JP2013004335A - 透明電極及び有機エレクトロルミネッセンス素子 - Google Patents
透明電極及び有機エレクトロルミネッセンス素子 Download PDFInfo
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- JP2013004335A JP2013004335A JP2011134872A JP2011134872A JP2013004335A JP 2013004335 A JP2013004335 A JP 2013004335A JP 2011134872 A JP2011134872 A JP 2011134872A JP 2011134872 A JP2011134872 A JP 2011134872A JP 2013004335 A JP2013004335 A JP 2013004335A
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- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 229910001456 vanadium ion Inorganic materials 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
【解決手段】基板上に、導電性ポリマー及び水系溶剤に分散可能なポリマーを含有する透明電極において、前記ポリマーが解離性基含有自己分散型ポリマーであり、かつガラス転移温度が、25℃以上80℃以下であることを特徴とする透明電極。
【選択図】なし
Description
本発明は、透明な基材上に導電性ポリマー及びバインダー樹脂を有する透明導電層を有する透明電極において、該バインダー樹脂が、ガラス転移温度が25℃以上80℃以下で、水系溶剤に分散可能なポリマーで、これらが解離性基含有自己分散型ポリマーであることを特徴とする。
本発明において、「導電性」とは、電気が流れる状態を指し、JIS K 7194の「導電性プラスチックの4探針法による抵抗率試験方法」に準拠した方法で測定したシート抵抗が1×108Ω/□より低いことをいう。
本発明に用いるπ共役系導電性高分子としては、特に限定されず、ポリチオフェン(基本のポリチオフェンを含む、以下同様)類、ポリピロール類、ポリインドール類、ポリカルバゾール類、ポリアニリン類、ポリアセチレン類、ポリフラン類、ポリパラフェニレンビニレン類、ポリアズレン類、ポリパラフェニレン類、ポリパラフェニレンサルファイド類、ポリイソチアナフテン類、ポリチアジル類、の鎖状導電性ポリマーを利用することができる。中でも、導電性、透明性、安定性等の観点からポリチオフェン類やポリアニリン類が好ましく、ポリエチレンジオキシチオフェンが最も好ましい。
π共役系導電性高分子の形成に用いられる前駆体モノマーは、分子内にπ共役系を有し、適切な酸化剤の作用によって高分子化した際にもその主鎖にπ共役系が形成されるものである。例えば、ピロール類及びその誘導体、チオフェン類及びその誘導体、アニリン類及びその誘導体等が挙げられる。
本発明に係る導電性ポリマーに用いられるポリ陰イオンは、置換もしくは未置換のポリアルキレン、置換もしくは未置換のポリアルケニレン、置換もしくは未置換のポリイミド、置換もしくは未置換のポリアミド、置換もしくは未置換のポリエステル及びこれらの共重合体であって、アニオン基を有する構成単位とアニオン基を有さない構成単位とからなるものである。
基材は、導電層を担持しうる板状体であり、透明電極を得るためには、JIS K 7361−1:1997(プラスチック−透明材料の全光線透過率の試験方法)に準拠した方法で測定した可視光波長領域における全光線透過率が80%以上のものが好ましく用いられる。
図1において、1はパターン状に形成された金属材料からなる第1導電層、2は導電性ポリマー及び水系溶媒に分散可能な解離性基含有自己分散型ポリマーを含有する第2導電層、3は基材を示す。
本発明の導電層は、上記の導電性ポリマー、水系溶媒に分散可能な解離性基含有自己分散型ポリマーを含有する塗布液を、基材上に塗布し、加熱、乾燥して形成する。導電層に金属材料からなる細線部を有する場合は、この金属材料からなる細線部が形成された基材上に塗布し、加熱、乾燥して形成する。この時パターン形成された金属細線部を完全に被覆してもよいし、一部を被覆または接触してもよい。
本発明の有機EL素子は、本発明の透明電極を具備することを特徴とする。
[ポリ−2−ヒドロキシエチルアクリレート(P−1)の合成]
300mlナスフラスコに2−ヒドロキシエチルアクリレート(東京化成社製)5.0g(43.1mmol、Fw116.12)、2,2′−アゾビス(2−メチルイソプロピオニトリル)0.7g(4.3mmol、Fw164.21)及びテトラヒドロフラン100mlを加え、8時間加熱還流した。その後、溶液を室温まで冷却し、激しく攪拌されたメチルエチルケトン2.0L中へ滴下した。反応溶液を1時間攪拌後、メチルエチルケトンをデカンテーションし、メチルエチルケトン100mlで壁面に付着した重合体を3回洗浄した。ポリマーはテトラヒドロフラン100mlに溶解し、200mlフラスコへ移し、ロータリーエバポレーターによりテトラヒドロフランを減圧留去した。その後、80℃3時間減圧することで、残留しているTHFを留去し、数平均分子量57,800、分子量分布1.24のP−1を4.1g(収率82%)得た。
装置:Waters2695(Separations Module)
検出器:Waters 2414(Refractive Index Detector)
カラム:Shodex Asahipak GF−7M HQ
溶離液:ジメチルホルムアミド(20mM LiBr含有)
流速:1.0ml/min
温度:40℃
〈基板の作製〉
厚み100μmのポリエチレンテレフタレートフィルム(コスモシャインA4100、東洋紡績株式会社製)の下引き加工していない面に、JSR株式会社製UV硬化型有機/無機ハイブリッドハードコート材:OPSTAR Z7501を塗布、乾燥後の平均膜厚が4μmになるようにワイヤーバーで塗布した後、80℃、3分で乾燥後、空気雰囲気下、高圧水銀ランプ使用して硬化条件1.0J/cm2で硬化を行い、平滑層を形成した。
パーヒドロポリシラザン(PHPS、AZエレクトロニックマテリアルズ(株)製アクアミカ NN320)の20質量%ジブチルエーテル溶液をワイヤレスバーにて、乾燥後の(平均)膜厚が、0.30μmとなるように塗布し、塗布試料を得た。
得られた塗布試料を温度85℃、湿度55%RHの雰囲気下で1分処理し、乾燥試料を得た。
乾燥試料をさらに温度25℃、湿度10%RH(露点温度−8℃)の雰囲気下に10分間保持し、除湿処理を行った。
除湿処理を行った試料を下記の条件で改質処理を行い、ガスバリア層を形成した。改質処理時の露点温度は−8℃で実施した。
株式会社エム・ディ・コム製エキシマ照射装置MODEL:MECL−M−1−200、波長172nm、ランプ封入ガス Xe
稼動ステージ上に固定した試料を以下の条件で改質処理を行った。
エキシマ光強度 60mW/cm2(172nm)
試料と光源の距離 1mm
ステージ加熱温度 70℃
照射装置内の酸素濃度 1%
エキシマ照射時間 3秒
上記のようにしてガスバリア性を有する透明電極用のフィルム基板を作製した。
上記で得られたガスバリア性を有する透明電極用フィルム基板上のバリアのない面に、以下の方法で第1導電層を形成した。
細線格子(金属材料)については以下に示す、グラビア印刷または銀ナノワイヤにより作製した。
銀ナノ粒子ペースト1(M−Dot SLP:三ツ星ベルト製)をRK Print Coat Instruments Ltd製グラビア印刷試験機K303MULTICOATERを用いて線幅50μm、高さ1.5μm、間隔1.0mmの細線格子を印刷した後、110℃、5分の乾燥処理を行った。
ランダムな網目構造については以下に示すように銀ナノワイヤを用いて作製した。
《透明電極の作製》
〈透明電極TC−101の作製〉
ガスバリア性を有する透明電極用のフィルム基板上にグラビア印刷にて第1導電層を形成した透明電極上に、下記塗布液Aを、押し出し法を用いて、乾燥膜厚300nmになるように押し出しヘッドのスリット間隙を調整して塗布し、110℃、5分で加熱乾燥し、導電性ポリマーと水系溶剤に分散可能なバインダー樹脂からなる第2導電層を形成し、得られた電極を8×8cmに切り出した。得られた電極を、オーブンを用いて110℃、30分加熱することで透明電極TC−101を作製した。
(塗布液A)
導電性ポリマー:PEDOT−PSS CLEVIOS PH510(固形分濃度1.89%、H.C.Starck社製) 1.59g
バインダー:ポリゾールFP3000(固形分54.4%水溶液) 0.13g
ジメチルスルホキシド(DMSO、導電性ポリマー溶液質量の10分の1)
0.16g
(透明電極TC−102〜TC−106の作製)
透明電極TC−101の作製において、塗布液Aのバインダーであるポリゾールを表1記載のバインダーに変更し、さらに塗布液Aへの添加固形分が70mgになるように添加量を変更した以外は透明電極TC−101の作製と同様にして、透明電極TC−102〜TC−106を作製した。
透明電極TC−101の作製において、ポリゾールFP3000をプラスコートRZ570に変更し、さらに塗布液AのPEDOT−PSS CLEVIOS PH510(固形分1.89%、H.C.Starck社製)を、ポリアニリンM(固形分濃度6.0%、ティーエーケミカル)0.5gに変更したこと以外は透明電極TC−101の作製と同様にして、透明電極TC−107を作製した。
(ランダムな網目構造)
銀ナノワイヤ分散液は、Adv.Mater.,2002,14,833〜837に記載の方法を参考に、PVP K30(分子量5万;ISP社製)を利用して、平均短径75nm、平均長さ35μmの銀ナノワイヤを作製し、限外濾過膜を用いて銀ナノワイヤを濾別、洗浄処理した後、ヒドロキシプロピルメチルセルロース60SH−50(信越化学工業社製)を銀に対し25質量%加えた水溶液に再分散し、銀ナノワイヤ分散液を調製した。
(銅メッシュ基板)
基板上に、補助電極として、下記の方法により、銅メッシュを作製し、金属微粒子除去液BFによるパターニングを行い、銅メッシュ基板を作製した。
透明電極TC−101の作製において、塗布液AのバインダーであるポリゾールFP3000を表1記載のバインダーに変更したこと以外は、透明電極TC−101の作製と同様にして、比較例の透明電極TC−110〜TC−114を作製した。
透明電極TC−101の作製において、塗布液A中のバインダーを使用しないこと以外は透明電極TC−101の作製と同様にして、透明電極TC−115を作製した。
バインダー樹脂のガラス転移温度(Tg)は、下記のようにして測定した。得られた透明電極のフィルム形状、透明性、表面抵抗(導電性)、表面粗さ及び膜強度を下記のように評価した。また、透明電極の安定性を評価するため、80℃90%RHの環境下で5日間置く強制劣化試験後の透明電極試料のフィルム形状、透明性、表面抵抗、表面粗さ及び膜強度の評価を行った。
示差走査熱量測定器(Perkin Elmer社製DSC−7型)を用いて、昇温速度10℃/分で測定し、JIS K7121(1987)に従い求めた。
JIS K 7361−1:1997に準拠して、東京電色社製 HAZE METER NDH5000を用いて、全光線透過率を測定し、下記基準で評価した。有機電子デバイスに用いるため、75%以上であることが好ましい。
○:75%〜80%未満
△:70%〜75%未満
×:70%未満
(表面抵抗)
JIS K 7194:1994に準拠して、抵抗率計(ロレスタGP(MCP−T610型):(株)三菱化学アナリテック製)を用いて表面抵抗を測定した。表面抵抗は100Ω/□以下であることが好ましく、有機電子デバイスを大面積にするには、30Ω/□以下であることが好ましい。
AFM(セイコーインスツル社製SPI3800Nプローブステーション及びSPA400多機能型ユニット)を使用し、約1cm角の大きさに切り取った試料を用いて、前記の方法(JIS B601(1994)に規定される表面粗さに準ずる。)で測定した。
導電層の膜の強度を、テープ剥離法により評価した。
○:3回の圧着剥離で変化無し
△:1回の圧着剥離で剥離が見られるが8割以上のパターンが残っている
×:1回の圧着剥離で剥離が見られ、残っているパターンが8割未満
評価の結果を表1に示す。
《有機ELデバイスの作製》
実施例1で作製した透明電極基板を超純水で洗浄後、パターン辺長20mmの正方形タイル状透明パターン一個が中央に配置されるように30mm角に切り出し、アノード電極に用いて、以下の手順でそれぞれ有機ELデバイスを作製した。正孔輸送層以降は蒸着により形成した。透明電極TC−101〜TC−115を用い、それぞれ有機EL素子OEL−201〜OEL−215を作製した。
真空度1×10−4Paまで減圧した後、化合物1の入った前記蒸着用るつぼに通電して加熱し、蒸着速度0.1nm/秒で蒸着し、厚さ30nmの正孔輸送層を設けた。
次に、以下の手順で各発光層を設けた。
さらに、形成した有機発光層と同じ領域に、化合物6を膜厚5nmに蒸着して正孔阻止層を形成した。
引き続き、形成した正孔阻止層と同じ領域に、CsFを膜厚比で10%になるように化合物6と共蒸着し、厚さ45nmの電子輸送層を形成した。
形成した電子輸送層の上に、透明電極を陽極として陽極外部取り出し端子及び15mm×15mmの陰極形成用材料としてAlを5×10−4Paの真空下にてマスク蒸着し、厚さ100nmの陽極を形成した。
得られた有機EL素子について発光ムラ及び寿命を下記のように評価した。
発光均一性は、KEITHLEY製ソースメジャーユニット2400型を用いて、直流電圧を有機EL素子に印加し発光させた。1000cd/m2で発光させた有機EL素子OEL−201〜OEL−217について、50倍の顕微鏡で各々の発光輝度ムラを観察した。また、有機EL素子OEL−201〜OEL−217をオーブンにて60%RH、80℃2時間加熱したのち、再び前記23±3℃、55±3%RHの環境下で1時間以上調湿した後、同様に発光均一性を観察した。
○:ほとんど均一発光しており、問題ない
△:部分的に若干発光ムラが見られるが、許容できる
×:全面にわたって発光ムラが見られ、許容できない
(寿命)
得られた有機EL素子の、初期の輝度を5000cd/m2で連続発光させて、電圧を固定して、輝度が半減するまでの時間を求めた。アノード電極をITOとした有機EL素子を上記と同様の方法で作製し、これに対する比率を求め、以下の基準で評価した。100%以上が好ましく、150%以上であることがより好ましい。
○:100〜150%未満
△:80〜100%未満
×:80%未満
評価の結果を表2に示す。
2 第2導電層
3 基材
Claims (4)
- 基板上に、導電性ポリマー及び水系溶剤に分散可能なポリマーを含有する透明電極において、前記ポリマーが解離性基含有自己分散型ポリマーであり、かつガラス転移温度が、25℃以上80℃以下であることを特徴とする透明電極。
- 前記解離性基含有自己分散型ポリマーのガラス転移温度が、50℃以上70℃以下であることを特徴とする請求項1に記載の透明電極。
- 基板上にパターン状に形成された銀含有導電性層を有することを特徴とする請求項1または2に記載の透明電極。
- 請求項1〜3のいずれか1項に記載の透明電極を具備することを特徴とする有機エレクトロルミネッセンス素子。
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