JP7353478B2 - 封止フィルム - Google Patents
封止フィルム Download PDFInfo
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- JP7353478B2 JP7353478B2 JP2022522690A JP2022522690A JP7353478B2 JP 7353478 B2 JP7353478 B2 JP 7353478B2 JP 2022522690 A JP2022522690 A JP 2022522690A JP 2022522690 A JP2022522690 A JP 2022522690A JP 7353478 B2 JP7353478 B2 JP 7353478B2
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Description
本出願は、2019年10月28日に出願された大韓民国特許出願第10-2019-0134808号に基づく優先権の利益を主張し、当該大韓民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組み込まれる。
本発明は、封止フィルム、それを含む有機電子装置及び前記有機電子装置の製造方法に関する。
封止層の製造
予め準備されたメタル層(SUS430、厚さ80μm)上に、前記封止層の第2層に付着された離型処理されたPETを剥離させ、ロールツーロール(Roll-to-Roll)工程で70℃でラミネーションして、第2層がメタル層と接するように封止フィルムを製造した。
CaO粒子の平均粒径を2.5μmに変更したこと以外は、実施例1と同一の方法によって有機電子素子封止用フィルムを製造した。
CaO粒子の平均粒径を1.5μmに変更したこと以外は、実施例1と同一の方法によって有機電子素子封止用フィルムを製造した。
CaO粒子の平均粒径を6μmに変更したこと以外は、実施例1と同一の方法によって有機電子素子封止用フィルムを製造した。
Ni粒子の平均粒径を2μmに変更したこと以外は、実施例1と同一の方法によって有機電子素子封止用フィルムを製造した。
CaO粒子の含量を1kgに変更したこと以外は、実施例1と同一の方法によって有機電子素子封止用フィルムを製造した。
実施例及び比較例で用いた輝点防止剤のアウトガスに対する吸着エネルギーを密度汎関数論(density functional theory)基盤の電子構造計算を通じて計算した。結晶形構造を有する輝点防止剤の最密充填面が表面に現われる2次元slab構造を作った後に構造最適化を進行し、この真空状態の表面上に輝点原因分子が吸着された構造に対する構造最適化を進行した後、この二つのシステムの総エネルギー(total energy)差から輝点原因分子の総エネルギーを引いた値を吸着エネルギーとして定義した。それぞれのシステムに対する総エネルギーの計算のために電子-電子間の相互作用を模した交換相関(exchange-correlation)でGGA(generalized gradient approximation)系列の関数であるrevised-PBE関数を用い、電子運動エネルギー(kinetic energy)のカットオフ(cutoff)は、500eVを用い、逆格子空間(reciprocal space)の原点に該当するガンマ点(gamma point)のみを含ませて計算した。各システムの原子構造を最適化するために共役勾配(conjugate gradient)法を用い、原子間の力が0.01eV/Å以下になるまで繰り返し計算を行った。一連の計算は、常用コードであるVASPを通じて行われた。実施例及び比較例で用いられた輝点防止剤であるNiのNH3及びHに対する吸着エネルギーは、それぞれ-0.54及び-2.624であった。
実施例で製造した封止フィルムに対して封止層を1.5cm x 1.5cmで裁断してサンプルとして製造した後、トルエン3gにとかす(sonication 20min、50℃)。その後、300メッシュのナイロンフィルタによりフィルタリングした後、フィルタを通過した溶液に対して粒度を測定する。粒度測定方法は、ISO 13320:2009によって認証された技術が適用された器機であるMastersizer(Malvern Panalytical Ltd)を用いた。ソフトウェア上の設定で粒子類型を非球形で入力した後に溶媒をトルエンで入力し、レベルセンサ閾値を20で入力する。その後、バックグラウンド測定時間とサンプル測定時間をそれぞれ10秒、5秒で入力し、測定オプスキュレーションの下限と上限をそれぞれ1と20パーセントで入力した後、測定を最小3回施行するように入力して設定を終える。トルエン溶媒を装置に投入して2000~3000RPMで循環した後、イニシャライズ及びバックグラウンド数値測定を施行し、前記フィルタリングされた輝点防止剤と水分吸着剤の分散溶液を投入して、ソフトウェア画面上のオプスキュレーション値を3~7パーセントの間となるようにした後に測定を施行した。測定過程で、粒径30μm以上領域で一定ではない頻度とシグナルで現われるピークは、ほこりなどによるノイズであると判断して除去した後、結果値を導出した。
薄膜トランジスタガラス基板上に有機電子素子を蒸着した後、実施例及び比較例で製造した封止フィルムを真空合着機を用いて25℃、真空度50mtorr、0.4MPaの条件で、前記素子上に有効ベゼルを長さが3~4mmとなるように合着して65インチサイズの有機電子パネルを製造した。前記有効ベゼルは、ガラス基板上の縁に有機電子素子なしに封止層がガラス基板と直接接することになる縁領域の外辺と内辺の距離を意味する。前記製造したパネルを85℃及び相対湿度85%で1000時間駆動した後、暗室で点灯して肉眼で不良画素の発生有無を確認した。不良画素は、周辺に比べて明るい輝点や周辺に比べて暗い輝点を不良画素であると判断した。不良画素が3個以下である場合、O、不良画素が10個未満である場合、Δ、不良画素が10個以上発生した場合、Xに分類した。
前記実験例3の測定が完了したパネルの縁領域で水分が浸透した長さとして透明度が増加した領域の外辺と内辺の距離を測定した。水分吸着剤は、水分との反応により透明度が増加して水分が浸透した領域と浸透していない領域を透明度差の境界点で区分した。水分遮断距離が2mm以下である場合、O、2mmを超過して高温、高湿耐久信頼性が良好ではない場合、Xに分類した。
2、4:封止層
3:輝点防止剤
5:水分吸着剤
21:基板
22:有機電子素子
12:封止層
13:メタル層
Claims (18)
- 水分吸着剤、輝点防止剤及び封止樹脂を含む封止層を含む封止フィルムであって、
前記封止層を有機溶剤に溶解させた後、300メッシュのナイロンフィルタでフィルタリングして通過されたサンプルに含まれている前記水分吸着剤と前記輝点防止剤に対して粒度分析した結果、下記一般式1による値が2.4~3.6の範囲を満足し、D50粒度分析による前記水分吸着剤の平均粒径に対する前記輝点防止剤の平均粒径の比が0.15~2.0であることを特徴とする、封止フィルム:
- 前記水分吸着剤は、粒径が100~15000nmの範囲内であることを特徴とする、請求項1に記載の封止フィルム。
- 前記輝点防止剤の粒径は、10nm~30μmの範囲内であることを特徴とする、請求項1に記載の封止フィルム。
- 前記輝点防止剤は、密度汎関数理論近似法(Density Functional Theory)によって計算されたアウトガスに対する吸着エネルギーが0eV以下であることを特徴とする、請求項1に記載の封止フィルム。
- 前記アウトガスは、酸素、H原子、H2分子又はNH3を含むことを特徴とする、請求項4に記載の封止フィルム。
- 前記水分吸着剤は、化学反応性吸着剤を含むことを特徴とする、請求項1に記載の封止フィルム。
- 前記水分吸着剤は、封止樹脂100重量部に対して5~250重量部の範囲内で含まれることを特徴とする、請求項1に記載の封止フィルム。
- 前記輝点防止剤は、封止樹脂100重量部に対して1~150重量部で含まれることを特徴とする、請求項1に記載の封止フィルム。
- 前記封止樹脂は、硬化性樹脂又は架橋可能な樹脂であることを特徴とする、請求項1に記載の封止フィルム。
- 前記封止層は、粘着付与剤をさらに含むことを特徴とする、請求項1に記載の封止フィルム。
- 前記封止層は、活性エネルギー線重合性化合物をさらに含むことを特徴とする、請求項1に記載の封止フィルム。
- 前記封止層の表面又は断面をSEMを通じて加速電圧15kVで後方散乱イメージ(Backscattered electron image)で確認したとき、100nm~20μmの粒径を有する水分吸着剤及び輝点防止剤が全体表面又は断面の面積で10%以上の範囲内であることを特徴とする、請求項1に記載の封止フィルム。
- 前記封止層の表面又は断面をSEMを通じて加速電圧15kVで後方散乱イメージ(Backscattered electron image)で確認したとき、輝点防止剤が占める面積は、水分吸着剤が占める面積より小さいことを特徴とする、請求項1に記載の封止フィルム。
- 前記封止層は、基板上に形成された有機電子素子の全面を密封することを特徴とする、請求項1に記載の封止フィルム。
- 前記封止層の一面に形成されるメタル層をさらに含むことを特徴とする、請求項1に記載の封止フィルム。
- 基板;前記基板上に形成された有機電子素子;及び前記有機電子素子を封止する請求項1に記載の封止フィルムを含むことを特徴とする、有機電子装置。
- 前記有機電子素子は、一対の電極、少なくとも発光層を含む有機層及びパッシベーション膜を含むことを特徴とする、請求項16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に請求項1に記載の封止フィルムが前記有機電子素子をカバーするように適用するステップを含むことを特徴とする、有機電子装置の製造方法。
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