JP6474914B2 - 接着剤組成物 - Google Patents
接着剤組成物 Download PDFInfo
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- JP6474914B2 JP6474914B2 JP2017549727A JP2017549727A JP6474914B2 JP 6474914 B2 JP6474914 B2 JP 6474914B2 JP 2017549727 A JP2017549727 A JP 2017549727A JP 2017549727 A JP2017549727 A JP 2017549727A JP 6474914 B2 JP6474914 B2 JP 6474914B2
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Description
本出願は2015年03月24日付け韓国特許出願第10−2015−0040738号に基づいた優先権の利益を主張し、該当韓国特許出願の文献に開示されたすべての内容は本明細書の一部として含まれる。
本出願は接着剤組成物、これを含む有機電子装置および前記有機電子装置の製造方法に関するものである。
F≧600gf
T=V0.5/V5
常温でオレフィン系樹脂としてポリイソブチレン樹脂(BASF社B14、Mw=65,000)、熱硬化性樹脂として水添BPAエポキシ樹脂(DIC社Epiclon 850、Mw=376)および光硬化性化合物としてエポキシ変性アクリレート(Sartomer、CN2003)を70:20:10(B14:Epiclon850:CN2003)の重量比率で混合容器に投入した。ラジカル開始剤として2、2−ジメトキシ−1、2−ジフェニルエタン−1−オン(Irgacure651、Ciba)を前記光硬化性化合物100重量部に対して1重量部を前記容器に投入し、熱硬化剤としてイミダゾール系硬化剤(2P4MHZ)を熱硬化性樹脂100重量部に対して5重量部投入した。一方、水分吸着剤としてカルシウムオキサイド(CaO、Aldrich)を前記オレフィン系樹脂100重量部に対して10重量部追加で容器に投入した。
オレフィン系樹脂、熱硬化性樹脂および光硬化性化合物を50:20:30の重量割合で混合容器に投入したことを除いては、実施例1と同じ方法で接着剤組成物を製造した。
オレフィン系樹脂、熱硬化性樹脂および光硬化性化合物を60:20:20の重量割合で混合容器に投入したことを除いては、実施例1と同じ方法で接着剤組成物を製造した。
オレフィン系樹脂、熱硬化性樹脂および光硬化性化合物を30:20:50の重量割合で混合容器に投入したことを除いては、実施例1と同じ方法で接着剤組成物を製造した。
オレフィン系樹脂、熱硬化性樹脂および光硬化性化合物を40:50:10の重量割合で混合容器に投入したことを除いては、実施例1と同じ方法で接着剤組成物を製造した。
オレフィン系樹脂および熱硬化性樹脂を80:20の重量割合で混合容器に投入し、光硬化性化合物は投入しなかったことを除いては、実施例1と同じ方法で接着剤組成物を製造した。
実施例1のオレフィン系樹脂の代わりにn−ブチルアクリレートおよびアクリル酸を95:5の重量比率で混合して共重合させたアクリル共重合体を使用し、前記アクリル共重合体、熱硬化性樹脂および光硬化性化合物を60:20:20の重量割合で混合容器に投入したことを除いては、実施例1と同じ方法で接着剤組成物を製造した。
実施例および比較例で製造した接着剤組成物を0.7T Soda−Limeガラスに塗布して同じガラスで圧着してサンプルを製造した後、メタルハライドランプを通じてUV−A領域帯の波長範囲を有する光を3J/cm2の光量で照射する。そして、前記サンプルの最外郭部位をペンで表示した後、100℃のオーブンに2時間の間硬化した後、初期形状の維持の有無を観察した(比較例1は100℃のオーブンに3時間の間熱硬化だけを進行)。目視で観察した結果、光照射直後の最外郭の形状がそのまま非常に良好に維持された場合◎、ペンで表示した境界を越えたが最外郭の形状がほとんど維持された場合O、ペンで表示した境界を越えて拡散されて最外郭の形状が維持されていない場合、Xで表示した。
実施例および比較例の接着剤組成物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めた。具体的には、100mm×100mm大きさのガラス基板上にカルシウム(Ca)を5mm×5mmの大きさおよび100nmの厚さで7個(7 spot)蒸着し、実施例および比較例の接着剤組成物をディスペンサを用いてカルシウム蒸着部から3mm間隔で周縁部(周辺部)に塗布した後、カバーガラスを各カルシウム蒸着箇所に合着後、接着剤組成物の幅が3mmになるように押さえ、5J/cm2でUV−A波長領域の光を照射した。その後、高温乾燥器内で100℃で3時間の間硬化させた後で(比較例1は100℃のオーブンに3時間の間熱硬化だけを進行)、14mm×14mmの大きさで封止されたカルシウム(Ca)試片をそれぞれ切断した。得られた試片を恒温恒湿チャンバーにて85℃の温度および85% R.H.の環境で1000時間の間放置した後、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て下記の表1に示した。
具体的には、実施例および比較例の接着剤組成物を横5cm縦9cmの大きさの下部ガラス上に円形に塗布し、前記接着剤組成物上に横5cm縦9cmの大きさの上部ガラスを前記下部ガラスと横方向に5cm縦方向に2.5cmだけ重ね合わせられるように積層して、前記接着剤組成物が17mmの直径および20μmの厚さの円形に重ね合わせられた試片を製造し、前記試片にUV−A領域帯の波長範囲を有する光を3J/cm2の光量で照射した後、前記上部ガラスおよび下部ガラスをテクスチャー・アナライザー(Texture Analyser−XT2 plus)に固定させ、25℃の温度下にて上部ガラスを縦方向に0.1mm/secの速度で引っ張った時、測定された力の最大値を測定してせん断強度Fと定義した。
10:側面封止層
11:前面封止層
21:基板
22:カバー基板
23:有機電子素子
Claims (15)
- 透湿度が50g/m2・day以下であるオレフィン系樹脂、熱硬化性樹脂および光硬化性化合物を含み、オレフィン系樹脂、熱硬化性樹脂および光硬化性化合物はそれぞれ40〜90重量部、5〜50重量部および1〜40重量部で含まれ、下記の一般式1を満足する、有機電子素子封止用接着剤組成物:
[一般式1]
F≧600gf
前記一般式1でFはせん断強度であり、前記接着剤組成物を横5cm縦9cmの大きさの下部ガラス上に円形に塗布し、前記接着剤組成物上に横5cm縦9cmの大きさの上部ガラスを前記下部ガラスと横方向に5cm縦方向に2.5cmだけ重ね合わせられるように積層して、前記接着剤組成物が17mmの直径および20μmの厚さの円形に重ね合わせられた試片を製造し、前記試片にUV−A領域帯の波長範囲を有する光を3J/cm2の光量で照射した後、前記上部ガラスおよび下部ガラスをテクスチャー・アナライザー(Texture Analyser−XT2 plus)に固定させ、25℃の温度下で上部ガラスを縦方向に0.1mm/secの速度で引っ張った時、測定された力の最大値を意味する。 - オレフィン系樹脂は重量平均分子量が10万以下である、請求項1に記載の接着剤組成物。
- 熱硬化性樹脂は熱硬化性官能基を一つ以上含む樹脂である、請求項1に記載の接着剤組成物。
- 熱硬化性官能基はエポキシ基、グリシジル基、イソシアヌレート基、ヒドロキシ基、カルボキシル基 またはアミド基を含む、請求項3に記載の接着剤組成物。
- 熱硬化性樹脂はオレフィン系樹脂100重量部に対して10〜70重量部で含まれる、請求項1に記載の接着剤組成物。
- 熱硬化剤をさらに含む、請求項1に記載の接着剤組成物。
- 熱硬化剤は潜在性硬化剤である、請求項6に記載の接着剤組成物。
- 光硬化性化合物は多官能性の活性エネルギー線重合性化合物を含む、請求項1に記載の接着剤組成物。
- 光硬化性化合物はオレフィン系樹脂100重量部に対して10〜100重量部で含まれる、請求項1に記載の接着剤組成物。
- 光硬化性化合物100重量部に対して0.1〜20重量部の光ラジカル開始剤をさらに含む、請求項1に記載の接着剤組成物。
- 水分吸着剤をさらに含む、請求項1に記載の接着剤組成物。
- 水分吸着剤はオレフィン系樹脂100重量部に対して5〜100重量部で含まれる、請求項11に記載の接着剤組成物。
- 基板;基板上に形成された有機電子素子;および前記基板の周縁部上に前記有機電子素子の側面を囲むように形成され、請求項1に記載された接着剤組成物を含む側面封止層を含む、有機電子装置。
- 有機電子素子の前面をカバーする前面封止層をさらに含み、前記前面封止層および側面封止層は同一平面上に存在する、請求項13に記載の有機電子装置。
- 上部に有機電子素子が形成された基板の周縁部上に、請求項1に記載された接着剤組成物を前記有機電子素子の側面を囲むように塗布する段階;前記接着剤組成物に光を照射する段階;および前記接着剤組成物に熱を加える段階を含む、有機電子装置の製造方法。
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