JP2017019960A - 感圧式接着剤、感圧式接着フィルム、およびそれを用いた光学積層体 - Google Patents
感圧式接着剤、感圧式接着フィルム、およびそれを用いた光学積層体 Download PDFInfo
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- JP2017019960A JP2017019960A JP2015140542A JP2015140542A JP2017019960A JP 2017019960 A JP2017019960 A JP 2017019960A JP 2015140542 A JP2015140542 A JP 2015140542A JP 2015140542 A JP2015140542 A JP 2015140542A JP 2017019960 A JP2017019960 A JP 2017019960A
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- ether
- acrylate
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- 125000003647 acryloyl group Chemical group O=C([*])C([H])=C([H])[H] 0.000 description 7
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Landscapes
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
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Abstract
Description
また、表示装置として利用するだけではなく、その表面にタッチパネルの機能を設けて、入力装置として利用されることもある。タッチパネルにも、保護フィルム、反射防止フィルムやITO蒸着樹脂フィルムなどが使用されている。
このようなフィルムは、感圧式接着剤を介して被着体に貼着して表示装置に使用されている。表示装置に用いられる感圧式接着剤は、まず透明性に優れることが要求されるので、アクリル系樹脂を主剤とする感圧式接着剤が一般に使用されている。
しかし、貼着後の積層体は、一般に、接着性向上のために高温下で一定時間保管した後に検査されるので、その間に剥離強度が高くなって偏光フィルムを剥ぎ取り難くなるばかりでなく、偏光フィルムの再剥離性が低下して剥がした後、ガラス面に糊残りや曇り等の汚染が生じる場合があった。
そこで感圧式接着剤の分子量や感圧式接着剤の架橋度を調整し、接着力を高くすることによって、偏光フィルムの寸法変化に抗して、過酷な環境下でも発泡、浮き、剥がれが生じないようにする試みがなされた。
例えば、感圧式接着光学フィルム用の感圧式接着剤として、α、β−エチレン性不飽和化合物を共重合した樹脂に可塑剤などの低分子量体を添加することで、感圧式接着層を適度に軟らかくして応力緩和性を付与する感圧式接着剤が開示されている(例えば特許文献1参照)。
また、電子顕微鏡でなければ確認できない10μm以下の気泡が、中央部に1m2あたり10個程度発生してしまう。
さらに、19インチ以上の表示装置では、見やすさの観点から光源の輝度を高く設定しなければならない。特許文献1に記載される感圧式接着剤を積層して用いてなる光学用の感圧式接着フィルム(光学用接着フィルムとも称す)は、19インチ未満の表示装置では白抜けは問題視されなかった。しかし、架橋剤による架橋収縮や不十分な接着性の影響で19インチ以上で使用される高輝度の光源を用いた表示装置では白抜けが目立ってしまうという問題も生じた。
さらには、透明性や樹脂、溶剤への溶解性(相溶性)、並びに耐湿熱性を併せ持つ感圧式接着剤が望まれていた。
本発明の感圧式接着剤は、分子中に1個以上の水酸基を含有するα,β−不飽和二重結合基含有化合物(a1)および分子中に水酸基を含有しないα,β−不飽和二重結合基含有化合物(a2)を含む単量体混合物を重合してなり、重量平均分子量100,000〜2,000,000、水酸基価0.1〜50mgKOH/gである共重合体(A)と、燐酸またはその誘導体(B)と、アミノ基またはエポキシ基を有するシラン化合物(C)と、ポリイソシアネート化合物(D)とを含有することが特徴である。
なお、本明細書では、「(メタ)アクリル」、「(メタ)アクリロイル」、「(メタ)アクリル酸」、「(メタ)アクリレート」、「(メタ)アクリロイルオキシ」、及び「(メタ)アリル」と表記した場合には、特に説明がない限り、それぞれ、「アクリルまたはメタクリル」、「アクリロイルまたはメタクリロイル」、「アクリル酸またはメタクリル酸」、「アクリレートまたはメタクリレート」、「アクリロイルオキシまたはメタクリロイルオキシ」、及び「アリルまたはメタリル」を表すものとする。
<共重合体(A)>
共重合体(A)は、分子中に1個以上の水酸基を含有するα,β−不飽和二重結合基含有化合物(a1)および分子中に水酸基を含有しないα,β−不飽和二重結合基含有化合物(a2)を含む単量体混合物を重合した樹脂である。分子中に1個以上の水酸基を含有するα,β−不飽和二重結合基含有化合物(a1)としては、その構造中に、1個以上の水酸基と、1個以上のα,β−不飽和二重結合基とを含有する化合物であり、このよう化合物(a1)としては、分子内に水酸基を有し、環状構造を有しない化合物(a1−1)と分子内に水酸基を有し、環状構造を有する化合物(a1−2)に類別できる。具体例として、以下の化合物が挙げられる。
化合物(a2)は、分子内に水酸基を有しないα,β−不飽和二重結合基を含有する化合物であり、上記共重合体(A)に上記成分(a2)を含有させることによって、前記化合物(a1)との共重合反応の効率化を図ることが容易である。また、上記共重合体(A)を容易に低粘度化できるとともに、塗工時の作業性を向上させることが容易となる。また、塗工物のガラス転移温度(以下、Tgと称す)を制御させて粘着性(タックとも称す)を向上したり、塗膜の凝集力を向上させて耐熱性や耐水性等の耐性の良好な感圧式接着層を形成することが可能となるものである。α,β−不飽和二重結合基含有化合物(a2−1)は、その単独重合体(ホモポリマーとも称す)が、Tgが0℃以下であり、側鎖にアルキル基を有するものが好ましい。化合物(a2−1)を共重合することにより、共重合体(A)にタックを付与することが可能となり、感圧式接着剤として有用に使用することが可能となる。
<FOX式>1/Tg=W1/Tg1+W2/Tg2+…+Wi/Tgi+…+Wn/Tgn
〔上記FOX式は、n種のα,β−不飽和二重結合基含有化合物からなる重合体を構成する各化合物の単独重合体のガラス転移温度をTgi(K)とし、各化合物の質量分率を、Wiとしており、(W1+W2+…+Wi+…Wn=1)である。〕
次に、P−OHを1つ以上有する化合物または加水分解によりP−OHを1つ以上形成し得る化合物(B)について説明する。P−OHを1つ以上有する化合物または加水分解によりP−OHを1つ以上形成し得る化合物(B)とは、燐酸類(b1)、燐酸金属または燐酸アンモニウム等の燐酸塩(b2)、ホスホニル基、ホスフィニル基、またはホスファニル基を含有する燐酸エステルや燐酸アミド等の燐酸系化合物(b3)等を指し、分子内にP−O−H結合を1つ以上有するか、又は、加水分解してP−O−H結合を1つ以上形成し得る化合物があげられる。化合物(B)は、前記した共重合体(A)中の水酸基や、後述のシラン化合物(C)中のアミノ基、エポキシ基、あるいはシロキシ基との間に、付加、置換あるいはキレート化反応を引き起こし、燐酸エステル化や燐酸アミド化が進行する。
例えば、燐酸水素二アンモニウム、燐酸二アンモニウム等の燐酸アンモニウム塩等が挙げられる。
次に、アミノ基またはエポキシ基を有するシラン化合物(C)について説明する。
アミノ基またはエポキシ基を有するシラン化合物(C)とは、アミノ基を有するシラン化合物(c1)またはエポキシ基を有するシラン化合物(c2)を意味する。シラン化合物(c1)に含有されるアミノ基は上記したP−OHを1つ以上有する化合物または加水分解によりP−OHを1つ以上形成し得る化合物(B)の燐酸基と塩を形成し、また、シラン化合物(c2)に含有されるエポキシ基は上記した燐酸またはその誘導体(B)の燐酸基と付加反応による結合を形成するため、感圧式接着剤の塗工乾燥時におけるシラン化合物(C)の飛散を抑制するだけでなく、塗膜中でのシラン化合物の定着性を向上することが可能となるため、本来のシラン化合物の特性を発揮しやすくなる。
また、シラン化合物(C)に含有されているアミノ基、あるいはエポキシ基は、後述のポリイソシアネート化合物(D)に含有されているイソシアネート基と架橋反応を起こし、またシラン化合物(C)に含まれるシロキシ基が共重合体(A)や後述の基材(G)に含有されている水酸基と架橋反応を起こし、感圧式接着剤と基材(G)や被着体との間に強固な相互作用を発現させることも可能である。
1,1,3,3−テトラメチルジシラザン、ヘキサメチルジシラザン、1,3−ジビニル−1,1,3,3−テトラメチルジシラザン、N,N'−ビス(トリメチルシリル)−N−フェニルウレア等の2官能のシリルアミノ基を保有するシリルアミン類;
1,1,3,3,5,5−ヘキサメチルシクロトリシラザン、1,1,3,3,5,5,7,7−オクタメチルシクロテトラシラザン等の3官能以上の環状シリルアミノ基を保有するシリルアミン類等が挙げられる。
次に、ポリイソシアネート化合物(D)について説明する。
ポリイソシアネート化合物(D)は、共重合体(A)の水酸基と架橋反応し、感圧式接着剤の架橋分子量を向上させ、凝集力を向上させる役割を持つ。また、化合物(D)は後述する基材(G)表面に存在する極性基や付着水との化学反応や物理吸着等の相互作用を向上させる効果が期待できる。さらには、コロナ放電処理等の物理処理、酸などで改質された化学処理のなされた基材に対しては、化合物(D)中のイソシアネート基と基材(G)との化学反応や投錨効果等により、共重合体(A)と基材(G)との間に強固な相互作用を発現させることも可能である。
ポリイソシアネート化合物(D)としては、芳香族ポリイソシアネート、脂肪族ポリイソシアネート、芳香脂肪族ポリイソシアネート、脂環族ポリイソシアネート等に類別される。
錫系化合物としては、ジブチル錫ジクロライド、ジブチル錫オキサイド、ジブチル錫ジブロマイド、ジブチル錫ジマレエート、ジブチル錫ジラウレート(別名:DBTDL)、ジブチル錫ジアセテート、ジブチル錫スルファイド、トリブチル錫スルファイド、トリブチル錫オキサイド、トリブチル錫アセテート、トリエチル錫エトキサイド、トリブチル錫エトキサイド、ジオクチル錫オキサイド、トリブチル錫クロライド、トリブチル錫トリクロロアセテート、2−エチルヘキサン酸錫等が挙げられる。
非錫系化合物としては、例えばジブチルチタニウムジクロライド、テトラブチルチタネート、ブトキシチタニウムトリクロライドなどのチタン系、オレイン酸鉛、2−エチルヘキサン酸鉛、安息香酸鉛、ナフテン酸鉛などの鉛系、2−エチルヘキサン酸鉄、鉄2,4−ペンタジオネートなどの鉄系、安息香酸酸コバルト、2−エチルヘキサン酸コバルトなどのコバルト系、ナフテン酸亜鉛、2−エチルヘキサン酸亜鉛などの亜鉛系、ナフテン酸ジルコニウムなどが挙げられる。
上記触媒の中で、ジブチル錫ジラウレート(別名:DBTDL)、2−エチルヘキサン酸錫等が反応性や衛生性の点で好ましい。
次にアミノ基及びエポキシ基を有さないシラン化合物(E)について説明する。
本発明の感圧式接着剤の一実施形態において、感圧式接着剤は、上記必須成分に加えて、アミノ基及びエポキシ基を有さないシラン化合物(E)を含んでもよい。シラン化合物(E)を併用することで、上記シラン化合物(C)とともに、シラン化合物同士の自己縮合反応を生じさせたり、基材(G)表面や被着体表面の極性基との間で化学反応や物理吸着の相互作用が発現し、感圧式接着剤の接着力を向上させることができる。特に、ガラスや金属箔、金属蒸着フィルム、金属板、または無機フィラー含有のフィルム等の無機材料表面に対し、化学反応や物理吸着の相互作用が高いため、接着強度を向上させることが容易となる。
次にエポキシ系化合物(F)について説明する。
本発明の感圧式接着剤の一実施形態において、感圧式接着剤は、上記必須成分に加えて、エポキシ系化合物(F)(ただし、シラン化合物(c2)に属するものを除く)を含んでもよい。化合物(F)を使用することによって、併用架橋が可能となるため、硬化塗膜の硬度化が可能となり、過酷な環境下における耐熱性又は耐湿熱性を向上させることが容易となる。
本発明の感圧式接着剤の一実施形態において、本発明による効果を損なわない範囲であれば、感圧式接着剤には、上記必須成分に加えて、その他の成分(Q)を適宜配合することも可能である。
その他の成分(Q)としては、例えば、重合硬化収縮率低減、熱膨張率低減、寸法安定性向上、弾性率向上、粘度調整、熱伝導率向上、強度向上、靭性向上、及び着色向上等の観点から、有機又は無機の充填剤を配合することができる。このような充填剤は、ポリマー、セラミックス、金属、金属酸化物、金属塩、及び染顔料等の材料から構成されるものであってよい。また、その形状については、特に限定されず、例えば、粒子状及び繊維状等であってよい。なお、上記ポリマー系の材料を配合する場合には、柔軟性付与剤、可塑剤、難燃化剤、保存安定剤、酸化防止剤、紫外線吸収剤、チクソトロピー付与剤、分散安定剤、流動性付与剤、タッキファイヤー、帯電防止剤及び消泡剤等の、独立した充填剤としてではなく、ポリマーブレンド又はポリマーアロイとして、感圧式接着剤中に、溶解、半溶解又はミクロ分散させることも可能である。
次に感圧式接着剤について、説明する。
本発明の感圧式接着剤は、分子中に1個以上の水酸基を含有するα,β−不飽和二重結合基含有化合物(a1)および分子中に水酸基を含有しないα,β−不飽和二重結合基含有化合物(a2)を含む単量体混合物を重合してなり、重量平均分子量100,000〜2,000,000、水酸基価0.1〜50mgKOH/gである共重合体(A)と、燐酸およびその誘導体(B)と、アミノ基またはエポキシ基を有するシラン化合物(C)と、ポリイソシアネート化合物(D)とを含有する事が特徴であり、必要に応じて、シラン化合物(E)、エポキシ化合物(F)、あるいはその他の成分(Q)を適宜配合したものである。
次に感圧式接着フィルムについて、説明する。
本発明の感圧式接着フィルムは、後述の基材(G)嬢に上記の感圧式接着剤からなる感圧式接着層が形成されたものである。感圧式接着フィルムの製造方法として、例えば、表面を剥離処理したシート状基材(剥離ライナーとも称す)の剥離処理面に感圧式接着剤を塗工、乾燥し、基材(G)を貼り合わせて作成する方法、または基材(G)に感圧式接着剤を直接塗工、乾燥し、接着層の表面に剥離ライナーの剥離処理面を貼り合わせて作成する方法が挙げられる。
例えば、偏光フィルムは偏光板とも呼ばれ、ポリビニルアルコール系偏光子の片面又は両面に、ポリノルボルネン系フィルムであるポリシクロオレフィ系フィルム、ポリアクリル酸エステル系樹脂のフィルム、ポリカーボネート系フィルム、またはポリエステル系フィルム等のフィルムを積層した多層構造フィルムである。偏光フィルムの場合、高温雰囲気及び高温高湿雰囲気に放置されたときにも、本発明による接着層は応力緩和性が良好であるため偏光フィルムの反りに起因する光漏れを抑制できる。
(合成例1)
重合槽、攪拌機、温度計、還流冷却器、滴下装置、窒素導入管を備えた重合反応装置の重合槽及び滴下装置に、下記単量体{分子中に1個以上の水酸基を含有するα,β−不飽和二重結合基含有化合物(a1)および分子中に水酸基を含有しないα,β−不飽和二重結合基含有化合物(a2)}、重合開始剤、及び有機溶剤をそれぞれ下記の比率で仕込んだ。
アクリル酸n−ブチル(a2−1) 39部
アクリル酸メチル(a2−2) 20部
アクリル酸2−ヒドロキシエチル(a1−1) 1部
アセトン(有機溶剤) 33部
V65(重合開始剤) 0.1部
[滴下装置]
アクリル酸n−ブチル(a2−1) 39部
アクリル酸2−ヒドロキシエチル(a1−1) 1部
アセトン(有機溶剤) 33部
V65(重合開始剤) 0.1部
表1に記載した材料を、化合物(a2−2)は全て重合槽に仕込み、化合物(a1)、化合物(a2−1)、有機溶剤および重合開始剤は、重合槽と滴下装置に半量ずつ仕込んだ以外は、合成例1と同様の方法で、それぞれ共重合体溶液を合成した。得られた共重合体の溶液外観、不揮発分濃度(NV)、溶液粘度(Vis)、重量平均分子量(Mw)、水酸基価(OHV)及びガラス転移温度(Tg)を以下の方法に従って求め、結果を表1に示した。
各合成例で得られた共重合体の溶液外観を観察し、目視にて評価した。
各合成例で得られた共重合体の溶液、約1gを金属容器に秤量し、150℃オーブン中にて20分間乾燥して、残分を秤量して残率計算をし、不揮発分濃度(固形分)とした(単位:%)。
各合成例で得られた共重合体溶液を23℃の雰囲気下でE型粘度計(東機産業社製 TV−22)にて、約1.2mlを測定用試料とし、回転速度0.5〜100rpm、1分間回転の条件で測定し、溶液粘度(mPa・s)とした。
数平均分子量(Mn)と重量平均分子量(Mw)の測定は、昭和電工社製GPC(ゲルパーミエーションクロマトグラフィー)を用いた。数平均分子量(Mn)と重量平均分子量(Mw)の決定は、標準物質としてポリスチレンの換算で行った。
装置名 : 昭和電工社製GPC(ゲルパーミエーションクロマトグラフィー)「ShodexGPC System−21」
カラム : 東ソー社製GMHXL 4本、東ソー社製HXL-H 1本を直列に連結した。
移動相溶媒 : テトラヒドロフラン
流量 : 1.0ml/分
カラム温度 : 40℃
共栓三角フラスコ中に試料、約1gを精密に量り採り、トルエン/エタノール(容量比:トルエン/エタノール=2/1)混合液100mlを加えて溶解した。次いで、アセチル化剤(無水酢酸25gをピリジンで溶解し、容量100mlとした溶液)を5ml加え、1時間攪拌した。これに、フェノールフタレイン試液を指示薬として加え、30秒間保持した。その後、溶液が淡紅色を呈するまで0.1Nアルコール性水酸化カリウム溶液で滴定した。
水酸基価は次式により求めた。水酸基価は樹脂の乾燥状態の数値とした(単位:mgKOH/g)。
水酸基価(mgKOH/g)=[{(b−a)×F×28.25}/S]/(不揮発分濃度/100)+D
ただし、S:試料の採取量(g)
a:0.1Nアルコール性水酸化カリウム溶液の消費量(ml)
b:空実験の0.1Nアルコール性水酸化カリウム溶液の消費量(ml)
F:0.1Nアルコール性水酸化カリウム溶液の力価
D:酸価(mgKOH/g)
ロボットDSC(示差走査熱量計、セイコーインスツルメンツ社製「RDC220」)に「SSC5200ディスクステーション」(セイコーインスツルメンツ社製)を接続して、測定に使用した。試料約10mgをアルミニウムパンに入れ、秤量して示差走査熱量計にセットし、試料を入れない同タイプのアルミニウムパンをリファレンスとして、100℃の温度で5分間保持した後、液体窒素を用いて−120℃まで急冷した。その後、昇温速度10℃/分で昇温して得られたDSCチャートからガラス転移温度(Tg、単位:℃)を決定した。
・化合物(a1−1)
2HEA:アクリル酸2−ヒドロキシエチル、4HBA:アクリル酸4−ヒドロキシブチル
・化合物(a1−2)
HPPA:アクリル酸2−ヒドロキシ−3−フェノキシプロピル
・化合物(a2−1)
BA:アクリル酸n−ブチル、2EHA:アクリル酸2−エチルヘキシル、LMA:メタクリル酸ラウリル
・化合物(a2−2)
MA:アクリル酸メチル、MMA:メタクリル酸メチル、PHEA:アクリル酸フェノキシエチル、AA:アクリル酸
・重合開始剤
V65:2,2'−アゾビス(2,4−ジメチルバレロニトリル) [和光純薬工業社製「V65」]、PBO:t−ブチルパーオキシ−2−エチルヘキサノエート [日油社製「パーブチルO」]
・有機溶剤
Ace:アセトン、MEK:メチルエチルケトン、MeAc:酢酸メチル、EAc:酢酸エチル
なお、表1中の有機溶剤の欄で、「Ace/EAc」という表記は、「共重合体重合時の有機溶剤/希釈溶剤」ということを表し、共重合体重合時の有機溶剤はAceを使用し、希釈溶剤はEAcを使用したことを意味する。
(実施例1〜90、比較例1〜14)
各合成例で得られた共重合体(A)100部に対して、P−OHを1つ以上有する化合物または加水分解によりP−OHを1つ以上形成し得る化合物(B)、アミノ基またはエポキシ基を有するシラン化合物(C)、及びポリイソシアネート化合物(D)を必須成分として、必要に応じてシラン化合物(E)、エポキシ系化合物(F)、及びその他の成分(Q)を、表2に挙げた重量比(部)で配合し、酢酸エチル等の追加溶剤を加えて不揮発分濃度を約30%に調整して感圧式接着剤を得た。得られた感圧式接着剤を各基材に塗工、乾燥、及び貼り合わせを施し、感圧式接着フィルムを以下の方法で評価した。それぞれの結果を表2に示す。
上記で得られた感圧式接着剤について、配合後、25℃における粘度を1時間おきに8時間後まで、B型粘度計(東京計器社製)を用い、25℃、12rpm、1分間回転の条件で測定し、ポットライフ(可使時間)を3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:8時間までの粘度上昇率が1.2倍未満。良好。
△:8時間までの粘度上昇率が1.2倍以上〜2倍未満。実用上使用可能
×:8時間未満で濁りが発生したり、ゲル化したり、または粘度上昇率が2倍以上。実用不可。
前記感圧式接着剤を、基材として厚さ38μmの剥離処理されたポリエチレンテレフタレートフィルム(セラピールMF:東レフィルム加工社製、以下「剥離ライナー」という)上に、乾燥後の厚さが25μmになるように塗工し、100℃で2分間熱風乾燥することで接着層を形成した。次いで、上記塗工面に100μm厚のポリエチレンテレフタレートフィルム(ポリエステルフィルム)を貼り合せて、感圧式接着フィルムを作製した。そして剥離ライナーを剥がした後の接着層表面(塗工面)を目視にて観察し、3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:平滑な塗工面が得られた。良好。
△:塗工面の端部に若干のハジキや発泡が認められるが、実用上使用可。
×:塗工面にハジキ、発泡やスジ引きが認められ、不良。
上記感圧式接着フィルムを幅25mmに裁断し、剥離ライナーを剥がし、露出した接着層を厚さ100μmの無アルカリガラス板に23℃、相対湿度50%の環境下で、ラミネータを用いて貼着した。続いて、50℃、5気圧の条件のオートクレーブ内に20分間保持して測定試料を得た。前記測定試料を、23℃で1日間放置した後に、23℃、相対湿度50%の環境下で、引張試験機(オリエンテック社製「テンシロン」)を用いて、剥離速度300mm/分、剥離角度180度の条件で剥離強度を測定した(貼合せ1日後の剥離強度測定)。また、前記測定試料を、23℃で14日間放置した後に、同様の方法で剥離強度を測定した(貼合せ14日後の剥離強度測定)。この剥離強度を接着力として3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:剥離強度が8.0(N/25mm)以上12.0(N/25mm)未満。良好。
△:剥離強度が5.0(N/25mm)以上8.0(N/25mm)未満、あるいは剥離力が12.0(N/25mm)以上15.0(N/25mm)未満。実用可。
×:剥離強度が5.0(N/25mm)未満、あるいは15.0(N/25mm)以上。不良。
感圧式接着剤を、上記剥離ライナー上に、乾燥後の厚さが25μmになるように塗工し、100℃で2分間熱風乾燥することで感圧式接着層を形成した。次いで、別途用意した剥離ライナーを接着層に貼り合せて、接着層が剥離ライナーで挟持された試料を作製した。
次に、両方の剥離ライナーを取り除き、感圧式接着層単体の外観を目視判定するとともに、HAZEを「NDH−300A(日本電色工業社製)」で測定した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:曇り等が観察されず、かつHAZE:0.5未満。良好。
△:曇り等は観察されないが、HAZE:0.5以上2未満、実用上支障無く使用できる。
×:曇りが観察される、またはHAZE:2以上。不良。
上記感圧式接着フィルムを、幅100mm×長さ100mmに裁断し、これを30枚重ね、40℃−60Kg/cm2の条件で1時間プレスした際の接着フィルム端部からの接着層のはみ出しの様子を以下のように3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:接着層のはみ出しが観測されない。良好。
△:0.3mm未満の接着層のはみ出しが観測されるが、実用上使用可能。
×:0.3mm以上の接着層のはみ出しが観測される。不良。
上記感圧式接着フィルムを、幅100mm×長さ100mmに裁断し、剥離ライナーを剥離して、ポリカーボネート(PC)板に貼り合わせて固定し、50℃雰囲気下で0.5MPaの圧力をかけ20分間オートクレーブ内に保持して「ポリエステルフィルム/感圧式接着層/PC板」なる構成の層構造を有する試験片(光学積層体)を作製した。上記試験片を用いて、80℃のオーブン中で24時間熱処理(耐熱性試験)を行った。この耐熱性試験後、試験片の接着界面(感圧式接着剤層とPC板との界面)を目視にて観察し、3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:気泡や浮きが全く認めず、良好。
△:細かい気泡や浮きが若干端部に認められるが、実用上使用可能。
×:全面的に気泡や浮きが認められた。不良。
前記感圧式接着剤を、基材として厚さ38μmの剥離処理されたポリエチレンテレフタレートフィルム(セラピールMF:東レフィルム加工株式会社製)(以下、「剥離ライナー」という。)上に、乾燥後の厚さが25μmになるように塗工し、100℃で2分間熱風乾燥することで感圧式接着層を形成した。 次いで、この接着層に、光学フィルム(I)として、ポリビニルアルコール(PVA)系偏光フィルム(HLC2−5618:SANRITZ製)の両面をトリアセチルセルロース系フィルム(以下、「TACフィルム」という)で挟んだ積層構造の偏光フィルムの片面を貼り合せ、次いで、温度35℃相対湿度55%の条件で1週間熟成させて「剥離ライナー/感圧式接着層/TACフィルム/PVA/TACフィルム」という構成の光学用感圧式接着フィルム(偏光フィルム接着シートとも称す)を得た。
上記の偏光フィルム接着シートの吸収軸の軸方向が、長辺に対して45°の角度になるように、80mm×150mmに裁断した。次に、剥離ライナーを剥がし、露出した感圧式接着層を厚さ0.4mmの無アルカリガラス板の両面に、それぞれの吸収軸の軸方向が直交するように配置して、50℃雰囲気下で5Kg/cm2の圧力をかけ、20分間オートクレーブ内に保持して貼り合せた後、80℃の雰囲気中に500時間放置した後に室温に戻し、四隅もしくは周辺端部からの光漏れ現象の有無を目視で観察し、光漏れ性として3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:光漏れが認められない。良好。
△:光漏れがやや目立つが、実用上使用可能。
×:光漏れが極めて顕著である。不良。
上記の偏光フィルム接着シートを25mm×150mmの大きさに裁断し、剥離ライナーを剥がし、厚さ1.1mmのフロートガラス板にラミネータを用いて貼り付け、50℃で5気圧の条件のオートクレーブ内に20分保持させて、偏光フィルム接着シートとガラス板との光学用積層体を得た。
この積層体の偏光フィルムを180度方向に300mm/分の速度で引き剥がし、剥離後のガラス表面の曇りを目視で観察し、3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
○:曇りがなく、実用上全く問題がない。非常に良好。
△:若干曇りが認められるが、実用上問題ない。良好。
×:全面的に感圧式接着剤の転着が認められ、実用不可である。
上記の偏光フィルム接着シートの剥離ライナーを剥がし、露出した感圧式接着層を厚さ0.4mmの無アルカリガラス板の片面に、50℃雰囲気下で5Kg/cm2の圧力をかけ、20分間オートクレーブ内に保持して貼り合せた後、80℃の雰囲気中に500時間放置した(耐熱性試験)。また、同様にして、60℃−相対湿度90%の恒温恒湿槽に500時間放置した(耐湿熱性試験)。
放置後、室温に戻し、偏光フィルム接着シートの浮き・剥がれ、発泡、クラックの発生状態を目視で観察し、3段階で評価した。「○」または「△」評価の場合、実際の使用時に支障ない。
発泡とは、感圧式接着層とガラスとの界面(周辺端部以外)に比較的大きな気泡が発生している状態である。
浮き・剥がれとは、偏光フィルム接着シートがガラスから浮き上がり、剥がれてしまっている状態である。
クラックとは、偏光フィルム接着シートの周辺端部に、直径1mm以下の細かい気泡がスジ状に連なるように発生している状態である。
それぞれの評価基準は以下の通りである。
○:発泡、浮き・剥がれやクラックが全く発生せず。良好。
△:0.5mm以下の発泡、浮き、剥がれ、クラックのいずれかの軽微な発生が認められるが、実用上使用可能。
×:全面的に発泡、浮き、剥がれ、クラック等、顕著な発生が認められる。実用上使用不可。
・共重合体(A)
合成例:表1記載の各合成例で得られた共重合体
・化合物(B)
OPA:オルト燐酸、PPA:ポリ燐酸、MPK:メタ燐酸カリウム、PTA:燐酸トリエタノールアミン、PTE:燐酸トリエチル
・化合物(C)
MAS:3−アミノプロピルトリメトキシシラン、DAS:N−(2−アミノメチル)3−アミノプロピルトリメトキシシラン、EPS:3−グリシドキシプロピルトリメトキシシラン、CHS:2−(3,4−エポキシシクロヘキシル)エチルトリメトキシシラン
・化合物(D)
TDI/TMP:トルレンジイソシネートのトリメチロールプロパンアダクト体、XDI/TMP:キシリレンジイソシネートのトリメチロールプロパンアダクト体
・化合物(E)
HTS:ヘキシルトリメトキシシラン
・化合物(F)
TGXA:N,N,N’,N’−テトラグリシジル−m−キシリレンジアミン
・成分(Q)
AO50:フェノール系酸化防止剤「アデカスタブ AO−50(アデカ社製)」
・追加溶剤
EAc:酢酸エチル
Claims (8)
- 分子中に1個以上の水酸基を有するα,β−不飽和二重結合基含有化合物(a1)および分子中に水酸基を有しないα,β−不飽和二重結合基含有化合物(a2)を含む単量体混合物を重合してなり、重量平均分子量100,000〜2,000,000、水酸基価0.1〜50mgKOH/gである共重合体(A)と、P−OHを1つ以上有する化合物または加水分解によりP−OHを1つ以上形成し得る化合物(B)と、アミノ基またはエポキシ基を有するシラン化合物(C)と、ポリイソシアネート化合物(D)とを含有する感圧式接着剤。
- 共重合体(A)100重量部に対して、P−OHを1つ以上有する化合物または加水分解によりP−OHを1つ以上形成し得る化合物(B)を0.01〜10重量部、アミノ基またはエポキシ基を有するシラン化合物(C)を0.01〜10重量部、及びポリイソシアネート化合物(D)を0.1〜30重量部含有することを特徴とする請求項1記載の感圧式接着剤。
- P−OHを1つ以上有する化合物または加水分解によりP−OHを1つ以上形成し得る化合物(B)が、燐酸類(b1)であることを特徴とする請求項1または2記載の感圧式接着剤。
- 更に、アミノ基及びエポキシ基を有さないシラン化合物(E)を含有することを特徴とする請求項1〜3いずれか記載の感圧式接着剤。
- 請求項1〜4いずれか記載の感圧式接着剤を含有する接着層を、基材(G)の少なくとも一方の面に積層してなることを特徴とする感圧式接着フィルム。
- 基材(G)が、透明フィルム(H)であることを特徴とする請求項5記載の感圧式接着フィルム。
- 透明フィルム(H)が、光学フィルム(I)であることを特徴とする請求項6記載の感圧式接着フィルム。
- 光学フィルム(I)と、請求項1〜4いずれか記載の感圧式接着剤から形成されてなる接着層と、ガラスとが順次積層されてなる光学積層体。
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JP2019031586A (ja) * | 2017-08-04 | 2019-02-28 | 日本合成化学工業株式会社 | 粘着剤組成物、およびそれを用いてなる粘着剤、偏光板用粘着剤、ならびに画像表示装置 |
JP2021162820A (ja) * | 2020-04-03 | 2021-10-11 | 日本化薬株式会社 | 偏光膜用接着組成物および偏光膜 |
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JP2021162820A (ja) * | 2020-04-03 | 2021-10-11 | 日本化薬株式会社 | 偏光膜用接着組成物および偏光膜 |
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