JP2013116992A - 透明導電性フィルム用粘着剤層、粘着剤層付き透明導電性フィルム、透明導電性積層体、およびタッチパネル - Google Patents
透明導電性フィルム用粘着剤層、粘着剤層付き透明導電性フィルム、透明導電性積層体、およびタッチパネル Download PDFInfo
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- JP2013116992A JP2013116992A JP2011265937A JP2011265937A JP2013116992A JP 2013116992 A JP2013116992 A JP 2013116992A JP 2011265937 A JP2011265937 A JP 2011265937A JP 2011265937 A JP2011265937 A JP 2011265937A JP 2013116992 A JP2013116992 A JP 2013116992A
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- transparent conductive
- adhesive layer
- sensitive adhesive
- pressure
- film
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
- C08F265/06—Polymerisation of acrylate or methacrylate esters on to polymers thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F271/00—Macromolecular compounds obtained by polymerising monomers on to polymers of nitrogen-containing monomers as defined in group C08F26/00
- C08F271/02—Macromolecular compounds obtained by polymerising monomers on to polymers of nitrogen-containing monomers as defined in group C08F26/00 on to polymers of monomers containing heterocyclic nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/003—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
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- C09J133/10—Homopolymers or copolymers of methacrylic acid esters
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Abstract
【解決手段】パターニングされた透明導電性薄膜を有する透明導電性フィルムに用いられる粘着剤層であって、前記粘着剤層は、アルキル(メタ)アクリレートを含有するモノマー成分を重合して得られるアクリル系ポリマー100重量部に対し、スチレン系オリゴマーを30〜150重量部含有するアクリル系粘着剤組成物から形成されたものであり、かつ、前記粘着剤層は、屈折率が1.50以上であり、厚さ30μmで測定した場合のヘイズ値が2%以下である。
【選択図】図1
Description
前記粘着剤層は、アルキル(メタ)アクリレートを含有するモノマー成分を重合して得られるアクリル系ポリマー100重量部に対し、スチレン系オリゴマーを30〜150重量部含有するアクリル系粘着剤組成物から形成されたものであり、
かつ、前記粘着剤層は、屈折率が1.50以上であり、
厚さ30μmで測定した場合のヘイズ値が2%以下であることを特徴とする透明導電性フィルム用粘着剤層、に関する。
アクリル系ポリマーおよびスチレン系オリゴマーの重量平均分子量はGPC(ゲルパーミエーションクロマトグラフィー)法の下記条件にて測定した。
カラム(アクリル系ポリマー):東ソー製、G7000HXL−H+GMHXL−H+GMHXL
カラム(スチレン系オリゴマー):東ソー製、GMHR−H+GMHHR+G2000MHHR
カラムサイズ:各7.8mmφ×30cm 計90cm
カラム温度:40℃
流速:0.8mL/min
溶離液:テトラヒドロフラン
溶液濃度:約0.1重量%
注入量:100μL
検出器:示差屈折計(RI)
標準試料:ポリスチレン
データ処理装置:東ソー製,GPC‐8020
JIS K5902に記載の環球法により測定した。
(アクリル系ポリマーの調製)
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、n−ブチルアクリレート100重量部および4−ヒドロキシブチルアクリレート3重量部からなるモノマー成分(1)を加え、さらに重合開始剤として2,2’−アゾビスイソブチロニトリル0.1重量部を酢酸エチル/トルエン=7/3(容量比)に調整した溶剤と共に前記フラスコに仕込み、緩やかに攪拌しながら窒素ガスを導入して1時間窒素置換した。前記溶剤は、溶液中の前記モノマー成分(1)が50重量%になるような割合で加えた。その後、前記フラスコ内の液温を58℃付近に保って8時間重合反応を行い、重量平均分子量90万のアクリル系ポリマー(1)を含有する溶液を得た。ただし、重合反応開始より2時間経過した後に、固形分が40重量%になるよう、酢酸エチルを1時間かけて滴下した。
得られたアクリル系ポリマー(1)を含有する溶液の固形分100重量部に対して、スチレン50重量部および4−ヒドロキシブチルアクリレート2.5重量部からなるグラフトモノマー成分(2)を加え、さらに重合開始剤としてベンゾイルパーオキサイド0.25重量部を酢酸エチルと共に、前記フラスコに投入し、充分に窒素置換した。前記酢酸エチルは、溶液中の前記アクリル系ポリマー(1)の固形分と前記グラフトモノマー成分(2)の合計が30重量%になるような割合で加えた。その後、窒素気流下で撹拌しながら60℃で3時間、70℃で3間重合反応を行い、前記グラフトモノマー成分(2)を、グラフト重合して、グラフト重合体を含有する溶液を得た。
得られたグラフト重合体を含有する溶液の固形分100重量部に対して、トルエンに溶解したスチレンオリゴマー(ヤスハラケミカル社製,SX−85,重量平均分子量1500,軟化点78℃)を固形分で80重量部となるように加え、さらに、トリメチロールプロパンのキシリレンジイソシアネート付加物(三井化学ポリウレタン社製,タケネートD−110N)1重量部を配合して、アクリル系粘着剤組成物を得た。
次いで、得られたアクリル系粘着剤組成物を、シリコーン処理を施した、38μmのポリエチレンテレフタレート(PET)フィルムの片面に、乾燥後の粘着剤層の厚さが30μmになるように塗布し、110℃で3分間乾燥を行い、粘着剤層を得た。
実施例1のアクリル系ポリマーの調製において、モノマー成分(1)の代わりに、n−ブチルアクリレート700重量部、2−メトキシエチルアクリレート30重量部および4−ヒドロキシブチルアクリレート1重量部からなるモノマー成分(2)を用いたこと以外は、実施例1と同様にして、アクリル系ポリマー(2)の調製を行った。また、実施例1において、アクリル系ポリマー(1)の代わりに、当該アクリル系ポリマー(2)を用いたこと以外は、実施例1と同様にして、グラフト重合体の調製、アクリル系粘着剤組成物の調製、粘着剤層の作製を行った。
実施例1のアクリル系ポリマーの調製において、モノマー成分(1)の代わりに、n−ブチルアクリレート700重量部、N−ビニルピロリドン30重量部および4−ヒドロキシブチルアクリレート1重量部からなるモノマー成分(3)を用いたこと以外は、実施例1と同様にして、アクリル系ポリマー(3)の調製を行った。また、実施例1において、アクリル系ポリマー(1)の代わりに、当該アクリル系ポリマー(3)を用いたこと以外は、実施例1と同様にして、グラフト重合体の調製、アクリル系粘着剤組成物の調製、粘着剤層の作製を行った。
実施例1のアクリル系粘着剤組成物の調製において、グラフト重合体の代わりに、アクリル系ポリマー(1)を用いたこと以外は、実施例1と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例1において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例1と同様にして、粘着剤層の作製を行った。
実施例1のアクリル系粘着剤組成物の調製において、グラフト重合体の代わりに、アクリル系ポリマー(1)を用いたこと、スチレンオリゴマーの添加量を50重量部になるように変えたこと以外は、実施例1と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例1において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例1と同様にして、粘着剤層の作製を行った。
(モノマーの部分重合)
攪拌羽根、温度計、窒素ガス導入管、冷却器を備えた4つ口フラスコに、n−ブチルアクリレート100重量部および4−ヒドロキシブチルアクリレート3重量部からなるモノマー成分(1)を加え、さらに光重合開始剤としてイルガキュア651(チバ・ジャパン社製)0.05重量部とイルガキュア184(チバ・ジャパン社製)0.05重量部を混合した後、窒素ガス雰囲気下で攪拌して溶存酸素を十分に除去した。次いで、前記混合物に紫外線(照度約5mW/cm2,120秒間)を照射し、前記モノマー成分(1)を一部重合して、重合率約10%の部分重合物(モノマーシロップ)を得た。
上記部分重合物に対して、トリメチロールプロパントリアクリレート0.5重量部と、トルエンに溶解したスチレンオリゴマー(ヤスハラケミカル社製,SX−85,重量平均分子量1500,軟化点78℃)を固形分で80重量部となるように加えて、均一に攪拌混合して、放射線照射用のアクリル系粘着剤組成物を得た。
次いで、得られた放射線照射用のアクリル系粘着剤組成物を、シリコーン処理を施した、38μmのポリエチレンテレフタレート(PET)フィルムの片面に、粘着剤層の厚さが30μmになるように塗布し、その上から同様のPETフィルムを設けた。その後、PETフィルムを介して、照度約5mW/cm2、光量約36000mJ/cm2の条件で紫外線を照射して、粘着剤層を得た。
実施例1のアクリル系粘着剤組成物の調製において、スチレンオリゴマーを添加しなかったこと以外は、実施例1と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例1において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例1と同様にして、粘着剤層の作製を行った。
実施例2のアクリル系粘着剤組成物の調製において、スチレンオリゴマーを添加しなかったこと以外は、実施例2と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例2において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例2と同様にして、粘着剤層の作製を行った。
実施例3のアクリル系粘着剤組成物の調製において、スチレンオリゴマーを添加しなかったこと以外は、実施例3と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例3において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例3と同様にして、粘着剤層の作製を行った。
実施例1のアクリル系粘着剤組成物の調製において、グラフト重合体の代わりに、アクリル系ポリマー(1)を用いたこと、スチレンオリゴマーを添加しなかったこと以外は、実施例1と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例1において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例1と同様にして、粘着剤層の作製を行った。
実施例1のアクリル系粘着剤組成物の調製において、スチレンオリゴマーを高軟化点のスチレンオリゴマー(ヤスハラケミカル社製,SX−100,重量平均分子量1500,軟化点100℃)に変えたこと以外は、実施例1と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例1において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例1と同様にして、粘着剤層の作製を行った。
実施例6のアクリル系粘着剤組成物の調製において、スチレンオリゴマー添加しなかったこと以外は、実施例6と同様にして、アクリル系粘着剤組成物の調製を行った。また、実施例6において、当該アクリル系粘着剤組成物を用いたこと以外は、実施例1と同様にして、粘着剤層の作製を行った。
各例で得られた粘着剤層を、離型フィルムから剥離して、スライドガラス(松浪硝子工業性、型番:S1111)に貼り合わせて、25℃の雰囲気下で、(株)村上色彩技術研究所社製の「反射・透過率計 HR−100型」を用いて、JIS K−7136に準じて、へイズ値(%)を測定した。当該値からスライドガラスのヘイズ値(0.2%)を差し引いた値を、粘着剤層のヘイズ値とした。ヘイズ値が2%未満の場合を「○」、2%以上の場合を「×」とした。
各例で得られた粘着剤層について、25℃の雰囲気で、ナトリウムD線を照射し、アッベ屈折率計(ATAGO社製,DM−M4)にて屈折率を測定した。
透明導電性薄膜(ITO膜)を設けた透明導電性フィルム(日東電工社製,エレクリスタ:V270L−TFMP)のITO膜側のITO膜を残したいところに、ポリイミド粘着テープ(幅1cm)を貼り合わせたものをサンプル1とした。当該サンプル1を、1mol/lに調整された塩酸に2分間浸漬して、ITO膜をエッチングした。その後、サンプル1をイオン交換水で充分に洗浄した後、120℃で10分間で乾燥させてから、サンプル1からポリイミド粘着テープを外した、ITO膜がパターニングされた透明導電性フィルムを得た。当該パターニングされた透明導電性フィルムに、140℃で90分間のアニール処理を施して、パターニングされたITO膜を結晶化させた。一方、各例で得られた粘着剤層を、厚さ100μmのPETフィルムに転写して、粘着剤層付きのPETフィルムとした。当該粘着剤層付きのPETフィルムを、上記で得られた透明導電性フィルムのパターニングされたITO膜(結晶)に貼り合わせたものをサンプル2とした。サンプル2について、下記基準で、蛍光灯下で目視にてパターニングされたITO膜の見え方を評価した。
◎:パターンがほとんど見えない。
○:パターンがうっすら見える。
△:パターンが見える。
−:透明性がないため、未評価。
パターン見えの評価で作製した粘着剤層付きのPETフィルムを、印刷段差付きのガラスに貼り合わせた。図5に、印刷段差付きのガラスを上部から見た図を示す。内側にあるガラスのサイズは5cm×10cm×0.7cmである。外側の黒い部分が印刷部であり、段差は25μmである。その後、85℃、40℃、常温(23℃)において24時間放置したときの粘着剤層を貼り合わせた面の浮きなど状態を、下記基準で評価した。
◎:85℃で浮きがない。
○:40℃で浮きがない。
△:常温で浮きがない。
2 透明導電性薄膜層
3 粘着剤層
4 離型フィルム
5 アンダーコート層
6 オリゴマー防止層
Claims (10)
- パターニングされた透明導電性薄膜を有する透明導電性フィルムに用いられる粘着剤層であって、
前記粘着剤層は、アルキル(メタ)アクリレートを含有するモノマー成分を重合して得られるアクリル系ポリマー100重量部に対し、スチレン系オリゴマーを30〜150重量部含有するアクリル系粘着剤組成物から形成されたものであり、
かつ、前記粘着剤層は、屈折率が1.50以上であり、
厚さ30μmで測定した場合のヘイズ値が2%以下であることを特徴とする透明導電性フィルム用粘着剤層。 - 前記スチレン系オリゴマーの軟化点が95℃以下であることを特徴とする請求項1記載の透明導電性フィルム用粘着剤層。
- 前記アクリル系ポリマーを形成するモノマー成分が、芳香族基含有モノマーを共重合モノマーとして含有することを特徴とする請求項1または2記載の透明導電性フィルム用粘着剤層。
- 前記芳香族基含有モノマーが、グラフト重合により前記アクリル系ポリマーに導入さていることを特徴とする請求項3記載の透明導電性フィルム用粘着剤層。
- 前記アクリル系ポリマーが、アルキル(メタ)アクリレートを含有するモノマー成分を放射線重合して得られたものであることを特徴とする請求項1〜4のいずれか1項に記載の透明導電性フィルム用粘着剤層。
- 第一の透明プラスチックフィルム基材の一方の面に、パターニングされた透明導電性薄膜を有し、当該透明導電性薄膜の上に請求項1〜5のいずれか1項に記載の粘着剤層をさらに有する粘着剤層付き透明導電性フィルム。
- 前記透明導電性薄膜は、少なくとも1層のアンダーコート層を介して、第一の透明プラスチックフィルム基材に設けられていることを特徴とする請求項6記載粘着剤層付き透明導電性フィルム。
- 第一の透明プラスチックフィルム基材における、前記透明導電性薄膜が設けられていない他方の面に、オリゴマー防止層が設けられていることを特徴とする請求項6または7記載の粘着剤層付き透明導電性フィルム。
- 請求項5〜8のいずれか1項に記載の粘着剤層付き透明導電性フィルムの粘着剤層に、さらに、第二の透明プラスチックフィルム基材が貼り合わされていることを特徴とする透明導電性積層体。
- 請求項5〜8のいずれか1項に記載の粘着剤層付き透明導電性フィルムまたは請求項9記載の透明導電性積層体が、電極板に用いられていることを特徴とするタッチパネル。
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CN201210514762.4A CN103131344B (zh) | 2011-12-05 | 2012-12-04 | 透明导电膜用粘合剂层、带粘合剂层的透明导电膜、透明导电层叠体以及触控面板 |
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