JP6538332B2 - 光学用両面粘着シート - Google Patents
光学用両面粘着シート Download PDFInfo
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- JP6538332B2 JP6538332B2 JP2014232599A JP2014232599A JP6538332B2 JP 6538332 B2 JP6538332 B2 JP 6538332B2 JP 2014232599 A JP2014232599 A JP 2014232599A JP 2014232599 A JP2014232599 A JP 2014232599A JP 6538332 B2 JP6538332 B2 JP 6538332B2
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- Prior art keywords
- sensitive adhesive
- pressure
- meth
- adhesive sheet
- optical
- Prior art date
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Description
本発明の光学用両面粘着シートは、粘着剤層を少なくとも1層有する。上記粘着剤層を構成する粘着剤としては、特に限定されないが、例えば、アクリル系粘着剤、ゴム系粘着剤、ビニルアルキルエーテル系粘着剤、シリコーン系粘着剤、ポリエステル系粘着剤、ポリアミド系粘着剤、ウレタン系粘着剤、フッ素系粘着剤、エポキシ系粘着剤などが挙げられる。中でも、粘着剤層を構成する粘着剤としては、透明性、粘着性、耐候性、コスト、粘着剤の設計のしやすさの点より、アクリル系粘着剤が好ましい。つまり、上記粘着剤層は、アクリル系粘着剤から構成されたアクリル系粘着剤層であることが好ましい。上記粘着剤は、単独で又は2種以上組み合わせて用いることができる。
吸光度A:前記紫外線吸収剤の0.08%トルエン溶液に対して、波長400nmの光を当て、測定される吸光度
本発明の光学用両面粘着シートが基材付き粘着シートである場合の基材としては、特に限定されないが、例えば、プラスチックフィルム、反射防止(AR)フィルム、偏光板、位相差板などの各種光学フィルムが挙げられる。上記プラスチックフィルムなどの素材としては、例えば、ポリエチレンテレフタレート(PET)等のポリエステル系樹脂、ポリメチルメタクリレート(PMMA)等のアクリル系樹脂、ポリカーボネート、トリアセチルセルロース(TAC)、ポリサルフォン、ポリアリレート、ポリイミド、ポリ塩化ビニル、ポリ酢酸ビニル、ポリエチレン、ポリプロピレン、エチレン−プロピレン共重合体、商品名「アートン」(環状オレフィン系ポリマー、JSR株式会社製)」、商品名「ゼオノア」(環状オレフィン系ポリマー、日本ゼオン株式会社製)等の環状オレフィン系ポリマーなどのプラスチック材料が挙げられる。なお、これらのプラスチック材料は、単独で又は2種以上を組み合わせて用いることができる。また、上記の「基材」とは、粘着シートを被着体(光学部材等)に貼付する際には、粘着剤層とともに被着体に貼付される部分である。粘着シートの使用時(貼付時)に剥離される剥離ライナーは「基材」には含まない。
本発明の光学用両面粘着シートは、使用時まで、粘着剤層の表面(粘着面)に剥離ライナー(セパレーター)が設けられていてもよい。なお、本発明の光学用両面粘着シートの各粘着面は、2枚の剥離ライナーによりそれぞれ保護されていてもよいし、両面が剥離面となっている剥離ライナー1枚により、ロール状に巻回される形態(巻回体)で保護されていてもよい。剥離ライナーは粘着剤層の保護材として用いられ、被着体に貼付する際に剥がされる。また、本発明の光学用両面粘着シートが基材レス粘着シートの場合、剥離ライナーは粘着剤層の支持体としての役割も担う。なお、剥離ライナーは必ずしも設けられなくてもよい。
本発明の光学用両面粘着シートのヘイズは、特に限定されないが、光学製品の外観特性、透明性、視認性の点より、5%以下が好ましく、より好ましくは3%以下であり、さらに好ましくは1.5%以下、特に好ましくは1%以下である。
ジシクロペンタニルメタクリレート(DCPMA、メタクリル酸ジシクロペンタニル):60重量部、メチルメタクリレート(MMA、メタクリル酸メチル):40重量部、連鎖移動剤としてのα−チオグリセロール:3.5重量部、及び重合溶媒としてのトルエン:100重量部を、4つ口フラスコに投入し、これらを窒素雰囲気下にて70℃で1時間撹拌した。次に、重合開始剤としての2,2’−アゾビスイソブチロニトリル:0.2重量部を4つ口フラスコに投入し、70℃で2時間反応させ、続いて、80℃で2時間反応させた。その後、反応液を130℃の温度雰囲気下に投入し、トルエン、連鎖移動剤、及び未反応モノマーを乾燥除去し、固形状のアクリル系ポリマー(「アクリル系ポリマー(A)と称する場合がある」)を得た。なお、アクリル系ポリマー(A)の重量平均分子量は、5.1×103であった。
アクリル酸2−エチルヘキシル(2EHA):67重量部、N−ビニル−2−ピロリドン(NVP):15重量部、アクリル酸2−ヒドロキシエチル(HEA):18重量部から構成されるモノマー混合物に、光重合開始剤(商品名「イルガキュア651」、BASF社製):0.035重量部、及び、光重合開始剤(商品名「イルガキュア184」、BASF社製):0.035重量部を配合した後、粘度(BH粘度計No.5ローター、10rpm、測定温度30℃)が約20Pa・sになるまで紫外線を照射して、上記モノマー成分の一部が重合したプレポリマー組成物を得た。
上記プレポリマー組成物に、上記アクリル系ポリマー(A):5重量部、ヘキサンジオールアクリレート(HDDA):0.075重量部、シランカップリング剤(商品名「KBM−403」、信越化学工業株式会社製):0.3重量部を混合し、アクリル系粘着剤組成物を得た。
上記アクリル系粘着剤組成物を、ポリエチレンテレフタレート(PET)系剥離ライナー(日東電工株式会社製、厚み:125μm)上に塗布し、粘着剤組成物層を形成した。次いで、上記粘着剤組成物層上に、PET系剥離ライナー(日東電工株式会社製、厚み:125μm)を設け、上記粘着剤組成物層を被覆して酸素を遮断した。そして、[剥離ライナー/粘着剤組成物層/剥離ライナー]の構成を有する積層体(積層体(I))を得た。
次に、上記積層体(I)に対して、積層体(I)の上面(剥離ライナー側)から、ブラックライト(株式会社東芝製)にて、照度3mW/cm2の紫外線を300秒間照射した。さらに90℃の乾燥機で2分間乾燥処理を行い、残存モノマーを揮発させて、[剥離ライナー/粘着剤層/剥離ライナー]の構成を有する積層体(積層体(II))を得た。なお、粘着剤層の厚みは500μmであった。
上記積層体(II)の片面の剥離ライナーを剥離し、上記粘着剤層の表面と、ポリエチレンテレフタレート(PET)フィルム(厚み:125μm、面内位相差Re:4200nm)の一方の表面とを貼り合わせ、[剥離ライナー/粘着剤層/PETフィルム]の構成を有する積層体(積層体(III))を得た。
さらに、別途作製した積層体(II)の片面の剥離ライナーを剥離し、粘着剤層の表面と、上記積層体(III)のPETフィルムの表面とを貼り合わせ、[剥離ライナー/粘着剤層/PETフィルム/粘着剤層/剥離ライナー]の構成を有する両面粘着シート(基材付き両面粘着シート)を作製した。両面粘着シートの厚み(剥離ライナーを除く厚み)は、1125μmであった。
アクリル酸n−ブチル(BA):57重量部、シクロヘキシルアクリレート(CHA):12重量部、アクリル酸4−ヒドロキシブチル(4HBA):23重量部、アクリル酸2−ヒドロキシエチル(HEA):8重量部から構成されるモノマー混合物に、光重合開始剤(商品名「イルガキュア651」、BASF社製):0.05重量部、及び、光重合開始剤(商品名「イルガキュア184」、BASF社製):0.05重量部を配合した後、粘度(BH粘度計No.5ローター、10rpm、測定温度30℃)が約20Pa・sになるまで紫外線を照射して、上記モノマー成分の一部が重合したプレポリマー組成物を得た。
上記プレポリマー組成物に、ジペンタエリスリトールヘキサアクリレート(DPHA):0.1重量部、シランカップリング剤(商品名「KBM−403」、信越化学工業株式会社製):0.3重量部を混合し、アクリル系粘着剤組成物を得た。
上記アクリル系粘着剤組成物を用いて、PETフィルムとしてPETフィルム(厚み:100μm、面内位相差Re:10000nm)を用いたこと以外は実施例1と同様にして、[剥離ライナー/粘着剤層/PETフィルム/粘着剤層/剥離ライナー]の構成を有する両面粘着シート(基材付き両面粘着シート)を作製した。両面粘着シートの厚み(剥離ライナーを除く厚み)は、1100μmであった。
アクリル酸2−エチルヘキシル(2EHA):40.5重量部、イソステアリルアクリレート(ISTA):40.5重量部、N−ビニル−2−ピロリドン(NVP):18重量部、アクリル酸4−ヒドロキシブチル(4HBA):1重量部から構成されるモノマー混合物に、光重合開始剤(商品名「イルガキュア651」、BASF社製):0.05重量部、及び、光重合開始剤(商品名「イルガキュア184」、BASF社製):0.5重量部を配合した後、粘度(BH粘度計No.5ローター、10rpm、測定温度30℃)が約20Pa・sになるまで紫外線を照射して、上記モノマー成分の一部が重合したプレポリマー組成物を得た。
上記プレポリマー組成物に、トリメチロールプロパントリアクリレート(TMPTA):0.02重量部、シランカップリング剤(商品名「KBM−403」、信越化学工業株式会社製):0.3重量部混合し、アクリル系粘着剤組成物を得た。
上記アクリル系粘着剤組成物を用いて、実施例1と同様にして、[剥離ライナー/粘着剤層/PETフィルム/粘着剤層/剥離ライナー]の構成を有する両面粘着シート(基材付き両面粘着シート)を作製した。両面粘着シートの厚み(剥離ライナーを除く厚み)は、1125μmであった。
粘着剤層の厚みが550μmとなるようにした以外は、実施例1で作製した積層体(II)と同様に積層体を作製し、粘着剤層のみからなり、粘着剤層の両面が剥離ライナーで保護されている基材レスタイプの両面粘着シートを作製した。両面粘着シートの厚みは550μmであった。
粘着剤層の厚みが610μmとなるようにした以外は、実施例1で作製した積層体(II)と同様に積層体を作製し、粘着剤層のみからなり、粘着剤層の両面が剥離ライナーで保護されている基材レスタイプの両面粘着シートを作製した。両面粘着シートの厚みは610μmであった。
粘着剤層の厚みが250μmとなるようにした以外は、実施例1で作製した積層体(II)と同様に積層体を作製し、粘着剤層のみからなり、粘着剤層の両面が剥離ライナーで保護されている基材レスタイプの両面粘着シートを作製した。両面粘着シートの厚みは250μmであった。
実施例及び比較例で得られた両面粘着シートについて、下記の測定を行った。その結果を表1に示した。
実施例及び比較例で得られた両面粘着シートの一方の剥離ライナーを剥がし、両面粘着シートをスライドガラス(商品名「MICRO SLIDE GLASS」、白研磨、NO.2、厚み:1.0〜1.2mm、松浪硝子株式会社製)に貼り付け、温度23℃、湿度50%RHの環境下で放置した。放置後、もう一方の剥離ライナーを取り除き、試験片とした。
なお、両面粘着シートを貼り付ける際には、ハンドローラーを用い、表面に指紋等の汚れがつかないようにし、異物や気泡を噛み込まないようにした。
上記試験片の全光線透過率を、23℃、50%RHの環境下において、ヘイズメーター(商品名「HM−150」、株式会社村上色彩技術研究所製)を用いて測定した。
全光線透過率の測定は、JIS K 7361−1に準じて行った。
実施例及び比較例で得られた両面粘着シートの一方の剥離ライナーを剥がし、両面粘着シートをスライドガラス(商品名「MICRO SLIDE GLASS」、白研磨、NO.2、厚み:1.0〜1.2mm、松浪硝子株式会社製)に貼り付け、温度23℃、湿度50%RHの環境下で放置した。放置後、もう一方の剥離ライナーを取り除き、試験片とした。
なお、両面粘着シートを貼り付ける際には、ハンドローラーを用い、表面に指紋等の汚れがつかないようにし、異物や気泡を噛み込まないようにした。
上記試験片のヘイズを、23℃、50%RHの環境下において、ヘイズメーター(商品名「HM−150」、株式会社村上色彩技術研究所製)を用いて測定した。
ヘイズの測定は、JIS K 7136に準じて行った。
実施例及び比較例で得られた両面粘着シートの一方の剥離ライナーを剥がし、両面粘着シートをスライドガラス(商品名「MICRO SLIDE GLASS」、白研磨、NO.2、厚み:1.0〜1.2mm、松浪硝子株式会社製)に貼り付け、温度23℃、湿度50%RHの環境下で放置した。放置後、もう一方の剥離ライナーを取り除き、試験片とした。
なお、両面粘着シートを貼り付ける際には、ハンドローラーを用い、表面に指紋等の汚れがつかないようにし、異物や気泡を噛み込まないようにした。
上記試験片のb*値を、簡易型分光色差計(商品名「DOT−3C」、株式会社村上色彩技術研究所製)を用いて測定した。なお、測定は、試験片の露出した粘着面に光を当てて行った。
b*値の測定は、JIS Z 8781−4(2013年)に準じて行った。
実施例及び比較例で得られた粘着剤層と同様にして、厚さが約2mmとなるように粘着剤層をそれぞれ作製し、これをφ7.9mmに打ち抜き、円柱状のペレットを作製して測定用サンプルとした。φ7.9mmパラレルプレートの治具に上記測定サンプルを固定し、動的粘弾性測定装置(レオメトリックス社製、ARES、測定:せん断モード、温度範囲:−70℃〜150℃、昇温速度:5℃/分、周波数:1Hz)により、貯蔵弾性率G’の温度依存性を測定し、25℃における貯蔵弾性率G’を25℃の弾性率とした。
実施例及び比較例で得られた粘着剤層と同様にして、厚さが約2mmとなるように粘着剤層をそれぞれ作製し、これをφ7.9mmに打ち抜き、円柱状のペレットを作製して測定用サンプルとした。φ7.9mmパラレルプレートの治具に上記測定サンプルを固定し、動的粘弾性測定装置(レオメトリックス社製、ARES、測定:せん断モード、温度範囲:−70℃〜150℃、昇温速度:5℃/分、周波数:1Hz)により、貯蔵弾性率G’の温度依存性を測定し、95℃における貯蔵弾性率G’を95℃の弾性率とした。
実施例及び比較例で得られた両面粘着シートを80mm×80mmのサイズに切り取ったものを試験片とした。上記試験片の一方の剥離ライナーを剥離したものを、段差付ガラス(ガラスの一方の面に、市販の両面粘着シートを用いてPETフィルムを縁状に貼り付けて0.5mmの段差を設けたもの。図3、図4及び図5参照。「下ガラス」と称する場合がある。)の段差を有する側のガラス面に貼り合わせた。そして、下ガラスと両面粘着シートの積層構造を有する構造物Aを得た。次に、構造物Aにおける両面粘着シートの剥離ライナーを剥離して、構造物Aを、100mm×100mmのサイズのガラス板(「上ガラス」と称する場合がある)の一方の面に、圧力0.3MPa、真空度100Paの条件で5秒間真空プレスをかけて貼り合わせた。そして、上ガラスと両面粘着シートと下ガラスの積層構造を有する構造物Bを得た。その後、構造物Bをオートクレーブに投入し、温度50℃、圧力0.5MPaの条件で15分間、オートクレーブ処理した。オートクレーブ処理後、構造物Bをオートクレーブから取り出し、構造物Bを目視で観察し、両面粘着シートの貼り合わせ性を下記基準で評価した。なお、従来のベゼル付きの車載用の光学製品におけるエアーギャップは通常0.5〜1.5mmであるため、0.5mmの段差を設けた下ガラスを用いて評価を行った。
○(良好) :両面粘着シートの全面で気泡が無く貼り合わせができている
×(不良) :両面粘着シートが上ガラスに届かず、きれいに貼り合わせできていない
実施例及び比較例で得られた両面粘着シートから50mm×100mmのサイズに切り取ったものを試験片とした。上記試験片の一方の剥離ライナーを剥がし、試験片をソーダガラス(厚み:0.7mm)に貼り付け、試験片のもう一方の剥離ライナーを剥がし、PPMA(商品名「MR200」、三菱レーヨン株式会社製、厚み:1mm)に貼り付けて、[ソーダガラス/両面粘着シート/PMMA]の構成を有する積層体を作製し、温度50℃、0.50MPaの環境下に15分間放置した。放置後の積層体を、さらに、95℃の環境下に100時間放置し、放置後の積層体を目視で観察した。接着信頼性を、下記のように評価した。
○(良好) :発泡が無く、且つ剥がれもない
△(使用可能) :一部発泡がある
×(不良) :発泡も剥がれもある
2 プラスチックカバー
3 印刷層
4 粘着シート
5 ガラスセンサー
6 フォーム
7 ベゼル
8 本発明の光学用両面粘着シート
9a 偏光板
9b 偏光板
10 液晶ディスプレイ
11 オンセル又はインセル
100 下ガラス(段差付ガラス)
101 ガラス板
102 両面粘着シート
103 PETフィルム
Claims (7)
- 95℃の弾性率が4.0×104Pa以上、25℃の弾性率が1.0×10 6 Pa以下である粘着剤層を少なくとも有し、
前記粘着剤層は、ベースポリマーとしてアクリル系ポリマーを含有するアクリル系粘着剤層であり、
前記アクリル系ポリマーは(メタ)アクリル酸アルキルエステルと、窒素原子を有するモノマー及び/又は分子内に水酸基を有するモノマーとをモノマー成分として構成された重合体であり、前記アクリル系ポリマーを構成する全モノマー成分中の窒素原子含有モノマー及び水酸基含有モノマーの割合の合計が15重量%以上であり、
厚みが500μm以上であり、車載用の光学製品に用いることを特徴とする光学用両面粘着シート。 - 前記光学用両面粘着シートが、基材の両面に粘着剤層を有する請求項1に記載の光学用両面粘着シート。
- 前記基材の厚みが75μm以上である請求項2に記載の光学用両面粘着シート。
- 前記基材の面内位相差が4000nm以上である請求項2又は3に記載の光学用両面粘着シート。
- 前記基材の面内位相差が20nm以下である請求項2又は3に記載の光学用両面粘着シート。
- 車載用の光学製品内のエアーギャップを埋めることに用いるフルラミネーション用である請求項1〜5のいずれか1項に記載の光学用両面粘着シート。
- 請求項1〜6のいずれか1項に記載の光学用両面粘着シートを有する車載用光学製品。
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