method, oxygen (O 2 ) is introduced into the atmosphere gas, and Ar / Performed in an O 2 atmosphere.
[0004]
[Problems to be solved by the invention]
However, in the laminated film of the metal oxide thin film and the metal thin film, the metal thin film is susceptible to oxidation, and the resistance value of the metal thin film is increased due to oxidative degradation, and the conductivity of the resulting laminated film is impaired. is there.
[0005]
An object of the present invention is to provide a laminated film having a low surface resistance value and excellent electrical conductivity by preventing such deterioration of the resistance value of the metal thin film.
[0006]
[Means for Solving the Problems]
Method of forming a laminated film of the present invention, by a sputtering method, method of forming a laminated film formed by lamination of a metallic oxide thin film and the metal thin film on the substrate, after forming the metal thin film, the metal oxide thin film formed By exposing the metal thin film to an oxygen gas atmosphere prior to the film, or by treating the surface of the metal thin film with oxygen plasma after the metal thin film is formed and before forming the metal oxide thin film, the interface between the metal oxide thin film of the metal thin film, with a thickness of 0.5 to 5 nm, and forming a laminated film oxide layer of the metal constituting the metal thin film is formed.
[0007]
As a result of examining the cause of the high resistance of the metal thin film in the conventional laminated film, the present inventors have found that the active oxygen (unstable oxygen) in the metal oxide thin film is different from the metal thin film in the conventional laminated film. It has been found that the metal thin film is oxidized, the metal thin film is corroded by moisture in the atmosphere, and the resistance value of the metal thin film is likely to deteriorate as a result.
[0008]
Accordingly, the present inventors have conducted further studies to reduce the influence of oxygen transfer from the metal oxide thin film to the metal thin film, moisture in the atmosphere, etc. As a result, the interface between the metal thin film and the metal oxide thin film By forming an oxide layer of the metal constituting the metal thin film on the surface, this oxide layer becomes a barrier layer, and from the movement of oxygen from the adjacent metal oxide thin film and the oxidative deterioration due to moisture in the atmosphere. It was found that the metal thin film can be protected.
[0009]
The present invention has been completed based on such findings. According to the present invention, it is possible to prevent deterioration of the resistance value due to oxidation of a metal thin film and obtain a highly conductive laminated film having a low surface resistance value. .
[0010]
This oxide layer is preferably formed on the surface opposite to the substrate side of the metal thin film.
[0011]
In the present invention, it is particularly effective for a laminated film in which a metal oxide thin film and a metal thin film are alternately formed in multiple layers. As the metal oxide thin film, ITO, indium oxide, tin oxide, zinc oxide, titanium oxide and One type of metal oxide selected from the group consisting of silicon oxide or a thin film of two or more types of composite metal oxides may be mentioned. As the other metal oxide film, for example, a film obtained by doping a zinc oxide film with Al, Si, B, Ti, Sn, Mg, Cr, F, Ga or the like having an ion radius smaller than that of Zn 2+ can be used in the same manner. it can. The doping amount is usually preferably 10% or less by atomic ratio. The metal thin film is selected from the group consisting of Ag, Au, Pt, Cu, Al, Cr, Ti, Zn, Sn, Ni, Co, Hf, Nb, Ta, W, Zr, Pb, Pd and In. A thin film of one kind of metal or two or more kinds of alloys may be mentioned. In particular, a laminated film in which the metal oxide thin film is ITO and the metal thin film is an Ag thin film is suitable. According to the present invention, a transparent conductive thin film having a surface resistance value of 3.5Ω / □ or less is preferably provided. Is done .
[0012]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the laminated film of the present invention will be described in detail with reference to the drawings.
[0013]
FIG. 1 is a cross-sectional view showing an embodiment of a laminated film of the present invention.
[0014]
This laminated film is a laminated film in which the metal oxide
[0015]
In the present invention, the type and thickness of the metal oxide
[0016]
The film thickness of the metal oxide
[0017]
When the thickness of the oxide layer 4 formed on the upper surface of the metal thin film 3 is excessively large, the surface resistance value of the obtained laminated film becomes high, and when it is excessively thin, the function as a barrier layer can be effectively obtained. The resistance value deteriorates due to the oxidative deterioration of the metal thin film 3. Therefore, the thickness of the oxide layer 4 is set to 0.5 to 5 nm.
[0018]
In addition, as the board | substrate 1 which forms such a laminated film, the thing of various materials and thickness is used according to a use, However, In the use as front plates, such as PDP, polyester, polyethylene terephthalate (PET), Polybutylene terephthalate, polymethyl methacrylate (PMMA), acrylic, polycarbonate (PC), polystyrene, triacetate, polyvinyl alcohol, polyvinyl chloride, polyvinylidene chloride, polyethylene, ethylene-vinyl acetate copolymer, polyurethane, cellophane, etc. Is a transparent film of PET, PC, PMMA, and usually has a thickness of about 1 μm to 10 mm, but may be a glass substrate.
[0019]
In such a laminated film of the present invention, when the metal oxide
[0020]
When the metal thin film 3 is exposed to an oxygen gas atmosphere, the substrate may be heated. As a method of plasma treatment, a method in which plasma is generated in a system in which O 2 is mixed in an inert gas such as Ar or a system only of O 2 and reaction (oxidation) can be caused on the surface of an object to be processed. Any method can be used. The voltage application method may be direct current, alternating current, microwave, or the like.
[0021]
In the method for forming a laminated film of the present invention, other film forming conditions are not particularly limited, and the laminated film can be formed according to a conventional method.
[0022]
That is, for example, a metal target and a metal oxide target are set in a vacuum chamber of a sputtering apparatus, a substrate is disposed, the inside of the vacuum chamber is evacuated, Ar gas and O 2 gas are introduced, and a pressure of 0.1 is set. A metal oxide thin film is formed by adjusting the voltage to about 1.0 Pa and applying a voltage to the metal oxide target. O 2 concentration in the atmosphere gas at that time, i.e., the volume ratio of O 2 to the sum of Ar gas and O 2 is preferably a 1~10vol%.
[0023]
Next, by replacing the atmospheric gas with the inside of the system as an Ar gas atmosphere of about 0.1 to 1.0 Pa, a voltage is applied to the metal target to form a metal thin film. Thereafter, the metal thin film is exposed to oxygen gas to form an O 2 gas atmosphere of about 1 to 5 Pa by replacing the atmospheric gas to form an oxide layer on the surface of the metal thin film. Thereafter, if necessary, the metal oxide thin film, the metal thin film, and the oxide layer are repeatedly formed to form a laminated film.
[0024]
【Example】
Hereinafter, the present invention will be described more specifically with reference to Examples and Comparative Examples.
[0025]
Example 1
ITO and Ag were set as targets of a magnetron DC sputtering apparatus, and a laminated film was formed using a PET film having a thickness of 188 μm as a substrate.
[0026]
First, after evacuating the vacuum tank to 1 × 10 −4 Pa or less with a turbo molecular pump, Ar gas 200 cc / min and O 2 gas 6 cc / min are introduced into the vacuum system so that the pressure becomes 0.5 Pa. Adjusted. In this state, a voltage was applied to the ITO target to form an ITO thin film on the substrate. Next, the gas in the vacuum chamber was entirely replaced with Ar gas to adjust the pressure to 0.5 Pa, and then a voltage was applied to the Ag target to form an Ag thin film. The gas in the vacuum chamber was all replaced with O 2 gas, the pressure was adjusted to 100 Pa, and held for 1 minute to form an oxide layer on the surface of the Ag thin film. At this time, the substrate was not heated. Thereafter, an ITO thin film was formed again in the same Ar / O 2 gas atmosphere as described above, and an ITO thin film with a thickness of 30 nm / Ag thin film with a thickness of 15 nm / Ag 2 O layer with a thickness of 5 nm / film on the substrate. A laminated film of ITO thin films having a thickness of 30 nm was formed.
[0027]
A weather resistance test was performed in which this laminated film was exposed to a wet heat atmosphere of 60 ° C. and 90% RH for 48 hours, and the surface resistance values before and after the test were examined. The results are shown in Table 1.
[0028]
Comparative Example 1
In Example 1, a laminated film was formed in the same manner except that the oxide layer was not formed. Similarly, the surface resistance values before and after the weather resistance test were examined, and the results are shown in Table 1.
[0029]
From Table 1, it can be seen that by forming the oxide layer, a laminated film having a low resistance value, excellent conductivity, and excellent weather resistance can be formed.
[0030]
[Table 1]
In addition, by switching the atmospheric gas in the same manner as in Example 1, a laminated film of ITO, Ag7 layer and barrier 3 layer was formed and used as an electromagnetic shielding heat ray cut film placed on the front surface of the PDP. However, good characteristics could be obtained over a long period of time.
[0032]
【The invention's effect】
As described above in detail, according to the present invention, a multilayer laminated film of a metal thin film and a metal oxide thin film, which has a low surface resistance value and is useful as an electromagnetic wave shielding heat ray cut film for a front panel of a PDP. A characteristic laminate film is provided.
[Brief description of the drawings]
FIG. 1 is a cross-sectional view showing an embodiment of a laminated film of the present invention.
[Explanation of symbols]
1
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| JP2000146892A JP4432206B2 (en) | 2000-05-18 | 2000-05-18 | Method for forming laminated film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000146892A JP4432206B2 (en) | 2000-05-18 | 2000-05-18 | Method for forming laminated film |
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| Publication Number | Publication Date |
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| JP2001328198A JP2001328198A (en) | 2001-11-27 |
| JP4432206B2 true JP4432206B2 (en) | 2010-03-17 |
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| JP2000146892A Expired - Fee Related JP4432206B2 (en) | 2000-05-18 | 2000-05-18 | Method for forming laminated film |
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