JPH11170420A - Transparent conductive film and its production - Google Patents

Transparent conductive film and its production

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Publication number
JPH11170420A
JPH11170420A JP34816197A JP34816197A JPH11170420A JP H11170420 A JPH11170420 A JP H11170420A JP 34816197 A JP34816197 A JP 34816197A JP 34816197 A JP34816197 A JP 34816197A JP H11170420 A JPH11170420 A JP H11170420A
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conductive film
transparent conductive
electroless plating
paste
transparent
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JP34816197A
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Japanese (ja)
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JP3363083B2 (en )
Inventor
Yasuo Kubo
Tetsuya Nakabeppu
Toshiharu Yoshikawa
哲也 中別府
泰生 久保
逸治 吉川
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Sumitomo Osaka Cement Co Ltd
住友大阪セメント株式会社
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Abstract

PROBLEM TO BE SOLVED: To provide a transparent conductive film in which reflection by a metallic fine particle and the degree of metallic luster are little, and to provide a method for producing the transparent conductive film which is easily produced at a low cost without necessitating a complex process.
SOLUTION: The transparent conductive film consists of both a metallic ultrafine particle catalyst layer formed into a prescribed pattern on the surface of a transparent substrate and a metallic layer 7 formed on the metallic ultrafine particle catalyst layer. The transparent conductive film is constituted so as to form the transparent conductive metallic layer 7 on only a pattern printing part by performing pattern printing by paste 5 containing an electroless plating catalyst 1 on the surface of the transparent substrate and performing electroless plating treatment on the electroless plating catalyst 1 applied to the pattern printing.
COPYRIGHT: (C)1999,JPO

Description

【発明の詳細な説明】 DETAILED DESCRIPTION OF THE INVENTION

【0001】 [0001]

【発明の属する技術分野】本発明は、各種表示装置の漏洩電磁波遮蔽膜、各種電子デバイスの透明電極、または透明面状発熱体等として有用な高い透明性と導電性を兼ね備えた透明導電膜およびその製造方法に関する。 The present invention relates to the leakage electromagnetic wave shielding film of various display devices, various electronic devices of the transparent electrode or a transparent conductive film has both a high useful transparency and conductivity as transparent planar heating element or the like, and As a method for manufacturing.

【0002】 [0002]

【従来の技術】従来、CRT,PDP,液晶ディスプレイ等の各種表示装置の漏洩電磁波遮蔽膜、各種電子デバイスの透明電極、または透明面状発熱体等として用いられる透明導電膜には、導電性メッシュを透明基体に貼り付けたもの、金属やITO等の導電性材料を蒸着やスパッタリングによって透明基体上に形成したもの、および特開平 5-16281号公報、特開平 5-283889 号公報に開示されているような透明導電膜があった。 Conventionally, CRT, PDP, leakage electromagnetic wave shielding film of various display devices such as liquid crystal display, the transparent conductive film used as various transparent electrodes of electronic devices or transparent planar heating element or the like, is conductive mesh those stuck on the transparent substrate, which is formed on the conductive material transparent substrate on the deposition or sputtering, such as metal or ITO, and JP 5-16281 and JP been disclosed in Japanese Patent Laid-Open No. 5-283889 there is a transparent conductive film of being.

【0003】これらの公報に開示された透明導電膜の概要は、以下のようにして製造されたものである。 [0003] Summary of the transparent conductive film disclosed in these publications are those prepared in the following manner. 透明基体上に親水性透明樹脂層を形成し、メッキ触媒を吸着させる。 A hydrophilic transparent resin layer formed on a transparent substrate, thereby adsorbing the plating catalyst. 親水性透明樹脂層上に無電解メッキ層を形成する。 Forming an electroless plating layer on a hydrophilic transparent resin layer. 親水性透明樹脂層を黒色にする。 A hydrophilic transparent resin layer to black. 無電解メッキ層上にパターン状のレジスト部を形成する。 Forming a patterned resist portion on the electroless plating layer. 非レジスト部をエッチングにより除去し、パターン化された透明導電膜を形成する。 Non resist portion is removed by etching to form a transparent conductive film which is patterned.

【0004】〔問題点〕前記従来の透明導電膜では、次に示すような多様な問題点があった。 [0004] In [Problems] The conventional transparent conductive film, there was a variety of problems such as the following is. 導電性メッシュを透明基体に貼り付けた場合には、金属製メッシュや、繊維の表面を金属でメッキしたメッシュが用いられる。 When pasting a conductive mesh on the transparent substrate, and a metal mesh, a mesh of the surface of the fiber was plated with a metal is used. それぞれのメッシュは規格の定まったものが用いられるために、メッシュの線幅やピッチを自由に変更することが難しく、特に、線幅を小さくするには限界があり、視認性に劣るものであった。 Each mesh to it has been determined the standard is used, it is difficult to freely change the line width and pitch of the mesh, in particular, to reduce the line width is limited, inferior in visibility It was. また、視認性を高めるためにメッシュ表面を黒色化し、メッシュ表面の反射を抑えようとする場合、工程が煩雑となり、コストが高くなる。 Further, a mesh surface blackened in order to enhance the visibility, when to be suppress the reflection of the mesh surface, process becomes complicated, the cost becomes high.

【0005】金属やITO等の導電性材料を蒸着やスパッタリングによって透明基体上に形成した場合には、金属光沢のため視認性が悪く、また、充分な導電性を得るために膜厚を厚くすると、光が吸収されるため、著しく透過性が悪くなる。 [0005] When forming a conductive material transparent substrate on the deposition or sputtering, such as metal or ITO has poor visibility because of metallic luster, also when increasing the thickness in order to obtain sufficient conductivity because the light is absorbed, significantly permeability is deteriorated. また、ITO等の透明導電性材料の膜では、導電性が低く、用途が限定され、かつ高価である。 Further, the film of transparent conductive material such as ITO, conductive low, applications are limited and expensive.

【0006】公報記載の透明導電膜の場合には、透明基体上に親水性透明樹脂層を形成して製造されたものであるため、製造工程が複雑となり、コスト的にも高価になる。 [0006] When the transparent conductive film of publication, because those prepared by forming a hydrophilic transparent resin layer on a transparent substrate, the manufacturing process becomes complicated and becomes expensive in cost. また、黒色化された親水性樹脂層は、無電解メッキ時に析出した微細金属粒子により遮光されるものであるが、黒色度が充分でなく、金属微粒子による反射があり、また、透明導電膜を斜視した場合には金属光沢色が目立つ。 Further, blackened hydrophilic resin layer is one in which light is shielded by the fine metal particles precipitated during electroless plating, blackness is not sufficient, there is reflected by the metal particles, also a transparent conductive film metallic luster color noticeable when perspective.

【0007】 [0007]

【発明が解決しようとする課題】本発明は前記課題を解決するために成されたものであり、そのための課題は、 [SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, problems therefor,
金属微粒子による反射や金属光沢の程度が少ない透明導電膜、および、複雑な工程を必要とせず製造が容易で安価にできる透明導電膜の製造方法を提供することにある。 Extent less transparent conductive film of reflection and metallic gloss by the metal fine particles, and is to provide a method for producing a transparent conductive film which can be easily manufactured at low cost without requiring a complicated process.

【0008】 [0008]

【課題を解決するための手段】本発明における請求項1 According to the present invention, in order to solve the problems] claim 1
に係る透明導電膜は、透明基体表面に所定のパターンに形成された金属超微粒子触媒層と、この金属超微粒子触媒層上に形成された金属層とからなることを特徴とするものである。 The transparent conductive film according to are those characterized by comprising a transparent metal ultrafine particle catalyst layer formed in a predetermined pattern on the substrate surface, and the metal ultrafine particle catalyst layer which is formed on the metal layer.

【0009】請求項2に係る透明導電膜は、前記所定のパターンが格子状あるいは網目状であることを特徴とする。 [0009] The transparent conductive film according to claim 2, wherein the predetermined pattern is a grid-like or mesh.

【0010】請求項3に係る透明導電膜は、前記所定のパターンの開口率が 60 %以上であることを特徴とする。 [0010] The transparent conductive film according to claim 3, the opening ratio of the predetermined pattern is characterized in that 60% or more.

【0011】請求項4に係る透明導電膜は、前記金属超微粒子触媒層が貴金属超微粒子からなることを特徴とする。 [0011] The transparent conductive film according to claim 4, wherein the metal ultrafine particle catalyst layer is characterized by comprising the noble metal ultrafine particles.

【0012】また、請求項5に係る透明導電膜は、前記金属超微粒子触媒層が貴金属超微粒子と反対の表面電荷をもった粒子に前記貴金属超微粒子を担持させて作製した担持体からなることを特徴とする。 [0012] The transparent conductive film according to claim 5, it is composed of a carrier in which the metal ultrafine particle catalyst layer was prepared by carrying the noble metal ultrafine particles to particles having an opposite surface charge and noble metal ultrafine particles the features.

【0013】請求項6に係る透明導電膜は、前記金属層がAu,Ag,Cu,Cr,Ni,Sn,Zn,Coの1種以上を含有することを特徴とするものである。 [0013] The transparent conductive film according to claim 6, wherein the metal layer is one which Au, Ag, Cu, Cr, Ni, Sn, Zn, characterized by containing one or more Co.

【0014】請求項7に係る透明導電膜の製造方法は、 [0014] The method for producing a transparent conductive film according to claim 7,
透明基体表面上に無電解メッキ触媒を含有するペーストでパターン印刷を行い、このパターン印刷された無電解メッキ触媒上に無電解メッキ処理を施して、パターン印刷部のみに透明導電性の金属層を形成させることを特徴とする。 It performs pattern printing with a paste containing an electroless plating catalyst on a transparent substrate surface, and electroless plating process on the patterns printed electroless plating on the catalyst, a transparent conductive metal layer only on the pattern printing unit characterized in that to form.

【0015】請求項8に係る透明導電膜の製造方法は、 [0015] The method for producing a transparent conductive film according to claim 8,
前記ペーストが前記無電解メッキ触媒として貴金属超微粒子を含有することを特徴とする。 Characterized in that the paste contains precious metal ultrafine particles as the electroless plating catalyst.

【0016】請求項9に係る透明導電膜の製造方法は、 The method for producing a transparent conductive film according to claim 9,
前記ペーストがチキソトロピー性を有することを特徴とする。 The paste is characterized by having a thixotropic property.

【0017】請求項10に係る透明導電膜の製造方法は、前記ペーストが前記無電解メッキ触媒と反対の表面電荷をもった粒子に前記無電解メッキ触媒を担持させて作製した担持体を含有することを特徴とする。 The method for producing a transparent conductive film according to claim 10, comprising a carrier, wherein the paste is prepared by supporting the electroless plating catalyst particles having an opposite surface charge and the electroless plating catalyst it is characterized in.

【0018】請求項11に係る透明導電膜の製造方法は、前記ペーストが黒色顔料を含むものであることを特徴とする。 The method for producing a transparent conductive film according to claim 11, characterized in that the paste is intended to include a black pigment.

【0019】請求項12に係る透明導電膜の製造方法は、前記パターン印刷がスクリーン印刷であることを特徴とする。 The method for producing a transparent conductive film according to claim 12, wherein the pattern printing is a screen printing.

【0020】 [0020]

【発明の実施の形態】以下、本発明の実施の形態を具体的に説明する。 BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, an embodiment of the present invention in detail. ただし、この実施の形態は、発明の趣旨をより良く理解させるため具体的に説明するものであり、特に指定のない限り、発明内容を限定するものではない。 However, this embodiment is intended to explain the purpose of better specifically in order to understand the invention, unless otherwise specified, it is not intended to limit the inventive subject matter.

【0021】〔透明導電膜〕この実施の形態では、スクリーン印刷によりパターン印刷を行って、ガラスまたはプラスチック等の透明基板表面に、所定のパターンを有する無電解メッキ触媒層を形成し、次いで、無電解メッキ処理を施すことによって、無電解メッキ触媒層上に金属層を形成させ、複雑な工程を必要とせずに、容易に、 [0021] In [transparent conductive film] This embodiment, by performing a pattern by a screen printing, on the transparent substrate surface such as glass or plastic, to form an electroless plating catalyst layer having a predetermined pattern, then no by performing electrolytic plating processing, electroless plating catalyst layer to form a metal layer, without the need for complicated steps, easily,
所定のパターンを形成した金属層を有する透明導電膜を製造することができ、この方法によって製造された透明導電膜は、高い導電性と透明性とを兼ね備える。 It is possible to manufacture a transparent conductive film having a metal layer having a predetermined pattern formed, a transparent conductive film produced by this method has both a high conductivity and transparency.

【0022】所定のパターンとしては、格子状、網目状、ストライプ状等に形成することができ、特に、格子状または網目状に形成することが好ましい。 [0022] as a predetermined pattern, a lattice shape, a mesh shape, it can be formed in a stripe shape or the like, in particular, is preferably formed in a grid pattern or mesh. このようにして所定のパターンを形成した金属層を有する透明導電膜では、その開口率を 60 %以上とすることで、CR In this way the transparent conductive film having a metal layer having a predetermined pattern formed, by the opening ratio is 60% or more, CR
T,PDP,液晶ディスプレイ等の各種表示装置における漏洩電磁波遮蔽膜として必要とされる高い透明性を得ることができる。 T, it is possible to obtain PDP, a high transparency required as leakage electromagnetic wave shielding film in various display devices such as liquid crystal display.

【0023】〔無電解メッキ触媒〕使用可能な無電解メッキ触媒としては、Pd,Au,Ag,Pt等の貴金属超微粒子が挙げられる。 [0023] As [electroless plating catalyst] available electroless plating catalyst, Pd, Au, Ag, include noble ultrafine particles such as Pt.

【0024】〔無電解メッキ触媒担持体〕無電解メッキ触媒として、Pd,Au,Ag,Pt等の貴金属超微粒子を用いた場合、無電解メッキ触媒担持体としては、前記無電解メッキ触媒と反対の表面電荷をもった粒子として微細アルミナゲル、シリカゲル等を用いることが好ましい。 [0024] As [electroless plating catalyst carrier] electroless plating catalyst, Pd, Au, Ag, when using a noble metal ultrafine particles such as Pt, as the electroless plating catalyst carrier, and the electroless plating catalyst opposite fine alumina gel as having a surface charge the particles, it is preferable to use silica gel or the like.

【0025】〔ペースト〕パターン印刷を行う場合に用いるペーストは、特に制限はなく、触媒粒子間および触媒粒子と基材との間をそれぞれ結合させるための接着性が良いものが望ましく、その中でも粘度が高いものが好ましい。 The paste used when performing [paste] Pattern printing is not particularly limited, it is desirable that a good adhesion for bonding each between the catalyst particles and between catalyst particles and the substrate, the viscosity among them what is high is preferable. また、分散剤、消泡脱泡剤、リベリング剤等を、適宜、添加することができる。 Furthermore, dispersing agents, defoaming defoaming agent, a Riberingu agent can appropriately be added. ペーストの粘度は 1 The viscosity of the paste 1
0 〜 1000 Pa・sec(10000 〜 1000000cP)、好ましくは 50 〜 500Pa・sec( 50000〜 500000 c 0 ~ 1000 Pa · sec (10000 ~ 1000000cP), preferably 50 ~ 500Pa · sec (50000~ 500000 c
P)とする。 P) and to.

【0026】溶媒としては、沸点が 200℃前後の比較的高い沸点を有する溶媒が用いられ、例えば、テルピネオール、ブチルカルビトール、ブチルカルビトールアセテート、エチルカルビトール、エチルカルビトールアセテート等が好適である。 [0026] As the solvent, a boiling point is used is a solvent having a relatively high boiling point of about 200 ° C., for example, terpineol, butyl carbitol, butyl carbitol acetate, ethyl carbitol, ethyl carbitol acetate or the like is suitable . この場合、溶媒の沸点が低すぎると、ペースト作製時あるいはスクリーン印刷時に溶媒が揮散して、ペーストの性状が変化、あるいはスクリーンマスクのメッシュにペーストが目詰まりし、また、溶媒の沸点が高すぎると、印刷後の乾燥に時間が掛かりすぎる。 In this case, the boiling point of the solvent is too low, the solvent is volatilized during the paste during preparation or screen printing, change the properties of the paste, or paste clogged the mesh of the screen mask and the boiling point of the solvent is too high and, take too long to dry after printing.

【0027】ペースト中に添加する結合剤(バインダー)としては,特に制限はなく、エチルセルロース、ニトロセルロース等のセルロース誘導体系、アクリル系、 [0027] As the binder to be added to the paste (binder) is not particularly limited, ethyl cellulose, cellulose derivative-based, such as nitrocellulose, acrylic,
酢酸ビニル系、PVA系等を用いることができる。 Vinyl acetate, can be used PVA-based or the like.

【0028】結合剤の量は、多いと基材との密着性は増大するが、無電解メッキ触媒が、結合剤中に埋没し、後工程の無電解メッキにおいて金属が析出しなくなる。 The amount of the binder, although the adhesion between the substrate often increases, electroless plating catalyst, buried in the binder, the metal is not deposited in the electroless plating in a subsequent step. また、少なすぎると、ペーストと基材との密着が不充分となり好ましくない。 Also, too little, unfavorably insufficient adhesion between the paste and the substrate. したがって、結合剤の量はペースト印刷、乾燥後、無電解メッキ触媒あるいは同触媒の担持体が皮膜の表面に露出する程度が好ましい。 Accordingly, the amount of the binder paste is printed, dried, the degree to which the bearing member of an electroless plating catalyst or the catalyst is exposed to the surface of the film is preferred.

【0029】ペーストへの要求特性のうち、微細なパターン印刷を行うためのペーストには、チキソトロピー性(揺変性)が必要であり、微細アルミナゲル、シリカゲル等の添加はペーストにその特性を付与することが可能であるため、好ましい。 [0029] Among the properties required of the paste, the paste for performing a fine pattern printing, it is necessary thixotropic (thixotropic), the addition of fine alumina gel, silica gel or the like imparts its properties to the paste since it is possible, preferably.

【0030】ペーストには、無電解メッキ触媒微粒子を無電解メッキ触媒と反対の表面電荷をもった粒子に担持させて作製した担持体を含有させることにより、無電解メッキ触媒を含有するペーストにチキソトロピー性(揺変性)を付与することができ、スクリーン印刷時において、精度の高いパターン形成が可能となる。 [0030] The paste by containing a carrier prepared by supporting an electroless plating catalyst particles to particles having an opposite surface charge and the electroless plating catalyst, thixotropic paste containing an electroless plating catalyst It can impart sex (thixotropic), during screen printing, thereby enabling highly accurate pattern formation.

【0031】したがって、無電解メッキ触媒のペーストへの添加方法としては、ペーストへ直接添加しても構わないが、貴金属超微粒子と反対の表面電荷をもった粒子に貴金属超微粒子を担持させた担持体を、ペースト中に均一に混合し、分散させることが望ましい。 [0031] Therefore, as a method of adding the electroless plating catalyst paste, supported but may be added directly to the paste, which was supported noble metal ultrafine particles to particles having an opposite surface charge and noble metal ultrafine particles the body, uniformly mixed in the paste, it is desirable to disperse.

【0032】例えば、クエン酸で安定化された貴金属コロイド粒子は、表面負電荷を有しているので、表面正荷電のアルミナ微粒子(アルミナゲル)に吸着担持させたものを用い、これをペースト中に混練し、均一に分散させる。 [0032] For example, the noble metal colloidal particles stabilized with citric acid, since they have a surface negative charge, using those adsorbed carried on the surface positively charged alumina particles (alumina gel), which in the paste the kneaded is dispersed homogeneously.

【0033】〔黒色顔料〕無電解メッキ触媒を含有するペーストは、メッキ皮膜の金属光沢による透明基板裏面の反射防止および色ムラや金属色の抑制のため、黒色顔料を含有させることが望ましい。 [0033] [black pigment] paste containing an electroless plating catalyst, for antireflection and color unevenness and metallic color suppression of the transparent substrate backside with a metal luster of the plating film, it is desirable to include a black pigment. この場合の黒色顔料としては、ペースト中に分散容易な粒子径 0.1μm以下の着色力の大きな黒色顔料が好ましい。 As the black pigment in the case, a large black pigment dispersion easy particle size 0.1μm or less of coloring power in the paste is preferred. 例えば、カーボンブラック、Fe 34 ,CuO−Cr 23 ,CuO− For example, carbon black, Fe 3 O 4, CuO- Cr 2 O 3, CuO-
Fe Fe 34 −Mn 23 ,CoO−Fe 23 −Cr 2 3 O 4 -Mn 2 O 3, CoO-Fe 2 O 3 -Cr 2
3などが使用可能である。 Such as O 3 can be used. このうち、特に、カーボンブラックが好ましい。 Among these, in particular, carbon black is preferred.

【0034】〔パターン印刷〕印刷法としては、特に制限しないが、スクリーン印刷法が好適である。 [0034] As [Pattern Printing] printing method is not particularly limited, screen printing method is preferable. スクリーンマスクとしては、成膜後得られる透明導電膜の透明性を維持するため、格子状構造または網目構造を有した開口率 60 %以上、平均開口径が7mm以下、平均開口径/平均線幅≧7としたものを用いることが好ましい。 The screen mask, in order to maintain the transparency of the transparent conductive film obtained after the film formation, lattice-like structure or network structure and has an opening ratio of 60% or more, an average opening diameter of 7mm or less, an average opening diameter / average line width it is preferable to use those with ≧ 7. スキージ走査速度、角度、印圧、スクリーンマスクの乳剤の厚さ、紗の太さ、オープニング等は適宜選択可能である。 Squeegee scanning speed, the angle, the printing pressure, the emulsion of the screen mask thickness, the thickness of the gauze, opening, etc. can be appropriately selected.

【0035】〔無電解メッキ処理〕通常の無電解メッキ浴が使用可能である。 [0035] [electroless plating process] ordinary electroless plating bath can be used. 使用できる金属としてはAu,A The metal can be used Au, A
g,Cu,Cr,Ni,Su,Zn,Coの一種以上を含有する金属である。 g, a metal containing Cu, Cr, Ni, Su, Zn, and one or more kinds of Co. これらの金属の導電性の点からは、Ag,Cu,Au,Ni等が好ましい。 In terms of electrical conductivity of these metals, Ag, Cu, Au, Ni, etc. are preferable. 例えば、無電解Cuメッキ浴、無電解Ni−Pメッキ浴、無電解N For example, an electroless Cu plating bath, an electroless Ni-P plating bath, an electroless N
i−Bメッキ浴、無電解Auメッキ浴等が使用可能である。 i-B plating bath, an electroless Au plating bath or the like can be used.

【0036】無電解メッキ処理においては、先の工程で無電解メッキ触媒を含有するペーストをパターン印刷しているので、無電解メッキ時にはパターン印刷した部分のみに金属の析出が起こり、高開口率の、即ち高い光透過性を有した高導電性の皮膜を得ることができる。 [0036] In the electroless plating, since the paste pattern printing containing an electroless plating catalyst in the preceding step, at the time of electroless plating occurs only on the metal deposition portion pattern printing, a high aperture ratio , i.e. it is possible to obtain a highly conductive film having a high light transmittance.

【0037】〔パターン状透明導電膜の形成〕無電解メッキ触媒を担持させた担持体を用いて透明導電膜を形成させる場合について概略例示すると、図1(イ)〜 [0037] In summary illustrated for the case of forming a transparent conductive film electroless plating catalyst with the carrier having supported thereon [patterned transparent conductive film formed of], FIG. 1 (a) to
(ホ)に示すように、無電解メッキ触媒1を担持体2に担持させてバインダー3とともに溶剤4に混合して分散させたペースト5を調製し(イ)、スクリーン印刷によってペースト5を基板6の表面上にパターン印刷し(ロ)、印刷後に乾燥させて溶媒を揮散させ(ハ)、基板6の表面にバインダー3により担持体2を結合した所定形状のパターンを形成させるとともに、無電解メッキ触媒1を担持体2の表面に露出させる(ニ)、さらに、 As shown in (e), the electroless plating catalyst 1 by supporting the carrier 2 a paste 5 was dispersed by mixing in a solvent 4 prepared with a binder 3 (b), a substrate paste 5 by screen printing 6 pattern printed on the surface of (ii), dried after printing solvent to volatilize and (c), together to form a pattern having a predetermined shape that combines the carrier 2 by a binder 3 on the surface of the substrate 6, the electroless plating exposing the catalyst 1 to the surface of the carrier 2 (d), further,
無電解メッキ処理を行って無電解メッキ触媒1を起点として金属を析出させ、基板6の表面に格子状または網目状のパターンを有する金属層7を形成させる。 Metal to deposit the electroless plating catalyst 1 by performing an electroless plating process as a starting point, to form a metal layer 7 having a lattice-like or net-like pattern on the surface of the substrate 6.

【0038】また、この工程中でペースト5に無電解メッキ触媒を直接に混入させても良い。 Further, it may be directly by mixing an electroless plating catalyst paste 5 in this process. その場合には、バインダーによって図中の担持体の代わりに触媒が基板6 In that case, the catalyst instead of carrier in the figure by the binder board 6
に直接結合されていることになる。 It will be coupled directly.

【0039】〔成膜後の透明導電膜〕このようにして、 [0039] [transparent conductive film after film formation] in this way,
無電解メッキ触媒含有印刷ペーストをパターン印刷すると、印刷部のみ選択的に無電解メッキがなされるので、 When the electroless plating catalyst-containing printing paste pattern printing, selectively only the printing unit so electroless plating is performed,
得られる透明導電膜の特性はパターン印刷に大きく影響される。 Properties of the transparent conductive film obtained is greatly affected by the pattern printing. メッキ皮膜(金属皮膜)部分は殆ど光透過性が期待できないので開口部を設けて、透明性を確保する。 Since plating film (metal film) portion can not be expected almost optically transparent is provided an opening, to ensure transparency.
したがって、開口率は透明性に大きく影響する。 Accordingly, the aperture ratio greatly affects the transparency. このため、開口率を 60 %以上とすることで必要な透明性を確保する。 Therefore, to ensure the necessary transparency by the aperture ratio of 60% or more.

【0040】開口パターンは、例えば格子状(網目状) The aperture pattern, for example grid-like (reticulated)
の構造が挙げられ、平均開口径/平均線幅≧7とすることで、開口率(光透過率)60%以上を確保できる。 Structure are exemplified in, that the average opening diameter / average line width ≧ 7, the aperture ratio (transmittance) can be secured more than 60%. 開口ピッチは大きいと格子状(網目状)構造が目立ち、視認性が悪化するから、開口ピッチは細かい程好ましく、1 Opening pitch is as large as the grid-like (like network) structure noticeable, since visibility is deteriorated, the opening pitch is preferably finer, 1
mm以下が好ましい。 mm or less is preferable.

【0041】透明導電膜の厚みは、特に限定されないが、厚くなると視認性が悪くなり、即ち、視野角が狭くなる。 The thickness of the transparent conductive film is not particularly limited, the visibility is deteriorated and becomes thicker, i.e., the viewing angle is narrowed. 無電解メッキで得られる金属膜の比抵抗は一般に Specific resistance of the metal film obtained by electroless plating is generally
10 -6 〜 10 -5 Ω・cmであり、開口率 60 %の場合、 A 10 -6 ~ 10 -5 Ω · cm , when the aperture ratio of 60%,
透明導電膜の面抵抗は厚さ1μmで1Ω/□以下の低抵抗のものが得られる。 Surface resistance of the transparent conductive film is 1 [Omega / □ the following a low resistance is obtained with a thickness of 1 [mu] m. したがって、無電解メッキによって得られる金属膜の厚みは、数μm以下で充分であり、 Therefore, the thickness of the metal film obtained by electroless plating is sufficient several μm or less,
従来品と比較して薄膜化が可能となり、視野角の広角化、視認性の向上が達成できる。 Compared to conventional products enables thin, wide angle viewing angle, improvement of visibility can be attained.

【0042】成膜後の透明導電膜に含有させた黒色顔料の効果は、メッキ皮膜の金属光沢による透明基板裏面(透明基体側から透視した場合の面)の反射を防止することができ、メッキによる析出金属皮膜の透明基板裏面の色ムラ抑制および金属色呈示抑制ができる。 The effect of the black pigment is contained in the transparent conductive film after film formation, it is possible to prevent reflection of the transparent substrate back surface by the metallic luster of the plating film (the surface when viewed through the transparent substrate side), plating It can precipitate the transparent substrate rear surface of the color unevenness suppression and metallic color presentation suppression of metal coating by.

【0043】その他、パターン形成金属層と組み合わせて使用することのできる皮膜には、 パターン状金属層上へのAG(防眩)膜、パターン状金属上あるいは裏面へのNIR(近赤外線)遮蔽膜、 [0043] Other, the coatings can be used in combination with patterned metal layer, AG (anti-glare) layer to patterned metal layer, NIR (near infrared) shielding layer to patterned metal on or back surface ,
裏面へのAR(反射防止)膜等がある。 It is AR (antireflection) film or the like on the back.

【0044】 [0044]

【実施例】〔第1実施例〕 (パラジウムコロイドの作製)精製水 89 重量部に塩化パラジウム 1重量部を溶解し、さらにクエン酸三ナトリウム 10 重量部を溶解して均一に攪拌した後、水素化ホウ素ナトリウム 0.01重量部を添加して塩化パラジウムを還元させ、クエン酸で安定、保護コロイド化されたパラジウムコロイドを得た。 EXAMPLES dissolving First Embodiment] (Preparation of palladium colloid) 1 part by weight of palladium chloride in purified water 89 parts by weight, after uniformly stirring and further dissolving trisodium citrate 10 parts by weight, the hydrogen sodium borohydride 0.01 parts by weight by reducing palladium chloride added, stable with citric acid to give the protected colloid palladium colloid. その後、限外濾過により濃縮脱塩を行い、パラジウム 0.5重量部を含有するパラジウムコロイドを得た。 Thereafter, the concentrated and desalted by ultrafiltration, to obtain a palladium colloid containing palladium 0.5 parts by weight.

【0045】(印刷用ペーストの作製)上記パラジウムコロイド 10 重量部に適量の精製水を加え、この希薄パラジウムコロイド溶液に日本アエロゾル製アルミナエアロゾルAl 23 −C、 10 重量部を添加懸濁させる。 [0045] (Preparation of printing paste) a suitable amount of purified water was added to the palladium colloid 10 parts by weight, the dilute palladium colloid solution Nippon Aerosol alumina aerosol Al 2 O 3 -C, is added suspended 10 parts by weight .
パラジウムコロイドはクエン酸で安定化されている為、 Since the palladium colloid which is stabilized with citric acid,
表面負荷電のコロイドであり、またアルミナゾルは逆に表面正荷電を示す為、懸濁液中で静電的に吸着、ヘテロ凝集を起こす。 A colloid surface negative charge, also alumina sol for showing the surface positively charged Conversely, electrostatically attracted in suspension, causing heteroaggregation. これを濾過により分離し、乾燥、解砕することにより、パラジウムコロイドを担持したアルミナゲルを得る。 Which was separated by filtration, dried, and pulverized to obtain an alumina gel carrying palladium colloid. このパラジウムコロイド担持アルミナゲル The palladium colloid-supported alumina gel
7重量部と 10 %エチルセルローステルピネオール溶液 7 parts by weight and 10% ethyl cellulose terpineol solution
30 重量部を3本ロールミルを用いて均一に混練し、分散させることにより印刷ペーストを作製した。 30 parts by weight were uniformly kneaded by using a three-roll mill, to prepare a printing paste by dispersing. 得られたペーストの粘度は 80000cPであった。 The viscosity of the resulting paste was 80000CP.

【0046】(スクリーン印刷)上記により得られたペーストを次に示すスクリーンマスクに載せ、マイクロテック社製スクリーン印刷機MT−750型を用い、3m [0046] (Screen Printing) placed on the following screen mask the resulting paste by the using a Microtec Co. screen printing machine MT-750 type, 3m
m厚( 320×320 (mm))の正方形アクリル板上に印刷を行った。 m was printed on a square acrylic plate having a thickness (320 × 320 (mm)). スクリーンマスクは、枠サイズ 750×750 Screen mask, frame size 750 × 750
(mm)、パターンサイズ 300×300 (mm)、L/S (Mm), the pattern size 300 × 300 (mm), L / S
=50/450 (μm)の格子状(メッシュ状)のパターンを有し、乳剤の厚み: 10 μm、メッシュ開き(ステンレス鋼):325 メッシュ、線径: 16 μm、オープニング: 62 %である。 = Has a pattern of 50/450 ([mu] m) grid (mesh form), emulsion thickness: 10 [mu] m, mesh opening (stainless steel): 325 mesh, wire diameter: 16 [mu] m, opening: 62%. また、スクリーン印刷条件は、印圧:1.6 Kg/cm 2 、スキージ速度:250mm/se In addition, screen printing conditions, the printing pressure: 1.6 Kg / cm 2, the squeegee speed: 250mm / se
c、クリアランス:3.0 mmである。 c, clearance: it is 3.0 mm. 印刷後、室温で 1 After printing, at room temperature for 1
5 分静置後、 60 ℃の乾燥器にて 2時間乾燥を行った。 5 minutes standing, was carried out for 2 hours drying at 60 ° C. of the dryer.
得られた印刷パターンは約L/S=60/440 の格子状のもので、ラインの切れ、印刷ムラ等は特に認められなかった。 The resulting printed pattern is of about L / S = 60/440 grid, cutting lines, uneven printing or the like was observed particularly.

【0047】(無電解Cuメッキ)上記得られたパラジウムコロイド含有ペースト印刷基板を奥野製薬(株)製無電解銅メッキ液(OPC−750シリーズ)中に浸漬させ、20分間、20℃で無電解銅メッキを行った。 [0047] (electroless Cu plating) is immersing the resultant palladium colloid containing paste printed substrate in Okuno Pharmaceutical Co., Ltd. electroless copper plating solution (OPC-750 series), 20 minutes, electroless at 20 ° C. a copper plating was carried out. 攪拌はエアー攪拌で行った。 Stirring was carried out at an air stirring. メッキ処理後に水洗い、乾燥を行った。 Washing after the plating process, drying was carried out.

【0048】得られた膜はラインの平均線幅が約 62 μ The average line width of the obtained film line of about 62 mu
m、平均開口径が 438μmの格子状パターンでメッキ施工表面は黄金色の銅金属光沢、裏面は若干銅金属光沢を示すがほぼ黒色の色調を呈していた。 m, the average opening diameter plated construction surface in a grid-like pattern of 438μm copper metallic luster golden, but the back surface shows a slightly copper metallic luster was exhibited a color tone of almost black. 膜の平均厚みは 8 The average thickness of the film 8
μmである。 It is μm.

【0049】また、この膜の表面抵抗値を三菱化学(株)製ロレスタAP(4端針法)を用いて測定した結果、0.8 Ω/□であった。 [0049] As a result of measurement of a surface resistance value of the film using a Mitsubishi Chemical Corp. Loresta AP (4 Tanhariho) was 0.8 Ω / □. なお、平均線幅は、光学顕微鏡を用い、膜の平面方向の形状を観察し、写真撮影して The average line width, using an optical microscope, to observe the planar direction of the shape of the membrane was photographed
50 カ所の線幅を測定し、平均化して求めた。 The line width of 50 locations were measured, it was determined by averaging.

【0050】膜厚は膜の一部を切り出し、熱硬化型の埋め込み樹脂中に封入し、ミクロトームで断面方向に薄片を切り出し、透過型電子顕微鏡で観察、線部の最高部の厚みを 10 カ所測定し、平均化して求めた。 The thickness cutting out a portion of the film, encapsulated in thermosetting potting, cutting out a thin cross section direction by a microtome, transmission electron microscopic observation, the best part thickness of 10 locations in the line section measured, it was determined by averaging.

【0051】膜の全光線透過率は、膜の一部を切り出し、自動ヘーズメータ(東京電色(株)製)を用いて裏面より測定した結果、72.7%であった。 The total light transmittance of the film, cutting out a portion of the film, results of measurement from the back using an automatic haze meter (manufactured by Tokyo Denshoku Co.), was 72.7%. また、印刷面の裏面の反射率は 4.1%であった。 The reflectance of the rear surface of the printed surface was 4.1%.

【0052】〔第2実施例〕実施例1のペースト作製条件が下記に変更になる以外は同じ。 [0052] except that [Second Embodiment] paste production conditions of Example 1 is changed to below the same. パラジウムコロイド担持アルミナゲル 6.5 重量部 カーボンブラック(三菱化学製 #990 ) 0.5 重量部 10%エチルセルロースのテルピネオール溶液 30 重量部 ペースト粘度 72000 cP Terpineol solution 30 parts by weight paste viscosity of palladium colloid-loaded alumina gel 6.5 parts by weight Carbon black (manufactured by Mitsubishi Chemical Corporation # 990) 0.5 part by weight of 10% ethyl cellulose 72000 cP

【0053】スクリーン印刷条件、使用マスク … 実施例1と同じ 無電解Cuメッキも同様 平均ライン線幅 60 μm 開口径 440 μm 膜厚 7 μm [0053] Screen printing conditions, the same electroless Cu plating and using masks ... Example 1 similarly average line linewidth 60 [mu] m opening size 440 [mu] m thickness 7 [mu] m

【0054】表面抵抗 0.9 Ω/□ 全光線透過率 75.3 % メッキ施工表面は黄金色の銅金属光沢 メッキ施工裏面は金属光沢が全く見られない黒色を呈していた。 [0054] surface resistance 0.9 Omega / □ total light transmittance of 75.3% plating construction surface copper metallic luster plating construction backside golden had a black color which metallic gloss is not observed at all. 裏面の反射率は 2.9% Reflectivity of the back surface is 2.9%

【0055】 [0055]

【0056】 [0056]

【発明の効果】以上のように本発明では、請求項1に係る透明導電膜では、透明基体表面に所定のパターンに形成された金属超微粒子触媒層と、この金属超微粒子触媒層上に形成された金属層とからなるから、最適な透明性と導電性とに調整することができ、高い透明性と導電性とを兼ね備えることができるとともに、金属層による反射や金属光沢の程度を少なくすることができる。 In the present invention as described above, according to the present invention, the transparent conductive film according to claim 1, the ultrafine metal particles catalyst layer formed in a predetermined pattern on a transparent substrate surface, formed on the metal ultrafine particle catalyst layer since consisting of metal layers, can be adjusted to the optimum transparency and conductivity, it is possible to combine a high transparency and conductivity, to reduce the degree of reflection and metallic gloss by the metal layer be able to.

【0057】請求項2に係る透明導電膜では、前記所定のパターンを格子状あるいは網目状としたことにより、 [0057] In the transparent conductive film according to claim 2, by the predetermined pattern has a lattice-like or mesh,
最適な透明性と導電性とを容易に調整する事ができる。 The optimal transparency and conductivity can be easily adjusted.

【0058】請求項3に係る透明導電膜では、所定のパターンの開口率を 60 %以上としたことによって、導電性を有しながら高い透明性を確保することができる。 [0058] In the transparent conductive film according to claim 3, the aperture ratio of the predetermined pattern by the 60% or more, it is possible to secure a high transparency while having conductivity.

【0059】請求項4に係る透明導電膜では、金属超微粒子触媒層が貴金属超微粒子からなるから、無電解メッキにより金属超微粒子触媒層上に金属層を析出させることができ、効果的に金属超微粒子触媒層に金属層を形成させることができる。 [0059] In the transparent conductive film according to claim 4, since the ultrafine metal particles catalyst layer is made of a noble metal ultrafine particles by electroless plating can be deposited a metal layer on the metal ultrafine particle catalyst layer, effectively a metal thereby forming a metal layer on the ultrafine particle catalyst layer.

【0060】請求項5に係る透明導電膜では、金属超微粒子触媒層が貴金属超微粒子と反対の表面電荷をもった粒子に前記貴金属超微粒子を担持させて作製した担持体からなることによって、印刷用ペーストにチキソトロピー性を与え、微細な格子状あるいは網目状等のパターンを形成させることができる。 [0060] In the transparent conductive film according to claim 5, by the metal ultrafine particle catalyst layer is made of a carrier prepared by carrying the noble metal ultrafine particles to particles having an opposite surface charge and noble metal ultrafine particles, printing giving thixotropy to use paste, it is possible to form fine lattice-like or pattern of the mesh, and the like.

【0061】請求項6に係る透明導電膜では、金属層がAu,Ag,Cu,Cr,Ni,Sn,Zn,Coの1 [0061] In the transparent conductive film according to claim 6, the metal layer is Au, Ag, Cu, Cr, Ni, Sn, Zn, Co 1
種以上を含有することによって、良好な導電性を付与することができる。 By including more species, it is possible to impart good electrical conductivity.

【0062】また、請求項7に係る透明導電膜の製造方法では、透明基体表面上に無電解メッキ触媒を含有するペーストでパターン印刷を行い、このパターン印刷された無電解メッキ触媒層上に無電解メッキ処理を施して、 [0062] In the manufacturing method of the transparent conductive film according to claim 7, performs pattern printing with a paste containing an electroless plating catalyst on a transparent substrate surface, free to the pattern printed electroless plating catalyst layer and subjected to electrolytic plating process,
パターン印刷部のみに透明導電性の金属層を形成させたことによって、形成されたパターン状に導電性金属層を形成できて、所定の透明性および導電性を有する透明導電膜を低コストで効果的に形成させることができる。 By having formed the transparent electrically conductive metal layer only on the pattern printing section, and can form a conductive metal layer formed pattern, effect a transparent conductive film having a predetermined transparency and conductivity at a low cost thereby to form.

【0063】請求項8に係る透明導電膜の製造方法では、ペーストが無電解メッキ触媒として貴金属超微粒子を含有するから、無電解メッキ触媒を無電解メッキによるメッキ金属を析出させる核として効果的に機能させることができ、金属層を容易に形成させることができる。 [0063] In the method for producing a transparent conductive film according to claim 8, since paste containing a noble metal ultrafine particles as an electroless plating catalyst, effectively an electroless plating catalyst as nuclei for precipitating a plating metal by electroless plating can be made to function, it is possible to easily form the metal layer.

【0064】請求項9に係る透明導電膜の製造方法では、ペーストがチキソトロピー性を有するために、印刷パターンを微細な形状に形成させることができる。 [0064] In the method for producing a transparent conductive film according to claim 9, in order to paste with thixotropy, the printed pattern can be formed into a fine shape.

【0065】請求項10に係る透明導電膜の製造方法では、ペーストが前記無電解メッキ触媒と反対の表面電荷をもった粒子に前記無電解メッキ触媒を担持させて作製した担持体を含有することにより、ペーストにチキソトロピー性を付与することができ、微細な印刷パターンを実現させることができる。 [0065] In the method for producing a transparent conductive film according to claim 10, which contains a carrier paste was prepared by supporting the electroless plating catalyst particles having an opposite surface charge and the electroless plating catalyst Accordingly, it is possible to impart thixotropy to the paste, it is possible to realize a fine printed pattern.

【0066】請求項11に係る透明導電膜の製造方法では、ペーストが黒色顔料を含むことにより、メッキにより形成した金属層の透明基板裏面側の反射を防止できるとともに色ムラを抑制することができる。 [0066] In the production method of the transparent conductive film according to claim 11, by paste containing a black pigment, it is possible to suppress the color unevenness with the reflection of the transparent substrate rear surface side of the metal layer formed by plating can be prevented .

【0067】請求項12に係る透明導電膜の製造方法では、パターン印刷がスクリーン印刷であることにより、 [0067] In the method for producing a transparent conductive film according to claim 12, by pattern printing is screen printing,
印刷工程を簡略化でき、作業性を向上させることができるとともに低コスト化させることができる。 It simplifies the printing process, it is possible to lower cost it is possible to improve the workability.

【図面の簡単な説明】 BRIEF DESCRIPTION OF THE DRAWINGS

【図1】本発明によるパターン状透明導電膜の形成過程を示す工程説明図であり、(イ)は調整されたペースト、(ロ)は基板上に印刷されたペースト、(ハ)は乾燥中の印刷基板、(ニ)は基板上に形成された無電解メッキ触媒を担持させた担持体のパターン、(ホ)は基板上に形成された透明導電膜をそれぞれ示す側面拡大説明図である。 Figure 1 is a process explanatory views showing a forming process of the patterned transparent conductive film according to the present invention, (a) paste, which is adjusted, (ii) paste printed on a substrate, (c) is in dry print substrate, (d) the pattern of carrier obtained by supporting an electroless plating catalyst formed on the substrate, (e) is a side enlarged view showing each of the transparent conductive film formed on a substrate.

【符号の説明】 DESCRIPTION OF SYMBOLS

1 無電解メッキ触媒 2 担持体 3 バインダー 4 溶媒 5 ペースト 6 基板 7 金属層 1 electroless plating catalyst 2 carrier 3 Binder 4 solvent 5 Paste 6 substrate 7 metal layer

Claims (12)

    【特許請求の範囲】 [The claims]
  1. 【請求項1】透明基体表面に所定のパターンに形成された金属超微粒子触媒層と、この金属超微粒子触媒層上に形成された金属層とからなることを特徴とする透明導電膜。 1. A transparent metal ultrafine particle catalyst layer formed in a predetermined pattern on the substrate surface, a transparent conductive film, characterized in that it consists of a metal ultrafine particle catalyst layer which is formed on the metal layer.
  2. 【請求項2】前記所定のパターンが格子状あるいは網目状であることを特徴とする請求項1記載の透明導電膜。 2. A transparent conductive film according to claim 1, wherein said predetermined pattern is a grid-like or mesh.
  3. 【請求項3】前記所定のパターンの開口率が 60 %以上であることを特徴とする請求項1記載の透明導電膜。 3. A transparent conductive film according to claim 1, wherein the opening ratio of the predetermined pattern is 60% or more.
  4. 【請求項4】前記金属超微粒子触媒層が貴金属超微粒子からなることを特徴とする請求項1記載の透明導電膜。 4. A transparent conductive film according to claim 1, wherein the metal ultrafine particle catalyst layer is characterized by comprising the noble metal ultrafine particles.
  5. 【請求項5】前記金属超微粒子触媒層が貴金属超微粒子と反対の表面電荷をもった粒子に前記貴金属超微粒子を担持させて作製した担持体からなることを特徴とする請求項1記載の透明導電膜。 5. The transparent according to claim 1, characterized in that it consists of carrier prepared by carrying the noble metal ultrafine particles to particles of the metal ultrafine particle catalyst layer having an opposite surface charge and noble metal ultrafine particles conductive film.
  6. 【請求項6】前記金属層がAu,Ag,Cu,Cr,N Wherein said metal layer is Au, Ag, Cu, Cr, N
    i,Sn,Zn,Coの1種以上を含有することを特徴とする請求項1記載の透明導電膜。 i, Sn, Zn, transparent conductive film according to claim 1, characterized by containing one or more Co.
  7. 【請求項7】透明基体表面上に無電解メッキ触媒を含有するペーストでパターン印刷を行い、このパターン印刷された無電解メッキ触媒上に無電解メッキ処理を施して、パターン印刷部のみに透明導電性の金属層を形成させることを特徴とする透明導電膜の製造方法。 7. performs pattern printing with a paste containing an electroless plating catalyst on a transparent substrate surface, and electroless plating process on the patterns printed electroless plating on the catalyst, the transparent conductive only in the pattern printing unit the method for producing a transparent conductive film, characterized in that to form the sex of the metal layer.
  8. 【請求項8】前記ペーストが前記無電解メッキ触媒として貴金属超微粒子を含有することを特徴とする請求項7 8. claims, characterized in that the paste contains precious metal ultrafine particles as the electroless plating catalyst 7
    記載の透明導電膜の製造方法。 The method for producing a transparent conductive film according.
  9. 【請求項9】前記ペーストがチキソトロピー性を有することを特徴とする請求項7に記載の透明導電膜の製造方法。 9. A method for producing a transparent conductive film according to claim 7, wherein the paste is characterized by having a thixotropic property.
  10. 【請求項10】前記ペーストが前記無電解メッキ触媒と反対の表面電荷をもった粒子に前記無電解メッキ触媒を担持させて作製した担持体を含有することを特徴とする請求項7記載の透明導電膜の製造方法。 10. A transparent according to claim 7, characterized in that it contains a carrier prepared by supporting the electroless plating catalyst particles in which the paste with opposite surface charges and the electroless plating catalyst manufacturing method of the conductive film.
  11. 【請求項11】前記ペーストが黒色顔料を含むものであることを特徴とする請求項7記載の透明導電膜の製造方法。 11. The method for producing a transparent conductive film according to claim 7, wherein the paste is intended to include a black pigment.
  12. 【請求項12】前記パターン印刷がスクリーン印刷であることを特徴とする請求項7記載の透明導電膜の製造方法。 12. A method for producing a transparent conductive film according to claim 7, wherein the pattern printing is a screen printing.
JP34816197A 1997-12-17 1997-12-17 Transparent substrate and a method of manufacturing the same Expired - Fee Related JP3363083B2 (en)

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