JPS6332620B2 - - Google Patents
Info
- Publication number
- JPS6332620B2 JPS6332620B2 JP9756484A JP9756484A JPS6332620B2 JP S6332620 B2 JPS6332620 B2 JP S6332620B2 JP 9756484 A JP9756484 A JP 9756484A JP 9756484 A JP9756484 A JP 9756484A JP S6332620 B2 JPS6332620 B2 JP S6332620B2
- Authority
- JP
- Japan
- Prior art keywords
- conductive film
- film
- transparent conductive
- transparent
- films
- 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.)
- Expired
Links
- 239000010408 film Substances 0.000 claims description 43
- 229920006254 polymer film Polymers 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- 238000004544 sputter deposition Methods 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 4
- 238000007733 ion plating Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 238000007738 vacuum evaporation Methods 0.000 claims 1
- 239000003513 alkali Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 5
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000001771 vacuum deposition Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000004695 Polyether sulfone Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229920006393 polyether sulfone Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- HEQWUWZWGPCGCD-UHFFFAOYSA-N cadmium(2+) oxygen(2-) tin(4+) Chemical compound [O--].[O--].[O--].[Cd++].[Sn+4] HEQWUWZWGPCGCD-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229910003437 indium oxide Inorganic materials 0.000 description 1
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 238000005289 physical deposition Methods 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
- Physical Vapour Deposition (AREA)
- Non-Insulated Conductors (AREA)
- Manufacturing Of Electric Cables (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は高分子に金属および/または金属酸化
物を主成分とする導電膜を付与した液晶表示素子
用透明電極に用いる透明導電性フイルムの製造方
法に関するものである。Detailed Description of the Invention [Industrial Field of Application] The present invention relates to a transparent conductive film for use in transparent electrodes for liquid crystal display devices, in which a conductive film containing a metal and/or metal oxide as a main component is applied to a polymer. This relates to a manufacturing method.
従来、透明導電性フイルムは主にポリエステル
フイルムをベースとし、エレクトロルミネツセン
スデイスプレイやエレクトロクロミツクデイスプ
レイの透明電極、デイフロスタ、透明ヒータ等の
面発熱体やタツチパネル等の面スイツチ、赤外線
反射膜、及び透明フレキシブル回路等に広く用い
られてきたが、最近は液晶表示素子への適用も検
討されている。
Conventionally, transparent conductive films are mainly based on polyester films, and are used in transparent electrodes of electroluminescent displays and electrochromic displays, surface heating elements such as day frosters and transparent heaters, surface switches such as touch panels, infrared reflective films, and It has been widely used in transparent flexible circuits and the like, but recently its application to liquid crystal display elements is also being considered.
透明導電性フイルムは、フイルム状の電極を使
用することにより素子を薄型化できる点、生産工
程において取り扱い易く打ち抜き加工等も可能で
ある点、フイルム状素材から連続生産が可能であ
り、コスト面でも有利になるという点より注目さ
れている。 Transparent conductive films can be made thinner by using film-shaped electrodes, are easy to handle during the production process and can be punched out, and can be manufactured continuously from film-shaped materials, making them cost-effective. It is attracting more attention than because it is advantageous.
通常の透明導電性フイルムは、透明性、導電性
にすぐれていることが必要でありさらに加工性と
して耐アルカリ性及び耐擦過傷性が要求される。
耐アルカリ性は、透明導電性フイルムのパターン
加工工程におけるレジスト剥離工程で用いるアル
カリ水溶液によつて導電性不良や断線を生じたり
しないため必要であり、耐擦過傷性は加工工程中
における取扱いにおいて導電性不良や断線が生じ
たりしないために要求される。 Ordinary transparent conductive films are required to have excellent transparency and conductivity, and are also required to have alkali resistance and abrasion resistance in terms of processability.
Alkali resistance is necessary to prevent poor conductivity or disconnection from occurring due to the alkaline aqueous solution used in the resist stripping process in the patterning process of transparent conductive films, and scratch resistance is necessary to prevent poor conductivity from occurring during handling during the processing process. This is required to prevent wire breakage from occurring.
しかし、通常の導電膜形成法である真空蒸着
法、イオンプレーテイング法及びスパツタリング
法では導電膜形成時に気相から固相への相転移の
ため急激な熱放出があり導電膜自体に強い内部応
力がかかる。 However, in the vacuum evaporation method, ion plating method, and sputtering method, which are the usual conductive film formation methods, rapid heat release occurs due to the phase transition from gas phase to solid phase during formation of the conductive film, which causes strong internal stress in the conductive film itself. It takes.
また、導電膜の結晶格子の乱れやピンホールな
どはどうしてもさけられず、これらは耐アルカリ
性及び耐擦過傷性を著しく劣化させる。この点に
関しては、導電膜上にさらにトツプコートを行う
ことによつて改良することが検討されてきた。し
かし従来の方法によるトツプコートは厚みのバラ
ツキが大きくピンホールが多いため、導電性が不
均一になること、およびエツチング工程でトツプ
コートの厚みのバラツキのためにエツチング時間
が不均一になるという重大な欠点をもつておつ
た。 Furthermore, disturbances in the crystal lattice and pinholes of the conductive film cannot be avoided, and these significantly deteriorate alkali resistance and scratch resistance. Regarding this point, attempts have been made to improve this by further applying a top coat on the conductive film. However, the top coat produced by the conventional method has large thickness variations and many pinholes, resulting in non-uniform conductivity, and has serious drawbacks such as non-uniform etching time due to variations in the top coat thickness during the etching process. I had it with me.
本発明は、従来のコーテイング方法では得られ
なかつた耐アルカリ性、耐擦過傷性にすぐれ、か
つ導電性、エツチング時間などに不均一さを生じ
ない透明導電性フイルムを得んとして研究した結
果、プラズマ重合膜をトツプコートとして付与す
れば、要求性能をすべて満足する透明導電性フイ
ルムが得られるとの知見を得、更にこの知見に基
づき種々研究を進めて本発明を完成するに至つた
ものである。
The present invention was developed as a result of research aimed at obtaining a transparent conductive film that has excellent alkali resistance and abrasion resistance, which could not be obtained using conventional coating methods, and that does not cause non-uniformity in conductivity, etching time, etc. It was discovered that a transparent conductive film that satisfies all required properties could be obtained by applying the film as a top coat, and based on this knowledge, various studies were conducted and the present invention was completed.
本発明は導電膜表面にプラズマ重合法によつて
トツプコートを行うことを特徴とする透明導電性
フイルムの製造方法である。
The present invention is a method for producing a transparent conductive film, which is characterized in that the surface of the conductive film is top coated by plasma polymerization.
本発明に用いる高分子フイルムは、真空蒸着、
イオンプレーテイング又はスパツタ法等で導電性
膜を形成する為に耐熱性のある高分子フイルムが
用いられ、ポリイミド、ポリアミドイミド、ポリ
アミド、ポリスルホン、ポリエーテルサルホン、
ポリエーテルケトンをはじめとしポリエステル系
樹脂、芳香族ポリアミド系樹脂等があげられる。
もちろんこれ等はホモポリマー、コポリマーとし
て単独又はブレンドして使用しても何等さしつか
えはない。 The polymer film used in the present invention can be produced by vacuum deposition,
Heat-resistant polymer films are used to form conductive films by ion plating or sputtering methods, and include polyimide, polyamideimide, polyamide, polysulfone, polyethersulfone,
Examples include polyester-based resins, aromatic polyamide-based resins, etc., including polyetherketone.
Of course, these may be used alone or as a blend as homopolymers or copolymers.
又導電性膜素材である金属および/または金属
酸化物としては、金、銀、ジルコニウム、インジ
ウム、錫、チタン等や又は、酸化錫、酸化インジ
ウム、錫−カドミウム酸化物等を使用することが
出来る。 Further, as the metal and/or metal oxide that is the conductive film material, gold, silver, zirconium, indium, tin, titanium, etc., or tin oxide, indium oxide, tin-cadmium oxide, etc. can be used. .
当然該導電性膜を高分子フイルムに付与するに
は、蒸着法、スパツタ法等の物理的堆積法や化学
メツキ法、気相メツキ法等の化学堆積法で、導電
性膜を付与しても何らさしつかえはない。 Of course, in order to apply the conductive film to the polymer film, it is possible to apply the conductive film by physical deposition methods such as vapor deposition or sputtering, or by chemical deposition methods such as chemical plating or vapor phase plating. There's nothing wrong with that.
又これ等の導電性膜を高分子フイルムに付与す
るのに、その密着性等を向上させる為に高分子フ
イルムと導電性膜の間に第3層を形成させたもの
であつても何ら差障りはなく、もしろ高分子フイ
ルムと導電性膜の密着性をあげるということは、
その透明導電性フイルムの可撓性や加工性を向上
させる為に望ましいものである。 Furthermore, when applying these conductive films to a polymer film, there is no difference even if a third layer is formed between the polymer film and the conductive film in order to improve the adhesion, etc. There is no problem, but if you want to improve the adhesion between the polymer film and the conductive film,
This is desirable in order to improve the flexibility and processability of the transparent conductive film.
高分子フイルムに導電性膜を付与したものに、
該導電性膜上にプラズマ法でトツプコートを行
う。 A polymer film with a conductive film added to it,
Top coating is performed on the conductive film using a plasma method.
プラズマ重合は、簡単な構造の有機モノマーを
プラズマ空間に導入し、気相中に生成するラジカ
ル種を該導電性膜上に重合させながら沈着させて
保護層である薄膜を形成させるものであり、有機
モノマーとしては、通常の触媒や光などで重合す
る物質を含めた多くの物質であればよく、例えば
スチレン、メチルメタアクリレート、アクリルニ
トリルやエチレン、プロピレン等のオレフイン系
のものでも良く、単独であつても又は2つ以上の
組合せであつても良い。さらにプラズマ処理に於
ては、有機モノマー単独であつても、これ等の有
機モノマーのキヤリヤーガスとしてアルゴン等の
不活性ガスを用いても良い。 In plasma polymerization, an organic monomer with a simple structure is introduced into a plasma space, and radical species generated in the gas phase are polymerized and deposited on the conductive film to form a thin film as a protective layer. The organic monomer may be any substance, including those that polymerize with ordinary catalysts or light, such as olefins such as styrene, methyl methacrylate, acrylonitrile, ethylene, and propylene; There may be one or a combination of two or more. Furthermore, in the plasma treatment, even if the organic monomer is used alone, an inert gas such as argon may be used as a carrier gas for the organic monomer.
有機モノマーを選択するには、本願発明におい
ては、耐アルカリ性の向上を計る目的から酸に弱
く、アルカリ性に強いものなる様な有機モノマー
を選択することが必要である。この様にして作製
したプラズマ重合膜は、高度に架橋したピンホー
ルのない均質薄膜であり、透明導電性フイルム用
のトツプコートとして、きわめて優れたものであ
る。 In selecting an organic monomer, in the present invention, it is necessary to select an organic monomer that is weak against acids and strong against alkalinity for the purpose of improving alkali resistance. The plasma polymerized film thus produced is a highly crosslinked, homogeneous thin film without pinholes, and is extremely suitable as a top coat for transparent conductive films.
本発明は、プラズマ重合膜の特性であるピンホ
ールのない均質薄膜をトツプコートすることによ
り、従来得られなかつた耐アルカリ性、耐擦過傷
性にすぐれ、かつ高透明性、高導電性を有する透
明導電膜の製造を行うというもので、工業的にき
わめてすぐれたものである。さらにコーテイング
厚の厚みむらがないことから、パターン加工しや
すいすぐれた透明導電性フイルムの製造方法であ
る。
By top-coating a homogeneous thin film without pinholes, which is a characteristic of a plasma polymerized film, the present invention provides a transparent conductive film that has excellent alkali resistance and abrasion resistance, as well as high transparency and high conductivity, which were previously unobtainable. It is an industrially excellent product. Furthermore, since there is no unevenness in the coating thickness, it is an excellent method for producing a transparent conductive film that is easy to pattern.
ポリエーテルサルホンフイルムを基板とし、真
空蒸着法にて厚さ300Åにインジウムを主成分と
する導電膜を形成した。これにスチレンのプラズ
マ重合膜を形成した。放電周波数5KHz放電電力
8w圧力1Torrで1分間プラズマ重合した。膜厚
は400Åだつた。このようにして作製した透明導
電性フイルムはシート抵抗320Ω/□、可視光の
透過率85%、水酸化カリウムの10%水溶液に10分
間浸漬した後のシート抵抗値は320Ω/□でまつ
たく変化しなかつた。このフイルムを水酸化カリ
ウム水溶液に浸漬した後光学顕著鏡で300倍に拡
大してもクラツクはまつたく見られなかつた。
Using a polyether sulfone film as a substrate, a conductive film containing indium as a main component was formed to a thickness of 300 Å using a vacuum evaporation method. A styrene plasma polymerized film was formed on this. Discharge frequency 5KHz discharge power
Plasma polymerization was performed at 8W pressure of 1 Torr for 1 minute. The film thickness was 400 Å. The transparent conductive film produced in this way has a sheet resistance of 320Ω/□, a visible light transmittance of 85%, and a sheet resistance value that changes rapidly at 320Ω/□ after being immersed in a 10% potassium hydroxide aqueous solution for 10 minutes. I didn't. Even after this film was immersed in an aqueous potassium hydroxide solution and magnified 300 times with an optical microscope, no cracks were clearly visible.
また、100g/cm2の荷重をかけたガーゼで五千
回摩擦したが抵抗値の変化はまつたくみられなか
つた。 Furthermore, no change in resistance value was observed even after rubbing 5,000 times with gauze under a load of 100 g/cm 2 .
実施例と同一の条件で導電膜を形成し、かつプ
ラズマ重合膜を形成しなかつた。シート抵抗値は
300Ω/□、可視光の透過率は83%であつた。こ
れを実施例と同じ条件で水酸化カリウム水溶液に
浸漬した。シート抵抗値は500Ω/□となり、光
学顕微鏡で300倍に拡大し観察するとクラツクが
多数発生していた。
A conductive film was formed under the same conditions as in the example, and no plasma polymerized film was formed. The sheet resistance value is
It was 300Ω/□, and the visible light transmittance was 83%. This was immersed in an aqueous potassium hydroxide solution under the same conditions as in the example. The sheet resistance value was 500Ω/□, and when observed under 300x magnification with an optical microscope, many cracks were observed.
また、100g/cm2の荷重をかけたガーゼで五千
回摩擦すると、シート抵抗が10KΩ/□になり、
耐擦過傷性が不良であつた。 Also, when rubbed 5,000 times with gauze with a load of 100g/ cm2 , the sheet resistance becomes 10KΩ/□,
Scratch resistance was poor.
以上の理由で本発明の透明導電性フイルムがす
ぐれている。 For the above reasons, the transparent conductive film of the present invention is excellent.
Claims (1)
テイング法、あるいはスパツタリング法にて金属
および/または金属酸化物の薄膜を導電層として
形成し、さらにプラズマ重合法にてトツプコート
層を形成することを特徴とする透明導電性フイル
ムの製造方法。1 A thin film of metal and/or metal oxide is formed as a conductive layer on a polymer film by vacuum evaporation, ion plating, or sputtering, and a top coat layer is further formed by plasma polymerization. A method for producing a transparent conductive film.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9756484A JPS60242050A (en) | 1984-05-17 | 1984-05-17 | Manufacture of transparent conductive film |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9756484A JPS60242050A (en) | 1984-05-17 | 1984-05-17 | Manufacture of transparent conductive film |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS60242050A JPS60242050A (en) | 1985-12-02 |
JPS6332620B2 true JPS6332620B2 (en) | 1988-06-30 |
Family
ID=14195725
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP9756484A Granted JPS60242050A (en) | 1984-05-17 | 1984-05-17 | Manufacture of transparent conductive film |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS60242050A (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2599176B2 (en) * | 1988-05-02 | 1997-04-09 | オリエント時計 株式会社 | Golden ornaments |
JPH0745708B2 (en) * | 1988-05-02 | 1995-05-17 | オリエント時計株式会社 | Complex mixed multilayer film |
-
1984
- 1984-05-17 JP JP9756484A patent/JPS60242050A/en active Granted
Also Published As
Publication number | Publication date |
---|---|
JPS60242050A (en) | 1985-12-02 |
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