JP4978297B2 - Transparent conductive gas barrier film - Google Patents
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本発明は、例えばLCDや有機EL素子を用いたフィルムディスプレイの電極として用いられる耐溶剤性に優れた透明導電性フィルムに関するものである。 The present invention relates to a transparent conductive film excellent in solvent resistance used as an electrode of a film display using, for example, an LCD or an organic EL element.
近年、液晶ディスプレイ(LCD)やエレクトロルミネッセンス(EL)ディスプレイなどのようなフラットパネルディスプレイが、広く普及してきた。
これらの情報機器の携帯性を向上するため、より一層の薄型化・軽量化、耐破損性が求められている。従来、LCD、タッチパネルの透明導電性基板として、重く、厚く、割れやすいガラス基板が用いられて来たが、これに代わる材料として、透明導電性樹脂基板が提案されている。しかし、透明導電性樹脂基板は、耐久性、耐溶剤性、ガスバリア性等の基本特性がガラス基板より劣っている。
In recent years, flat panel displays such as liquid crystal displays (LCD) and electroluminescence (EL) displays have become widespread.
In order to improve the portability of these information devices, further reduction in thickness / weight and damage resistance are required. Conventionally, glass substrates that are heavy, thick, and easy to break have been used as transparent conductive substrates for LCDs and touch panels, but transparent conductive resin substrates have been proposed as an alternative material. However, the transparent conductive resin substrate is inferior to the glass substrate in basic characteristics such as durability, solvent resistance, and gas barrier properties.
例えば、透明導電性樹脂基板を、LCD用電極基板として利用しようとした場合、金属酸化物層を設けることにより、ガスバリア性は付与できる。しかし、液晶配向膜形成過程で、液晶配向膜の前駆材料をN−メチルピロリドン(NMP)等の溶剤に溶解した塗工液をコーティングする際に、上記溶剤に透明導電性樹脂基板が、白化、膨潤等の損傷を受ける。そこで、基板の上記溶剤による白化を防止するために、基板上に高分子膜を塗布し、耐溶剤性を付与することが一般的に行われている(特許文献1)。 For example, when a transparent conductive resin substrate is to be used as an electrode substrate for LCD, gas barrier properties can be imparted by providing a metal oxide layer. However, in the process of forming the liquid crystal alignment film, when the coating liquid prepared by dissolving the precursor material of the liquid crystal alignment film in a solvent such as N-methylpyrrolidone (NMP) is coated, the transparent conductive resin substrate is whitened in the solvent, Damage such as swelling. Therefore, in order to prevent whitening of the substrate due to the solvent, it is generally performed to apply a polymer film on the substrate to impart solvent resistance (Patent Document 1).
しかしながら、上記従来の技術では、少なくとも3層成膜する必要があることに加えて、有機層/無機層/有機層という積層のため無機層は真空プロセス、有機層は大気中プロセスと、成膜プロセスが全く違う工程を順に通すことによるコストアップは避けることができない。
よってできるだけ単一プロセスで各層を形成することができる膜構成が望まれている。しかし、ディスプレイ基板として使用に耐えうるガスバリア層を形成するには今のところ真空プロセス以外にない。有機層を真空プロセスで形成可能なものに置換することが望まれている。
Therefore, a film configuration capable of forming each layer by a single process as much as possible is desired. However, there is currently no vacuum process other than the vacuum process to form a gas barrier layer that can be used as a display substrate. It is desirable to replace the organic layer with one that can be formed by a vacuum process.
本発明の目的は、かかる従来技術の問題点を解決し、真空プロセスのみの単一プロセスによって製造可能であるとともに、耐溶剤性に優れた透明導電性フィルムを提供することにある。 An object of the present invention is to solve the problems of the prior art and to provide a transparent conductive film which can be produced by a single process only of a vacuum process and has excellent solvent resistance.
請求項1に記載の発明は、プラスチックフィルムの少なくとも一方の面に、プラズマイオン注入法によって層厚が15nm以上150nm以下であるイオン注入層が形成されており、前記イオン注入層の上にガスバリア層、透明導電層を順次形成してなることを特徴とする透明導電性ガスバリアフィルムである。
請求項2に記載の発明は、前記イオン注入層は、プラズマソースとして希ガス、水素、窒素、アンモニアガスのうち少なくとも一種類のガスを用いて形成されたものであることを特徴とする請求項1に記載の透明導電性ガスバリアフィルムである。
請求項3に記載の発明は、前記イオン注入層のC=C結合(Bc=c)とC−C結合(Bc−c)との比である、Bc=c/Bc−cが0.2以上であることを特徴とする請求項1または2に記載の透明導電性フィルムである。
According to the first aspect of the present invention, an ion implantation layer having a layer thickness of 15 nm or more and 150 nm or less is formed on at least one surface of the plastic film by a plasma ion implantation method, and a gas barrier layer is formed on the ion implantation layer. The transparent conductive gas barrier film is formed by sequentially forming transparent conductive layers.
The invention according to
The invention according to
本発明の透明導電性フィルムは、プラスチックフィルムの少なくとも一方の面に、プラズマイオン注入法によって層厚が15nm以上150nm以下であるイオン注入層が形成されており、前記イオン注入層の上にガスバリア層、透明導電層を順次形成してなることを特徴としている。従来技術は上述のように、耐溶剤性を高めるためにアクリレートのような耐溶剤性の高い高分子膜を形成した後、ガスバリア層及び透明導電性薄膜を形成していたが、本発明では、上記イオン注入層が耐溶剤性を付与するものであり、従来技術と同等の性能を提供する。イオン注入層においてはイオン注入によってプラスチックの基本構造の結合が切断され新たに炭素の二重結合が形成されることによって、プラスチック表面に溶剤に対して可溶ではない炭素の二重結合が多く含まれた薄膜が形成され、これが耐溶剤性に寄与する。
このように本発明によれば、真空プロセスのみの単一プロセスによって製造可能であるとともに、耐溶剤性に優れた透明導電性フィルムを提供することができる。
In the transparent conductive film of the present invention, an ion implantation layer having a layer thickness of 15 nm or more and 150 nm or less is formed on at least one surface of a plastic film by a plasma ion implantation method, and a gas barrier layer is formed on the ion implantation layer. The transparent conductive layer is sequentially formed. As described above, the prior art has formed a gas barrier layer and a transparent conductive thin film after forming a polymer film having high solvent resistance such as acrylate in order to improve solvent resistance. The ion-implanted layer imparts solvent resistance and provides performance equivalent to that of the prior art. In the ion-implanted layer, the bond of the plastic basic structure is cut by ion implantation and new carbon double bonds are formed, so that there are many carbon double bonds that are not soluble in the solvent on the plastic surface. A thin film is formed, which contributes to solvent resistance.
As described above, according to the present invention, it is possible to provide a transparent conductive film that can be manufactured by a single process including only a vacuum process and is excellent in solvent resistance.
以下、本発明の実施の形態を図面を用いながら詳細に説明する。
図1は、本発明の透明導電性ガスバリアフィルムの一形態の断面図である。図1の形態の透明導電性ガスバリアフィルムは、プラスチックフィルム(1)上に、イオン注入層(2)が形成され、さらにガスバリア層(3)および透明導電層(4)が順次形成されている。このイオン注入層(2)はプラズマイオン注入法によって形成されており、その上に形成されているガスバリア層(3)は例えば、DC及びRFマグネトロンスパッタリング法もしくはCVD法によって形成されており、透明導電層(4)は例えば、DCスパッタリング方式により形成された膜である。
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
FIG. 1 is a cross-sectional view of one embodiment of the transparent conductive gas barrier film of the present invention. In the transparent conductive gas barrier film in the form of FIG. 1, an ion implantation layer (2) is formed on a plastic film (1), and a gas barrier layer (3) and a transparent conductive layer (4) are sequentially formed. This ion implantation layer (2) is formed by a plasma ion implantation method, and the gas barrier layer (3) formed thereon is formed by, for example, a DC and RF magnetron sputtering method or a CVD method. The layer (4) is, for example, a film formed by a DC sputtering method.
本発明の透明導電性フィルムを構成するプラスチックフィルム(1)としては、例えばポリエチレンテレフタレート(PET)に代表されるポリエステルフィルムや、ポリカーボネートフィルム、ポリアリレートフィルムやポリエーテルサルフォンフィルム等のエンジニアリングプラスチックフィルムなどが挙げられる。特にLCD用途に用いる場合は、複屈折率の少ないプラスチックフィルムが好ましい。なお本発明の透明導電性フィルムは、ディスプレイ全面に貼りつける形になるので,このプラスチックフィルム(1)は透明性を有することが必要条件となる。 基材の厚さは特に限定はしないが、100ミクロン〜200ミクロン程度が適している。 Examples of the plastic film (1) constituting the transparent conductive film of the present invention include a polyester film represented by polyethylene terephthalate (PET), an engineering plastic film such as a polycarbonate film, a polyarylate film, and a polyethersulfone film. Is mentioned. In particular, when used for LCD, a plastic film having a low birefringence is preferable. In addition, since the transparent conductive film of this invention becomes a form affixed on the display whole surface, it becomes a necessary condition that this plastic film (1) has transparency. The thickness of the substrate is not particularly limited, but about 100 to 200 microns is suitable.
また、イオン注入層(2)は、プラズマイオン注入法によって形成されている。プラズマイオン注入条件は、プラスチックフィルム(1)に印加するパルス電圧が5kV〜20kV、パルス幅が10μsec〜20μsec程度の条件が適している。また、イオン注入に使用するプラズマソースとしては希ガス、水素、窒素、アンモニアガスのうち少なくとも一種類のガスが好ましい。上記したプラズマソースを用いることで、プラスチックフィルム(1)表面がより活性化され、後述するガスバリア層との密着が良くなる。十分な密度を有するイオン注入層をより短時間で形成するためには、プラズマソースとしてはイオン注入深度が比較的浅く、プラズマの安定性が良好なアルゴンを用いることが特に好ましい。
またイオン注入層(2)層の層厚は15nm以上150nm以下が好ましい。15nm未満では充分な耐溶剤性が得られない。また150nmを超えると、良好な透明性を得られない可能性が高い。
さらに好ましいイオン注入層(2)層の層厚は30nm以上70nm以下である。
The ion implantation layer (2) is formed by a plasma ion implantation method. As the plasma ion implantation conditions, a pulse voltage applied to the plastic film (1) of 5 kV to 20 kV and a pulse width of about 10 μsec to 20 μsec are suitable. Further, as a plasma source used for ion implantation, at least one kind of gas among rare gas, hydrogen, nitrogen, and ammonia gas is preferable. By using the plasma source described above, the surface of the plastic film (1) is more activated, and adhesion with a gas barrier layer described later is improved. In order to form an ion-implanted layer having a sufficient density in a shorter time, it is particularly preferable to use argon with a relatively shallow ion implantation depth and good plasma stability as the plasma source.
The layer thickness of the ion implantation layer (2) is preferably 15 nm or more and 150 nm or less. If it is less than 15 nm, sufficient solvent resistance cannot be obtained. Moreover, when it exceeds 150 nm, possibility that favorable transparency will not be acquired is high.
The layer thickness of the more preferable ion implantation layer (2) is 30 nm or more and 70 nm or less.
また本発明によれば、イオン注入層のC=C結合(Bc=c)とC−C結合(Bc−c)との比である、Bc=c/Bc−cが0.2以上であることが好ましい。この値が0.2以上であることにより、アモルファス化が進み、耐溶剤性が向上し、硬度も増す。Bc=c/Bc−cは、化学修飾法を用いて測定することができる。Bc=cを検出する場合は、臭素をクロロホルムで希釈したものにサンプルを浸すことにより、サンプル表面にあるC=CをC-Brで置換し、それをXPSを用いて測定することにより、C-CとC-Brの比が測定できこれがすなわち、C-C結合とC=C結合の比となる。
さらに好ましいBc=c/Bc−cは0.2〜0.5である。
Further, according to the present invention, Bc = c / Bc-c, which is a ratio of C = C bond (Bc = c) and CC bond (Bc-c) of the ion implantation layer, is 0.2 or more. It is preferable. When this value is 0.2 or more, amorphization progresses, solvent resistance is improved, and hardness is increased. Bc = c / Bc-c can be measured using a chemical modification method. When detecting Bc = c, the sample is immersed in a solution of bromine diluted with chloroform, C = C on the sample surface is replaced with C-Br, and it is measured using XPS. And C-Br ratio can be measured, that is, the ratio of CC bond to C = C bond.
More preferable Bc = c / Bc-c is 0.2 to 0.5.
本発明におけるガスバリア層(3)は、高い透明性と高いガスバリア性能を有していれば特に限定されないが、DCスパッタリング法やCVD法で形成された、酸化珪素薄膜や、酸窒化珪素が好んで用いられる。 The gas barrier layer (3) in the present invention is not particularly limited as long as it has high transparency and high gas barrier performance, but a silicon oxide thin film or silicon oxynitride formed by a DC sputtering method or a CVD method is preferred. Used.
本発明における透明導電層(4)の材料としては、酸化インジウムスズ(ITO)が特に多く用いられているが、酸化亜鉛や酸化錫等、高い透明性と高い導電性を有していれば特に限定されない。 As the material of the transparent conductive layer (4) in the present invention, indium tin oxide (ITO) is used in particular, especially if it has high transparency and high conductivity such as zinc oxide and tin oxide. It is not limited.
以下、実施例および比較例により、本発明をさらに具体的に説明するが、本発明は下記例に制限されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further more concretely, this invention is not restrict | limited to the following example.
〈実施例1〉
厚さ100μmのPETフィルム(東レ社製、T60)基材にアルゴンイオン注入層を設けた。その際、基材に印加した電圧は20kVでパルス幅は20μ秒であった。40秒間、アルゴンイオン注入を行ったところ、約30nmのイオン注入層を得た。このイオン注入層上に、NMPを数滴垂らし80℃5分間保持後、水洗し外観変化を見たところ、滴下前と変化は見られなかった。この際、イオン注入層のBc=c/Bc−cは0.5であった。その後、ガスバリア層としてDCマグネトロンスパッタ法によって20nmの物理的膜厚を有する酸化珪素薄膜を形成した。この積層体の酸素透過速度をMOCON社製OXTRANにて30℃、70%RHの条件下で測定したところ0.2cc/m2/dayであり、水蒸気透過速度を同じくMOCON社製PERMATRANにて40℃、90%RHの条件下で測定したところ0.2g/m2/dayであり、良好なガスバリア性能を有していた。その後、ガスバリア層上にITO薄膜をDCマグネトロンスパッタ法によって150nm成膜した。この際、表面抵抗値は35Ω/□であった。以上の積層体を再び同様にNMP処理を行ったところ外観に変化は見られなかった。
<Example 1>
An argon ion-implanted layer was provided on a 100 μm-thick PET film (Toray Industries, T60) substrate. At that time, the voltage applied to the substrate was 20 kV and the pulse width was 20 μsec. When argon ion implantation was performed for 40 seconds, an ion implantation layer of about 30 nm was obtained. On this ion-implanted layer, a few drops of NMP were dropped and held at 80 ° C. for 5 minutes, then washed with water and the appearance was changed. At this time, Bc = c / Bc-c of the ion implantation layer was 0.5. Thereafter, a silicon oxide thin film having a physical film thickness of 20 nm was formed as a gas barrier layer by DC magnetron sputtering. The oxygen transmission rate of this laminate was measured with MOCON OXTRAN at 30 ° C and 70% RH and found to be 0.2 cc / m 2 / day, and the water vapor transmission rate was 40 ° C with MOCON PERMATRAN. When measured under the condition of 90% RH, it was 0.2 g / m 2 / day and had good gas barrier performance. Thereafter, an ITO thin film was formed on the gas barrier layer to a thickness of 150 nm by DC magnetron sputtering. At this time, the surface resistance value was 35Ω / □. When the above laminate was similarly subjected to NMP treatment again, no change in appearance was observed.
<実施例2>
厚さ188μmのポリカーボネートフィルム(帝人社製、パンライト)基材に、窒素イオン注入層を設けた。その際、基材に印加した電圧は5kVでパルス幅は20μ秒であった。40秒間、窒素イオン注入を行ったところ、約15nmのイオン注入層を得た。この積層体上に、NMPを数滴垂らし80℃5分間保持後、水洗し外観変化を見たところ、滴下前と変化は見られなかった。この際、イオン注入層のBc=c/Bc−cは0.2であった。その後、ガスバリア層としてDCマグネトロンスパッタ法によって20nmの物理的膜厚を有する酸化珪素薄膜を形成した。この積層体の酸素透過速度をMOCON社製OXTRANにて30℃、70%RHの条件下で測定したところ0.15cc/m2/dayであり、水蒸気透過速度を同じくMOCON社製PERMATRANにて40℃、90%RHの条件下で測定したところ0.12g/m2/dayであり、良好なガスバリア性能を有していた。その後、同様にITO薄膜をDCマグネトロンスパッタ法によって150nm成膜した。この際、表面抵抗値は35Ω/□であった。以上の積層体を再び同様にNMP処理を行ったところ外観に変化は見られなかった。
<Example 2>
A nitrogen ion-implanted layer was provided on a polycarbonate film substrate (Panlite, manufactured by Teijin Limited) having a thickness of 188 μm. At that time, the voltage applied to the substrate was 5 kV and the pulse width was 20 μsec. When nitrogen ion implantation was performed for 40 seconds, an ion implantation layer of about 15 nm was obtained. On this laminate, several drops of NMP were dropped and kept at 80 ° C. for 5 minutes, then washed with water and the appearance was changed. At this time, Bc = c / Bc-c of the ion implantation layer was 0.2. Thereafter, a silicon oxide thin film having a physical film thickness of 20 nm was formed as a gas barrier layer by DC magnetron sputtering. The oxygen transmission rate of this laminate was measured at 30 ° C. and 70% RH using an OXTRAN manufactured by MOCON, and found to be 0.15 cc / m 2 / day, and the water vapor transmission rate was 40 ° C. using PERMATRAN manufactured by MOCON. When measured under the condition of 90% RH, it was 0.12 g / m 2 / day and had good gas barrier performance. Thereafter, similarly, an ITO thin film was formed to a thickness of 150 nm by a DC magnetron sputtering method. At this time, the surface resistance value was 35Ω / □. When the above laminate was similarly subjected to NMP treatment again, no change in appearance was observed.
<実施例3>
厚さ188μmのポリカーボネート(帝人社製、パンライト)基材に、水素イオン注入層を設けた。その際、基材に印加した電圧は20kVでパルス幅は20μ秒であった。300秒間、水素イオン注入を行ったところ、約150nmのイオン注入層を得た。この積層体上に、NMPを数滴垂らし80℃5分間保持後、水洗し外観変化を見たところ、滴下前と変化は見られなかった。この際、イオン注入層のBc=c/Bc−cは0.35であった。その後、ガスバリア層としてDCマグネトロンスパッタ法によって20nmの物理的膜厚を有する酸化珪素薄膜を形成した。この積層体の酸素透過速度をMOCON社製OXTRANにて30℃、70%RHの条件下で測定したところ0.15cc/m2/dayであり、水蒸気透過速度を同じくMOCON社製PERMATRANにて40℃、90%RHの条件下で測定したところ0.12g/m2/dayであり、良好なガスバリア性能を有していた。その後、同様にITO薄膜をDCマグネトロンスパッタ法によって150nm成膜した。この際、表面抵抗値は35Ω/□であった。以上の積層体を再び同様にNMP処理を行ったところ外観に変化は見られなかった。
<Example 3>
A hydrogen ion-implanted layer was provided on a polycarbonate substrate (Panlite, Teijin Ltd.) having a thickness of 188 μm. At that time, the voltage applied to the substrate was 20 kV and the pulse width was 20 μsec. When hydrogen ion implantation was performed for 300 seconds, an ion implantation layer of about 150 nm was obtained. On this laminate, several drops of NMP were dropped and kept at 80 ° C. for 5 minutes, then washed with water and the appearance was changed. At this time, Bc = c / Bc-c of the ion implantation layer was 0.35. Thereafter, a silicon oxide thin film having a physical film thickness of 20 nm was formed as a gas barrier layer by DC magnetron sputtering. The oxygen transmission rate of this laminate was measured at 30 ° C. and 70% RH using an OXTRAN manufactured by MOCON, and found to be 0.15 cc / m 2 / day, and the water vapor transmission rate was 40 ° C. using PERMATRAN manufactured by MOCON. When measured under the condition of 90% RH, it was 0.12 g / m 2 / day and had good gas barrier performance. Thereafter, similarly, an ITO thin film was formed to a thickness of 150 nm by a DC magnetron sputtering method. At this time, the surface resistance value was 35Ω / □. When the above laminate was similarly subjected to NMP treatment again, no change in appearance was observed.
〈比較例1〉
厚さ188μmのポリカーボネート(帝人社製、パンライト)基材に、アルゴンイオン注入層を設けた。その際、基材に印加した電圧は1kVでパルス幅は20μ秒であった。40秒間、水素イオン注入を行ったところ、7.5nmのイオン注入層を得た。この積層体上に、NMPを数滴垂らし80℃5分間保持後、水洗し外観変化を見たところ、白濁が見られた。この際、イオン注入層のBc=c/Bc−cは0.1であった。その後、ガスバリア層としてDCマグネトロンスパッタ法によって20nmの物理的膜厚を有する酸化珪素薄膜を形成した。この積層体の酸素透過速度をMOCON社製OXTRANにて30℃、70%RHの条件下で測定したところ0.15cc/m2/dayであり、水蒸気透過速度を同じくMOCON社製PERMATRANにて40℃、90%RHの条件下で測定したところ0.12g/m2/dayであり、良好なガスバリア性能を有していた。その後、同様にITO薄膜をDCマグネトロンスパッタ法によって150nm成膜した。この際、表面抵抗値は35Ω/□であった。以上の積層体を再び同様にNMP処理を行ったところやはり白濁が見られた。
<Comparative example 1>
An argon ion-implanted layer was provided on a polycarbonate substrate (Panlite, manufactured by Teijin Limited) having a thickness of 188 μm. At that time, the voltage applied to the substrate was 1 kV and the pulse width was 20 μsec. When hydrogen ion implantation was performed for 40 seconds, a 7.5 nm ion-implanted layer was obtained. On this laminate, several drops of NMP were dropped and kept at 80 ° C. for 5 minutes, then washed with water and the appearance changed. As a result, white turbidity was observed. At this time, Bc = c / Bc-c of the ion implantation layer was 0.1. Thereafter, a silicon oxide thin film having a physical film thickness of 20 nm was formed as a gas barrier layer by DC magnetron sputtering. The oxygen transmission rate of this laminate was measured at 30 ° C. and 70% RH using an OXTRAN manufactured by MOCON, and found to be 0.15 cc / m 2 / day, and the water vapor transmission rate was 40 ° C. using PERMATRAN manufactured by MOCON. When measured under the condition of 90% RH, it was 0.12 g / m 2 / day and had good gas barrier performance. Thereafter, similarly, an ITO thin film was formed to a thickness of 150 nm by a DC magnetron sputtering method. At this time, the surface resistance value was 35Ω / □. When the above laminate was again subjected to NMP treatment, white turbidity was still observed.
本発明の透明導電性フィルムは、真空プロセスのみを用いて形成でき、コスト性に優れるとともに、耐溶剤性にも優れるので、例えばLCDや有機EL素子を用いたフィルムディスプレイの電極として有用である。 The transparent conductive film of the present invention can be formed using only a vacuum process, and is excellent in cost and solvent resistance. Therefore, the transparent conductive film is useful as an electrode of a film display using, for example, an LCD or an organic EL element.
(1) プラスチックフィルム
(2) イオン注入層
(3) ガスバリア層
(4) 透明導電層
(1) Plastic film (2) Ion implantation layer (3) Gas barrier layer (4) Transparent conductive layer
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