JP2010278287A - 有機エレクトロルミネッセンス素子、該素子を用いた表示装置、照明装置及び有機エレクトロルミネッセンス素子の製造方法 - Google Patents
有機エレクトロルミネッセンス素子、該素子を用いた表示装置、照明装置及び有機エレクトロルミネッセンス素子の製造方法 Download PDFInfo
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- JP2010278287A JP2010278287A JP2009130166A JP2009130166A JP2010278287A JP 2010278287 A JP2010278287 A JP 2010278287A JP 2009130166 A JP2009130166 A JP 2009130166A JP 2009130166 A JP2009130166 A JP 2009130166A JP 2010278287 A JP2010278287 A JP 2010278287A
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Images
Abstract
【解決手段】陽極、陰極間に構成層として、ドーパント及びホストを含有する少なくとも1層の発光層を有する有機エレクトロルミネッセンス素子において、
該発光層は塗布法で成膜され、且つ、前記発光層は、X線回折で測定される微結晶を含有しないことを特徴とする有機エレクトロルミネッセンス素子。
【選択図】なし
Description
該発光層は塗布法で成膜され、且つ、前記発光層は、X線回折で測定される微結晶を含有しないことを特徴とする有機エレクトロルミネッセンス素子。
5.前記ドーパントがリン光発光を呈することを特徴とする前記2〜4のいずれか1項に記載の有機エレクトロルミネッセンス素子。
7.前記一般式(1)のM1がイリジウムであることを特徴とする前記6に記載の有機エレクトロルミネッセンス素子。
(a)該発光層は塗布法で成膜され、
(b)前記発光層は、X線回折で測定される微結晶を含有しない有機エレクトロルミネッセンス素子である。
次に、本発明の有機EL素子の層構成の好ましい具体例を以下に示すが、本発明はこれらに限定されない。
(ii)陽極/正孔輸送層/発光層/電子輸送層/陰極
(iii)陽極/正孔輸送層/発光層/正孔阻止層/電子輸送層/陰極
(iv)陽極/正孔輸送層/発光層/正孔阻止層/電子輸送層/陰極バッファー層/陰極
(v)陽極/陽極バッファー層/正孔輸送層/発光層/正孔阻止層/電子輸送層/陰極バッファー層/陰極
《上記の各層の形成法》
本発明の有機エレクトロルミネッセンス素子は、構成層である少なくとも1層の発光層が塗布法で成膜形成されていればよく、その他の層の形成方法は特に塗布成膜方法に限定されず、必要に応じて、蒸着法等を用いて成膜することもできる。
以下、本発明の有機EL素子の製造方法として、発光層の塗布成膜法を詳述する。本発明において塗布成膜法とは塗布後、乾燥が終了するまでの方法をいう。
発光層のX線回折測定には、例えば、株式会社リガク製薄膜構造評価装置ATX−Gを用いることができる。その測定条件を下記に示す。
本発明に係る発光層は、電極または電子輸送層、正孔輸送層から注入されてくる電子及び正孔が再結合して発光する層であり、発光する部分は発光層の層内であっても発光層と隣接層との界面であってもよい。
ここで、本発明においてホストとは、発光層に含有される化合物の内で室温(25℃)においてリン光発光のリン光量子収率が、0.1未満の化合物である。好ましくはリン光量子収率が0.01未満である。また、発光層に含有される化合物の中で、その層中での質量比が20%以上であることが好ましい。
一般式(a)で表される部分構造について説明する。
本発明に係るホスト化合物は、上記一般式(a)で表される部分構造を少なくとも3個有するが、好ましい態様としては、下記の一般式(a−1)、(a−2)または(a−3)で表される化合物が好ましい。
次にドーパントについて説明する。
注入層は必要に応じて設けることができ、陽極と発光層または正孔輸送層の間、及び陰極と発光層または電子輸送層との間に存在させてもよい。
阻止層は、有機化合物薄膜の構成層として必要に応じて設けられるものである。
正孔輸送層とは正孔を輸送する機能を有する正孔輸送材料からなり、広い意味で正孔注入層、電子阻止層も正孔輸送層の機能を有する。正孔輸送層は単層または複数層設けることができる。
電子輸送層とは電子を輸送する機能を有する材料からなり、広い意味で電子注入層、正孔阻止層も電子輸送層の機能を有する。電子輸送層は単層または複数層設けることができる。
有機EL素子における陽極としては、仕事関数の大きい(4eV以上)金属、合金、電気伝導性化合物及びこれらの混合物を電極物質とするものが好ましく用いられる。このような電極物質の具体例としては、Au等の金属、CuI、インジウムチンオキシド(ITO)、SnO2、ZnO等の導電性透明材料が挙げられる。また、IDIXO(In2O3−ZnO)等非晶質で透明導電膜を作製可能な材料を用いてもよい。
一方、陰極としては仕事関数の小さい(4eV以下)金属(電子注入性金属と称する)、合金、電気伝導性化合物及びこれらの混合物を電極物質とするものが用いられる。このような電極物質の具体例としては、ナトリウム、ナトリウム−カリウム合金、マグネシウム、リチウム、マグネシウム/銅混合物、マグネシウム/銀混合物、マグネシウム/アルミニウム混合物、マグネシウム/インジウム混合物、アルミニウム/酸化アルミニウム(Al2O3)混合物、インジウム、リチウム/アルミニウム混合物、希土類金属等が挙げられる。
本発明の有機EL素子に用いることのできる支持基板(以下、基体、基板、基材、支持体等とも言う)としては、ガラス、プラスチック等の種類には特に限定はなく、また透明であっても不透明であってもよい。支持基板側から光を取り出す場合には、支持基板は透明であることが好ましい。好ましく用いられる透明な支持基板としては、ガラス、石英、透明樹脂フィルムを挙げることができる。特に好ましい支持基板は、有機EL素子にフレキシブル性を与えることが可能な樹脂フィルムである。
本発明に用いられる封止手段としては、例えば、封止部材と電極、支持基板とを接着剤で接着する方法を挙げることができる。
有機層を挟み支持基板と対向する側の前記封止膜、あるいは前記封止用フィルムの外側に、素子の機械的強度を高めるために保護膜、あるいは保護板を設けてもよい。特に封止が前記封止膜により行われている場合には、その機械的強度は必ずしも高くないため、このような保護膜、保護板を設けることが好ましい。これに使用することができる材料としては、前記封止に用いたのと同様なガラス板、ポリマー板・フィルム、金属板・フィルム等を用いることができるが、軽量、且つ薄膜化ということからポリマーフィルムを用いることが好ましい。
有機EL素子は空気よりも屈折率の高い(屈折率が1.7〜2.1程度)層の内部で発光し、発光層で発生した光のうち15%から20%程度の光しか取り出せないことが一般的に言われている。これは、臨界角以上の角度θで界面(透明基板と空気との界面)に入射する光は、全反射を起こし素子外部に取り出すことができないことや、透明電極ないし発光層と透明基板との間で光が全反射を起こし、光が透明電極ないし発光層を導波し、結果として光が素子側面方向に逃げるためである。
本発明の有機EL素子は基板の光取り出し側に、例えば、マイクロレンズアレイ状の構造を設けるように加工したり、あるいは所謂集光シートと組み合わせることにより、特定方向、例えば、素子発光面に対し正面方向に集光することにより、特定方向上の輝度を高めることができる。
本発明の有機EL素子の作製方法の一例として、陽極/正孔注入層/正孔輸送層/発光層/電子輸送層/電子注入層/陰極からなる有機EL素子の作製法を説明する。
本発明においては、有機エレクトロルミネッセンス素子の有機層に要求される非常に薄く、且つ高平滑性の単層塗布膜を形成するために効果的な方法として、スロット型コータ塗布方法、またはインクジェット塗布方法が好ましい。下記に、スロット型コータ塗布方法、またはインクジェット塗布方法について詳細に説明する。
本発明に係る有機EL素子を適用した表示装置、照明装置について説明する。本発明に係る有機EL素子は、画像を投影するタイプのプロジェクション装置や、静止画像や動画像を直接視認するタイプの表示装置(ディスプレイ)として使用してもよいし、照明用や露光光源のような一種のランプとして使用してもよい。
《有機EL素子101の作製》
陽極として厚さ200μmのポリエーテルサルフォン(住友ベークライト製フィルム、以下、PESと略記する)上に、大気圧プラズマ重合法を用い透明ガスバリア性フィルムを作製した。
トルエン中に、HT−Aを0.45質量%、HT−Bを0.05質量%になるように溶解させ正孔輸送層用塗布液を調製した。
酢酸ブチル中に、H−31を1質量%、ペリレンを0.1質量%になるように溶解させ、発光層用塗布液を調製した。
2,2,3,3−テトラフルオロ−1−プロパノール中に、ET−Aを0.75質量%になるように溶解させ、電子輸送層用塗布液を調製した。
有機EL素子101の作製において、発光層の塗布乾燥条件を以下のように変更した以外は同様にして、有機EL素子102を作製した。
酢酸ブチル中に、H−31を1質量%、ペリレンを0.1質量%になるように溶解させ、発光層用塗布液を調製した。
有機EL素子101の作製において、表1のようにホスト、ドーパント、発光層の塗布溶媒および乾燥条件を変更した以外は同様にして、有機EL素子103〜110を作製した。
前記スロット型コータ塗布方法での有機EL素子101の作製において、以下の手順で正孔輸送層、発光層、電子輸送層を設けること以外は同様にして、有機EL素子201を作製した。
正孔輸送層用塗布液を有機EL素子101の作製で用いた溶液と同じように調製し、直径3mのバックアップロールを利用し、インクジェット塗布装置を利用して、塗布速度4m/分、乾燥後膜厚を正孔輸送層20nmになるように塗布した。
作製した有機エレクトロルミネッセンス素子(有機EL素子101〜110、有機EL素子201)について、下記のようにしてパワー効率及び発光寿命を評価した。
作製した有機エレクトロルミネッセンス素子に対し、2.5mA/cm2定電流を印加したときのパワー効率(lm/W)を測定した。なお、測定には分光放射輝度計CS−1000(コニカミノルタセンシング製)を用いた。有機エレクトロルミネッセンス素子(有機EL素子101〜110、有機EL素子201)のパワー効率は、有機EL素子101の測定値を100とした相対値で表した。
作製した有機エレクトロルミネッセンス素子に対し、正面輝度1000cd/m2となるような電流を与え、連続駆動した。正面輝度が初期の半減値(500cd/m2)になるまでに掛かる時間を求め、有機エレクトロルミネッセンス素子(有機EL素子101〜110、有機EL素子201)の寿命を有機EL素子101の測定値を100とした相対値で表した。
下記の表1に記載のホスト化合物の分子量計算においては、下記の原子量値を用い、また、高分子であるポリビニルカルバゾールについては、従来公知のGPC法による測定値(数平均分子量)を用いた。
H(水素原子)=1.00794
N(窒素原子)=14.00674
O(酸素原子)=15.9994
また、分子量の計算においては、上記の原子量値を用い、下4桁の値を四捨五入した値を用いた。
H−27(C42H26N2O)=574.681
H−31(C102H64N6)=1373.671
得られた結果を表1に示す。
2 バックアップロール
10、20、30 塗布ユニット
11、12 コータ
12、22 送液ポンプ
13、23、33 塗布液タンク
111、211 スリット
31 インクジェットユニット
311 インクジェットヘッド
Claims (11)
- 陽極、陰極間に構成層として、ドーパント及びホストを含有する少なくとも1層の発光層を有する有機エレクトロルミネッセンス素子において、
該発光層は塗布法で成膜され、且つ、前記発光層は、X線回折で測定される微結晶を含有しないことを特徴とする有機エレクトロルミネッセンス素子。 - 前記ホストの分子量が1500以下であることを特徴とする請求項1に記載の有機エレクトロルミネッセンス素子。
- 前記ホストの分子量が800以下であることを特徴とする請求項1または2に記載の有機エレクトロルミネッセンス素子。
- 前記ドーパントがリン光発光を呈することを特徴とする請求項2〜4のいずれか1項に記載の有機エレクトロルミネッセンス素子。
- 前記一般式(1)のM1がイリジウムであることを特徴とする請求項6に記載の有機エレクトロルミネッセンス素子。
- 請求項1〜7のいずれか1項に記載の有機エレクトロルミネッセンス素子を用いたことを特徴とする表示装置。
- 請求項1〜7のいずれか1項に記載の有機エレクトロルミネッセンス素子を用いたことを特徴とする照明装置。
- 請求項1〜7のいずれか1項に記載の有機エレクトロルミネッセンス素子の製造方法であって、該発光層の少なくとも1層が低分子有機化合物からなる発光層であり、該発光層の塗布、成膜及び乾燥後の最終的な膜厚の5%増の膜厚までの乾燥時間を20秒以下で前記発光層を形成する工程を有し、且つ、前記発光層中の低分子有機化合物の微結晶によるX線回折ピークが検出されないことを特徴とする有機エレクトロルミネッセンス素子の製造方法。
- 前記乾燥時間が10秒以下であることを特徴とする請求項10に記載の有機エレクトロルミネッセンス素子の製造方法。
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JP2012169518A (ja) * | 2011-02-16 | 2012-09-06 | Konica Minolta Holdings Inc | 有機エレクトロルミネッセンス素子及び有機エレクトロルミネッセンス素子の製造方法 |
WO2012137958A1 (ja) | 2011-04-07 | 2012-10-11 | 三菱化学株式会社 | 有機化合物、電荷輸送材料、該化合物を含有する組成物、有機電界発光素子、表示装置及び照明装置 |
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