JP5896388B2 - 接着フィルム及びこれを利用した有機電子装置の封止方法 - Google Patents
接着フィルム及びこれを利用した有機電子装置の封止方法 Download PDFInfo
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- JP5896388B2 JP5896388B2 JP2014540966A JP2014540966A JP5896388B2 JP 5896388 B2 JP5896388 B2 JP 5896388B2 JP 2014540966 A JP2014540966 A JP 2014540966A JP 2014540966 A JP2014540966 A JP 2014540966A JP 5896388 B2 JP5896388 B2 JP 5896388B2
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- adhesive film
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- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- HDUMBHAAKGUHAR-UHFFFAOYSA-J titanium(4+);disulfate Chemical compound [Ti+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O HDUMBHAAKGUHAR-UHFFFAOYSA-J 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 150000003681 vanadium Chemical class 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Description
[1.第1のサブ接着剤層溶液の製造]
エポキシ樹脂(YD−128、KUKDO化学)50g及びフェノキシ樹脂(YP−50、東都化成)50gを反応器内に投入し、メチルエチルケトン100gで希釈した。ここに、イミダゾール硬化剤(2MA.OK、四国化成)1gを添加した後、溶液を均質化した。
水分吸着剤として、MgO10gをメチルエチルケトンに20wt%の濃度で投入して水分吸着剤溶液を製造し、前記溶液をボールミル工程によって24時間ミリングした。また、これとは別に、常温で反応器にエポキシ樹脂(YD−128、KUKDO化学)60g及びフェノキシ樹脂(YP−50、東都化成)40gを投入し、メチルエチルケトン100gで希釈した。その後、イミダゾール硬化剤(2MA.OK、四国化成)1gを添加した後、溶液を均質化した。前記均質化された溶液にあらかじめ準備した水分吸着剤溶液を投入し、1時間の間高速撹拌して第2のサブ接着剤層の溶液を製造した。
前記準備した第1のサブ接着剤層の溶液を離型PETの離型面にコンマコートを使用して塗布し、乾燥器で130℃に3分間乾燥し、厚さが15μmの第1のサブ接着剤層を形成した。
実施例1の製造過程で、第2のサブ接着剤層の溶液のみで厚さ45μmの単一層構造を有した接着フィルムを製造した。
第1のサブ接着剤層溶液及び第2のサブ接着剤層溶液を下記のように製造したことの以外は、実施例1と同一に実施して多層構造の接着フィルムを製造した。
エポキシ樹脂(YD−128、KUKDO化学)25g、エポキシ樹脂(YD−014、KUKDO化学)35g及びフェノキシ樹脂(YP−50、東都化成)40gを反応器内に投入し、メチルエチルケトン100gで希釈した。ここに、イミダゾール硬化剤(2MA.OK、四国化成)1gを添加して溶液を均質化した。
水分吸着剤として、MgO10gをメチルエチルケトンに20wt%の濃度で投入して水分吸着剤溶液を製造し、前記溶液をボールミル工程によって24時間ミリングした。また、これとは別に、常温で反応器にエポキシ樹脂(YD−128、KUKDO化学)55g及びフェノキシ樹脂(YP−50、東都化成)45gを投入し、メチルエチルケトン100gで希釈した。その後、イミダゾール硬化剤(2MA.OK、四国化成)1gを添加した後、溶液を均質化した。前記均質化された溶液にあらかじめ準備した水分吸着剤溶液を投入し、1時間の間高速撹拌して第2のサブ接着剤層の溶液を製造した。
第1のサブ接着剤層溶液及び第2のサブ接着剤層溶液を下記のように製造したことの以外は、実施例1と同一に実施して多層構造の接着フィルムを製造した。
エポキシ樹脂(YD−128、KUKDO化学)50g及びフェノキシ樹脂(YP−50、東都化成)50gを反応器内に投入し、メチルエチルケトン100gで希釈した。ここに、イミダゾール硬化剤(2MA.OK、四国化成)1gを添加して溶液を均質化し、ナノシリカ(Aerosil R972、エボニック)3gを均一に分散させた。
水分吸着剤として、MgO10gをメチルエチルケトンに20wt%の濃度で投入して水分吸着剤溶液を製造し、前記溶液をボールミル工程によって24時間ミリングした。また、これとは別に、常温で反応器にエポキシ樹脂(YD−128、KUKDO化学)50g及びフェノキシ樹脂(YP−50、東都化成)50gを投入し、メチルエチルケトン100gで希釈した。その後、イミダゾール硬化剤(2MA.OK、四国化成)1gを添加した後、溶液を均質化した。前記均質化された溶液にあらかじめ準備した水分吸着剤溶液を投入し、1時間の間高速撹拌して第2のサブ接着剤層の溶液を製造した。
実施例1の製造過程で、第1のサブ接着剤層溶液に使用したフェノキシ樹脂(YP−50、東都化成)の含量を30gに変更したことの以外は、実施例1と同一に実施して多層構造の接着フィルムを製造した。
実施例2の製造過程で、第2の接着剤層溶液においてエポキシ樹脂、フェノキシ樹脂を、各々エポキシ樹脂(YD−128、KUKDO化学)20g及びフェノキシ樹脂(YP−50、東都化成)80gに変更して使用したことの以外は、実施例2と同一に実施して厚さ45μmの単一層構造を有する接着フィルムを製造した。
実施例2の製造過程で、第2の接着剤層溶液においてエポキシ樹脂、フェノキシ樹脂を、各々エポキシ樹脂(YD−128、KUKDO化学)80g及びフェノキシ樹脂(YP−50、東都化成)20gに変更して使用したことの以外は、実施例2と同一に実施して厚さ45μmの単一層構造を有する接着フィルムを製造した。
実施例1の製造過程で、第2のサブ接着剤層溶液に添加する水分吸着剤溶液の製造時に、MgOの含量を70gに変更したことの以外は、実施例1と同一に実施して多層構造の接着フィルムを製造した。
実施例1〜実施例4及び比較例1〜比較例5の接着フィルムの接着剤層の温度による粘度をARESで測定し、常温及び80℃での粘度を下記表1に示した。
ARESを利用して実施例1、実施例3、実施例4及び比較例1、比較例5の接着フィルムの接着剤層の二つのサブ接着剤層の粘度を各々測定し、80℃での粘度及びその差を下記表2に示した。
実施例1〜実施例4及び比較例1〜比較例5の接着フィルムの接着剤層が、合着温度である80℃で接着フィルムの初期先端から離脱する程度を顕微鏡を利用して測定し、下記表3に示した。
実施例1〜実施例4及び比較例1〜比較例5の接着フィルムの水分遮断特性を調査するために、カルシウムテストを進行した。具体的には、100mm×100mmサイズのガラス基板上にカルシウム(Ca)を5mm×5mmのサイズ及び100nmの厚さで9個(9 spot)蒸着し、これとは別に、実施例1〜実施例4及び比較例1〜実施例5の接着フィルムが転写されたカバーガラスを各カルシウム蒸着箇所に真空プレス(Vacuum press)を使用して、80℃で1分間圧着した。その後、高温乾燥器内で100℃に3時間硬化させた後、11mm×11mmサイズで封止されたカルシウム(Ca)試片を各々切断した。得られた試片を恒温恒湿チャンバで85℃の温度及び85%R.H.の環境に放置した後、水分浸透による酸化反応によってカルシウムが透明になり始めた時点を評価し、下記表4に示した。
実施例1〜実施例4及び比較例1〜比較例5の接着フィルムを利用して3インチの有機発光パネルを製造する時、合着時にバブルが残留する程度を顕微鏡で観察し、下記表5に示した。
22 接着剤層
31 基板
32 接着フィルム
33 有機電子装置
34 第2の基板(カバー基板)
Claims (23)
- 有機電子装置を封止する接着フィルムであって、
前記接着フィルムは、硬化性樹脂及び前記硬化性樹脂100重量部に対して、5重量部〜100重量部の水分吸着剤を含む接着剤層を含み、
前記接着剤層は、未硬化状態で30℃〜130℃の範囲の任意の温度での粘度が101〜106Pa・sであり、15℃から35℃の範囲の任意の温度の常温での粘度は、106Pa・s以上であり、
前記接着剤層は、少なくとも2層のサブ接着剤層からなり、各々のサブ接着剤層間の未硬化状態で30℃〜130℃の範囲の任意の温度での粘度差が、30Pa・s未満であることを特徴とする接着フィルム。 - 前記接着フィルムを未硬化状態で50℃〜100℃の温度範囲で被着剤にラミネーションする場合、前記接着剤層の接着剤の離脱する程度が元々の位置から1mm以下であることを特徴とする請求項1に記載の接着フィルム。
- 前記接着フィルムを未硬化状態で50℃〜100℃の範囲の任意の温度で被着剤にラミネーションする場合、前記各々のサブ接着剤層の接着剤が離脱する程度の差が、0μm〜300μmであることを特徴とする請求項1に記載の接着フィルム。
- 前記各々のサブ接着剤層の中で少なくとも1層以上のサブ接着剤層が硬化性樹脂及び水分吸着剤を含むことを特徴とする請求項1に記載の接着フィルム。
- 前記硬化性樹脂は、硬化状態で透湿度が20g/m2・day以下であることを特徴とする請求項1に記載の接着フィルム。
- 硬化性樹脂は、熱硬化型樹脂または光硬化型樹脂であることを特徴とする請求項1に記載の接着フィルム。
- 前記硬化性樹脂は、グリシジル基、イソシアネート基、ヒドロキシ基、カルボキシル基、アミド基、エポキシド基、環状エーテル基、スルフィド基、アセタール基またはラクトン基から選択される一つ以上の硬化性官能基を含むことを特徴とする請求項1に記載の接着フィルム。
- 前記硬化性樹脂は、分子構造内に芳香族基を含むエポキシ樹脂であることを特徴とする請求項1に記載の接着フィルム。
- 前記水分吸着剤は、アルミナ、金属酸化物、金属塩または五酸化リンであることを特徴とする請求項1に記載の接着フィルム。
- 前記水分吸着剤は、P2O5、Li2O、Na2O、BaO、CaO、MgO、Li2SO4、Na2SO4、CaSO4、MgSO4、CoSO4、Ga2(SO4)3、Ti(SO4)2、NiSO4、CaCl2、MgCl2、SrCl2、YCl3、CuCl2、CsF、TaF5、NbF5、LiBr、CaBr2、CeBr3、SeBr4、VBr3、MgBr2、BaI2、MgI2、Ba(ClO4)2及びMg(ClO4)2からなる群より選択される一つ以上であることを特徴とする請求項1に記載の接着フィルム。
- 前記接着剤層は、フィラーをさらに含むことを特徴とする請求項1に記載の接着フィルム。
- 前記フィラーは、クレイ、タルク、シリカ、硫酸バリウム、水酸化アルミニウム、炭酸カルシウム、炭酸マグネシウム、ゼオライト、ジルコニア、チタニアまたはモンモリルロナイトからなる群より選択される一つ以上であることを特徴とする請求項11に記載の接着フィルム。
- 前記接着剤層は、硬化性樹脂100重量部に対して、1重量部〜50重量部のフィラーを含むことを特徴とする請求項11に記載の接着フィルム。
- 前記接着剤層は、硬化剤をさらに含むことを特徴とする請求項1に記載の接着フィルム。
- 前記硬化剤は、アミン系化合物、イミダゾール系化合物、フェノール系化合物、リン系化合物または酸無水物系化合物であることを特徴とする請求項14に記載の接着フィルム。
- 前記接着剤層は、硬化性樹脂100重量部に対して、1重量部〜10重量部の硬化剤を含むことを特徴とする請求項14に記載の接着フィルム。
- 前記接着剤層は、高分子量樹脂をさらに含むことを特徴とする請求項1に記載の接着フィルム。
- 基板、前記基板上に形成された有機電子装置、及び前記有機電子装置の全面をカバーするように有機電子装置を封止する請求項1〜請求項17のいずれか一項に記載の接着フィルムを含むことを特徴とする有機電子装置の封止製品。
- 前記接着フィルムの上部に第2の基板をさらに含み、前記接着フィルムが前記第2の基板と前記基板とを接着することを特徴とする請求項18に記載の有機電子装置の封止製品。
- 上部に有機電子装置が形成された基板に、請求項1〜請求項17のいずれか一項に記載の接着フィルムを、前記接着フィルムの接着剤層が前記有機電子装置の全面をカバーするように適用する段階及び前記接着剤層を硬化する段階を含むことを特徴とする有機電子装置の封止方法。
- 前記接着フィルムを前記有機電子装置に適用する段階は、接着フィルムのホットロールラミネート、熱圧着または真空圧着方法で実行することを特徴とする請求項20に記載の有機電子装置の封止方法。
- 前記接着フィルムを前記有機電子装置に適用する段階は、50℃〜100℃の温度で実行することを特徴とする請求項20に記載の有機電子装置の封止方法。
- 前記硬化段階は、70℃〜110℃の温度範囲で加熱するかUVを照射して実行することを特徴とする請求項20に記載の有機電子装置の封止方法。
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