JP2823931B2 - Conductive transparent film and method for producing the same - Google Patents
Conductive transparent film and method for producing the sameInfo
- Publication number
- JP2823931B2 JP2823931B2 JP2073290A JP7329090A JP2823931B2 JP 2823931 B2 JP2823931 B2 JP 2823931B2 JP 2073290 A JP2073290 A JP 2073290A JP 7329090 A JP7329090 A JP 7329090A JP 2823931 B2 JP2823931 B2 JP 2823931B2
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- Japan
- Prior art keywords
- film
- conductive transparent
- conductivity
- transparent
- transparent film
- Prior art date
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- Compositions Of Macromolecular Compounds (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Physical Vapour Deposition (AREA)
- Conductive Materials (AREA)
- Non-Insulated Conductors (AREA)
- Manufacturing Of Electric Cables (AREA)
- Laminated Bodies (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、ほとんど無色透明で、導電性の優れている
可とう性フィルム及びその製造方法に関する。Description: TECHNICAL FIELD The present invention relates to a flexible film which is almost colorless and transparent and has excellent conductivity, and a method for producing the same.
導電性透明フィルムとして、ポリエチレンテレフタレ
ート（以下、PETと略記する）などの透明プラスチック
フィルムにインジウム・スズ酸化物（以下、ITOと略記
する）膜を形成したフィルムが市販されている。As the conductive transparent film, a film in which an indium tin oxide (hereinafter abbreviated as ITO) film is formed on a transparent plastic film such as polyethylene terephthalate (hereinafter abbreviated as PET) is commercially available.
これらの導電性透明フィルムは透明性の点では優れて
いるが、導電性の点では表面抵抗が数100Ω／□であ
り、十分な導電性が得られないという欠点があった。These conductive transparent films are excellent in terms of transparency, but have a drawback that, in terms of conductivity, the surface resistance is several hundred Ω / □, and sufficient conductivity cannot be obtained.
本発明の目的は、透明性と導電性が共に優れている可
とう性の導電性透明フィルムを提供することにある。An object of the present invention is to provide a flexible conductive transparent film having excellent transparency and conductivity.
本発明を概説すれば、本発明の第１の発明は導電性透
明フィルムに関する発明であって、可視光領域で透明な
含フッ素ポリイミドフィルムにITO膜が形成されている
ことを特徴とする。In general, the present invention relates to a conductive transparent film, and is characterized in that an ITO film is formed on a fluorine-containing polyimide film that is transparent in a visible light region.
そして、本発明の第２の発明は高導電性透明フィルム
の製造方法に関する発明であって、可視光領域で透明な
ポリイミドフィルムにITO膜を形成して高導電性透明フ
ィルムを製造するに当り、該ポリイミドフィルムに高温
でエレクトロン サイクロトロン レゾナンス スパッ
タをして該ITO膜の形成させることを特徴とする。And the second invention of the present invention is an invention relating to a method for producing a highly conductive transparent film, and in forming an ITO film on a transparent polyimide film in a visible light region to produce a highly conductive transparent film, The polyimide film is subjected to electron cyclotron resonance sputtering at a high temperature to form the ITO film.
本発明者らは、透明性を維持しながら導電性を向上さ
せる方法について種々検討した結果、ITO膜の形成に当
り、耐熱性の優れた透明ポリイミドを利用し、できるだ
け高い温度で処理を行うこと、特にエレクトロン サイ
クロトロン レゾナンス（以下、ECRと略記する）スパ
ッタでITO膜を作製することにより、導電性を非常に高
くし得ることを見出した。The present inventors have conducted various studies on a method of improving conductivity while maintaining transparency, and found that in forming an ITO film, a transparent polyimide having excellent heat resistance was used, and treatment was performed at a temperature as high as possible. In particular, it has been found that the conductivity can be made very high by forming an ITO film by electron cyclotron resonance (hereinafter abbreviated as ECR) sputtering.
本発明における透明性フィルムとしては、例えば下記
の構造式〔Ｉ〕、〔II〕、〔III〕及び〔IV〕： で表されるポリイミドフィルムがある。As the transparent film in the present invention, for example, the following structural formulas [I], [II], [III] and [IV]: There is a polyimide film represented by
それにITO膜を形成する場合、前述のように、高温で
実施するほど、導電性が向上することを見出した。その
具体的温度についてみると、その上限は、使用するポリ
イミドフィルムの耐熱性限界であり、下限は所望の導電
性が得られる温度であって、好ましくは200〜400℃の範
囲内である。このような高温加熱処理においては、従来
のPETフィルムは当然熱的に耐えられず、使用できな
い。そして、この高温処理を、単に加熱処理でなく、EC
Rスパッタで行うと、透明性に悪影響を与えることな
く、導電性が更に向上することを見出した。As described above, it has been found that the conductivity is improved as the temperature is increased when an ITO film is formed. As for the specific temperature, the upper limit is the heat resistance limit of the polyimide film used, and the lower limit is the temperature at which the desired conductivity is obtained, and is preferably within the range of 200 to 400 ° C. In such a high-temperature heat treatment, the conventional PET film cannot naturally be used thermally and cannot be used. And this high temperature treatment is not simply a heat treatment,
It has been found that conductivity is further improved by performing R sputtering without adversely affecting transparency.
以下、実施例により、本発明の導電性透明フィルム及
びその製造方法について詳細に説明するが、本発明はこ
れらの実施例に限定されるものではない。Hereinafter, the conductive transparent film of the present invention and the method for producing the same will be described in detail with reference to Examples, but the present invention is not limited to these Examples.
実施例１ 透明フィルムとして前記構造式〔Ｉ〕で表されるポリ
イミドのフィルムを用いた。このポリイミドフィルム
は、ピロメリット酸二無水物と2,2′−ビス（トリフル
オロメチル）−4,4′−ジアミノビフェニルを反応させ
て得たポリアミック酸溶液をシリコン基板上にキャスト
後、窒素雰囲気中70℃で２時間、200℃で１時間、300℃
で１時間加熱処理することにより作製した（ポリアミッ
ク酸溶液の製造は、先願である特願平１−71737号明細
書の実施例に示す方法によった）。次に、ECRスパッタ
装置を用い、４×104Paの真空中で、厚さ約40μｍのポ
リイミドフィルムに厚さ約1500ÅのITO膜を形成した。
このとき、ITO膜形成中は、ポリイミドフィルムを300℃
に保持した。得られた導電性透明フィルムの特性を後記
表１に他の例と共に示す。このフィルムは透明性、導電
性が共に良好であった。Example 1 A polyimide film represented by the above structural formula [I] was used as a transparent film. This polyimide film is prepared by casting a polyamic acid solution obtained by reacting pyromellitic dianhydride with 2,2'-bis (trifluoromethyl) -4,4'-diaminobiphenyl on a silicon substrate, and then applying a nitrogen atmosphere. Medium 70 ° C for 2 hours, 200 ° C for 1 hour, 300 ° C
(The production of the polyamic acid solution was carried out according to the method described in the example of Japanese Patent Application No. 1-71737, which was a prior application). Next, using an ECR sputtering apparatus, an ITO film having a thickness of about 1500 ° was formed on a polyimide film having a thickness of about 40 μm in a vacuum of 4 × 10 4 Pa.
At this time, during the formation of the ITO film, the polyimide film is heated to 300 ° C.
Held. The properties of the obtained conductive transparent film are shown in Table 1 below together with other examples. This film had good transparency and conductivity.
実施例２ 透明フィルムとして前記構造式〔II〕で表されるポリ
イミドのフィルムを用いた。このポリイミドフィルム
は、2,2−ビス（3,4−ジカルボキシフェニル）−ヘキサ
フルオロプロパン二無水物と2,2′−ビス（トリフルオ
ロメチル）−4,4′−ジアミノビフェニルを反応させて
得たポリアミック酸溶液をシリコン基板上にキャスト
後、窒素雰囲気中で実施例１と同様の熱処理を行うこと
により作製した（ポリアミック酸溶液の製造は、前記特
願平１−71737号明細書の実施例に示す方法によっ
た）。次に、実施例１と同様の操作により、厚さ約65μ
ｍのポリイミドフィルムに厚さ約1800ÅのITO膜を形成
した。得られた導電性透明フィルムの特性を表１に示
す。このフィルムはと透明性、導電性が共に良好であっ
た。Example 2 A polyimide film represented by the above structural formula [II] was used as a transparent film. This polyimide film is prepared by reacting 2,2-bis (3,4-dicarboxyphenyl) -hexafluoropropane dianhydride with 2,2'-bis (trifluoromethyl) -4,4'-diaminobiphenyl. The resulting polyamic acid solution was cast on a silicon substrate, and then subjected to the same heat treatment as in Example 1 in a nitrogen atmosphere (the polyamic acid solution was produced by the method described in the specification of Japanese Patent Application No. 1-71737). According to the method shown in the example). Next, the same operation as in Example 1 was performed to a thickness of about 65 μm.
An about 1800-mm-thick ITO film was formed on a m-th polyimide film. Table 1 shows the properties of the obtained conductive transparent film. This film was excellent in both transparency and conductivity.
実施例３ 透明フィルムとして前記構造式〔III〕で表されるポ
リイミドのフィルムを用いた。このポリイミドは、商品
名SIXEF−44（ヘキスト社）として知られるものである
が、ポリイミドフィルムは、2,2−ビス（3,4−ジカルボ
キシフェニル）−ヘキサフルオロプロパン二無水物と2,
2−ビス（４−アミノフェニル）ヘキサフルオロプロパ
ンを反応させて得たポリアミック酸溶液をシリコン基板
上にキャスト後、窒素雰囲気中で実施例１と同様の熱処
理を行うことにより作製した（ポリアミック酸溶液の製
造は、前記特願平１−71737号明細書の実施例に示す方
法によった）。次に、実施例１と同様の操作により、厚
さ約60μｍのポリイミドフィルムに厚さ約1600ÅのITO
膜を形成した。ただし、ITO膜形成中におけるポリイミ
ドフィルムの温度は250℃にした。得られた導電性透明
フィルムの特性を表１に示す。このフィルムは透明性、
導電性が共に良好であった。Example 3 A polyimide film represented by the above structural formula [III] was used as a transparent film. This polyimide is known as trade name SIXEF-44 (Hoechst), but the polyimide film is 2,2-bis (3,4-dicarboxyphenyl) -hexafluoropropane dianhydride and 2,2
A polyamic acid solution obtained by reacting 2-bis (4-aminophenyl) hexafluoropropane was cast on a silicon substrate, and then subjected to the same heat treatment as in Example 1 in a nitrogen atmosphere (polyamic acid solution Was produced according to the method described in the example of the specification of Japanese Patent Application No. 1-71737. Next, an ITO film having a thickness of about 1600 mm was formed on a polyimide film having a thickness of about 60 μm by the same operation as in Example 1.
A film was formed. However, the temperature of the polyimide film during the formation of the ITO film was 250 ° C. Table 1 shows the properties of the obtained conductive transparent film. This film is transparent,
Both conductivity were good.
実施例４ 透明フィルムとして前記構造式〔IV〕で表されるポリ
イミドのフィルムを用いた。このポリイミドは、商品名
SIXEF−33（ヘキスト社）として知られるものである
が、ポリイミドフィルムは、2,2−ビス（3,4−ジカルボ
キシフェニル）−ヘキサフルオロプロパン二無水物と2,
2−ビス（３−アミノフェニル）ヘキサフルオロプロパ
ンを反応させて得たポリアミック酸溶液をシリコン基板
上にキャスト後、窒素雰囲気中で実施例１と同様の熱処
理を行うことにより作製した（ポリアミック酸溶液の製
造は、前記特願平１−71737号明細書の実施例に示す方
法と同様の方法によった）。次に、実施例３と同様の操
作により、厚さ約70μｍのポリイミドフィルムに厚さ約
1600ÅのITO膜を形成した。得られた導電性透明フィル
ムの特性を表１に示す。このフィルムは透明性、導電性
が共に良好であった。Example 4 A polyimide film represented by the above structural formula [IV] was used as a transparent film. This polyimide is a trade name
Known as SIXEF-33 (Hoechst), the polyimide film comprises 2,2-bis (3,4-dicarboxyphenyl) -hexafluoropropane dianhydride and 2,2-bis (3,4-dicarboxyphenyl) -hexafluoropropane dianhydride.
A polyamic acid solution obtained by reacting 2-bis (3-aminophenyl) hexafluoropropane was cast on a silicon substrate, and then subjected to the same heat treatment as in Example 1 in a nitrogen atmosphere (polyamic acid solution). Was manufactured by the same method as the method described in the example of Japanese Patent Application No. 1-71737. Next, in the same manner as in Example 3, a polyimide film having a thickness of about 70 μm was
A 1600 mm thick ITO film was formed. Table 1 shows the properties of the obtained conductive transparent film. This film had good transparency and conductivity.
比較例１ 実施例で作製した厚さ約４μｍのポリイミドフィルム
に、実施例１と同様の操作により、厚さ約1500ÅのITO
膜を形成した。ただし、実施例１とは異なり、ITO膜形
成中のポリイミドフィルムの温度を100℃とした。得ら
れた導電性透明フィルムの特性を表１に示す。このフィ
ルムは透明性は良好てあったが、導電性は実施例１のフ
ィルムより劣っていた。Comparative Example 1 An ITO film having a thickness of about 1500 mm was formed on the polyimide film having a thickness of about 4 μm prepared in the example by the same operation as in the example 1.
A film was formed. However, unlike Example 1, the temperature of the polyimide film during the formation of the ITO film was set to 100 ° C. Table 1 shows the properties of the obtained conductive transparent film. This film had good transparency, but was inferior in conductivity to the film of Example 1.
比較例２ 実施例２で作製した厚さ約65μｍのポリイミドフィル
ムに、比較例１と同様の操作により、厚さ約1800ÅのIT
O膜を形成した。得られた導電性透明フィルムの特性を
表１に示す。このフィルムは透明性は良好であったが、
導電性は実施例２のフィルムより劣っていた。Comparative Example 2 An about 1800 mm thick IT film was formed on the polyimide film having a thickness of about 65 μm prepared in Example 2 by the same operation as in Comparative Example 1.
An O film was formed. Table 1 shows the properties of the obtained conductive transparent film. This film had good transparency,
The conductivity was inferior to the film of Example 2.
比較例３ 実施例３で作製した厚さ約60μｍのポリイミドフィル
ムに、比較例１と同様の操作により、厚さ約1600ÅのIT
O膜を形成した。得られた導電性透明フィルムの特性を
表１に示す。このフィルムは透明性は良好であったが、
導電性は実施例３のフィルムより劣っていた。Comparative Example 3 An about 1600 mm thick IT film was formed on the polyimide film having a thickness of about 60 μm prepared in Example 3 by the same operation as in Comparative Example 1.
An O film was formed. Table 1 shows the properties of the obtained conductive transparent film. This film had good transparency,
The conductivity was inferior to the film of Example 3.
比較例４ 実施例４で作製した厚さ約70μｍのポリイミドフィル
ムに、比較例１と同様の操作により、厚さ約1600ÅのIT
O膜を形成した。得られた導電性透明フィルムの特性を
表１に示す。このフィルムは透明性は良好であったが、
導電性は実施例４のフィルムより劣っていた。Comparative Example 4 An approximately 1600 mm thick IT film was formed on the polyimide film having a thickness of about 70 μm prepared in Example 4 by the same operation as in Comparative Example 1.
An O film was formed. Table 1 shows the properties of the obtained conductive transparent film. This film had good transparency,
The conductivity was inferior to the film of Example 4.
比較例５ 厚さ約100μｍのPETフィルムに、比較例１と同様の操
作により、厚さ約500ÅのITO膜を形成した。得られた導
電性透明フィルムの特性を表１に示す。このフィルムは
透明性は良好であったが、導電性は上記実施例のいずれ
よりも劣っていた。しかし、PETフィルムに従来法でITO
膜を蒸着した市販品に比べると、表面抵抗が1/2以下
で、市販品より導電性が明らかに優れていた。Comparative Example 5 An ITO film having a thickness of about 500 ° was formed on a PET film having a thickness of about 100 μm by the same operation as in Comparative Example 1. Table 1 shows the properties of the obtained conductive transparent film. This film had good transparency but poorer conductivity than any of the above examples. However, the conventional method of adding ITO film to PET film
The surface resistance was 品 or less compared to the commercial product on which the film was deposited, and the conductivity was clearly superior to the commercial product.
これらの結果から、ポリイミドフィルムを高温に保持
した状態で、特に好ましくはECRスパッタによりITO膜を
形成した本発明の導電性透明フィルムは透明性、導電性
が共に良好であることが明らかになった。 From these results, it was revealed that the conductive transparent film of the present invention, in which the ITO film was formed by ECR sputtering particularly preferably while maintaining the polyimide film at a high temperature, had good transparency and conductivity. .
以上説明したように、本発明の導電性透明フィルム
は、従来の導電性透明フィルムに比べ、導電性が優れて
いるという利点があるため、透明性、導電性が共に優れ
た耐熱性、可とう性を有する導電性透明フィルムを提供
することができる。As described above, the conductive transparent film of the present invention has the advantage of being superior in conductivity as compared with a conventional conductive transparent film, and therefore has excellent heat resistance and transparency, both of which have excellent transparency and conductivity. The conductive transparent film having the property can be provided.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 山本 二三男 東京都千代田区内幸町１丁目１番６号 日本電信電話株式会社内 (72)発明者 松浦 武利 東京都千代田区内幸町１丁目１番６号 日本電信電話株式会社内 (72)発明者 久保田 英志 東京都品川区西五反田１丁目11番８号 株式会社アフテイ内 (56)参考文献 特開 昭63−232205（ＪＰ，Ａ) 特開 昭62−222518（ＪＰ，Ａ) 特開 昭60−121606（ＪＰ，Ａ) 特開 平２−251564（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) C23C 14/00 - 14/58 C08L 79/08────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Fumio Yamamoto 1-1-6 Uchisaiwaicho, Chiyoda-ku, Tokyo Nippon Telegraph and Telephone Corporation (72) Takeshi Matsuura 1-1-6 Uchisaiwaicho, Chiyoda-ku, Tokyo Japan Telegraph and Telephone Co., Ltd. (72) Inventor Eiji Kubota 1-11-8 Nishigotanda, Shinagawa-ku, Tokyo Aftei Co., Ltd. (56) References JP-A-63-232205 (JP, A) JP-A-62-222518 (JP, A) JP-A-60-121606 (JP, A) JP-A-2-251564 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) C23C 14/00-14 / 58 C08L 79/08
Claims (2)
され、かつ作製時に300℃の加熱処理工程を経た可視光
領域で透明な含フッ素ポリイミドフィルムにインジウム
・スズ酸化物膜が形成されており、かつ該インジウム・
スズ酸化物膜の形成時の温度が300℃であることを特徴
とする導電性透明フィルム。 An indium-tin oxide film is formed on a fluorine-containing polyimide film which is represented by the following structural formula (I) or (II) and which has been subjected to a heat treatment step at 300 ° C. during manufacture and is transparent in the visible light region. Is formed and the indium
A conductive transparent film, wherein the temperature at the time of forming the tin oxide film is 300 ° C.
され、かつ作製時に300℃の加熱処理工程を経た可視光
領域で透明な含フッ素ポリイミドフィルムにインジウム
・スズ酸化物膜を形成して導電性透明フィルムを製造す
るに当り、該ポリイミドフィルムに300℃の温度でエレ
クトロン サイクロトロン レゾナンス スパッタをし
て該インジウム・スズ酸化物膜を形成させることを特徴
とする導電性透明フィルムの製造方法。 2. An indium tin oxide film, which is represented by the following structural formula (I) or (II) and has been subjected to a heat treatment step at 300 ° C. during preparation and which is transparent in the visible light region and is transparent to a fluorinated polyimide film. In producing the conductive transparent film, the polyimide film is subjected to electron cyclotron resonance sputtering at a temperature of 300 ° C. to form the indium tin oxide film. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2073290A JP2823931B2 (en) | 1990-03-26 | 1990-03-26 | Conductive transparent film and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2073290A JP2823931B2 (en) | 1990-03-26 | 1990-03-26 | Conductive transparent film and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03274256A JPH03274256A (en) | 1991-12-05 |
| JP2823931B2 true JP2823931B2 (en) | 1998-11-11 |
Family
ID=13513873
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2073290A Expired - Fee Related JP2823931B2 (en) | 1990-03-26 | 1990-03-26 | Conductive transparent film and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2823931B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006090448A1 (en) * | 2005-02-23 | 2006-08-31 | Jsr Corporation | Process for producing transparent conductive laminate, and touch panel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7550194B2 (en) * | 2005-08-03 | 2009-06-23 | E. I. Du Pont De Nemours And Company | Low color polyimide compositions useful in optical type applications and methods and compositions relating thereto |
| KR101688173B1 (en) * | 2011-12-26 | 2016-12-21 | 코오롱인더스트리 주식회사 | Plastic substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60121606A (en) * | 1983-12-05 | 1985-06-29 | コニカ株式会社 | Transparent conductive film |
| JPS62222518A (en) * | 1986-03-24 | 1987-09-30 | 東レ株式会社 | Manufacture of transparent conductive film |
-
1990
- 1990-03-26 JP JP2073290A patent/JP2823931B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006090448A1 (en) * | 2005-02-23 | 2006-08-31 | Jsr Corporation | Process for producing transparent conductive laminate, and touch panel |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03274256A (en) | 1991-12-05 |
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