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JP3239991B2 - エレクトロルミネセンス装置およびその製造方法 - Google Patents

エレクトロルミネセンス装置およびその製造方法

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Publication number
JP3239991B2
JP3239991B2 JP11615997A JP11615997A JP3239991B2 JP 3239991 B2 JP3239991 B2 JP 3239991B2 JP 11615997 A JP11615997 A JP 11615997A JP 11615997 A JP11615997 A JP 11615997A JP 3239991 B2 JP3239991 B2 JP 3239991B2
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Prior art keywords
layer
electroluminescent device
electroluminescent
polymer
contact layer
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JPH1092577A (ja
Inventor
リチャード ヘンリー フレンド
ジェルミー ヘンリー バローグス
ドナル ドナット コーナー ブラッドリー
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Cambridge Display Technology Ltd
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Cambridge Display Technology Ltd
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Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B33/00—Electroluminescent light sources
    • H05B33/12—Light sources with substantially two-dimensional radiating surfaces
    • H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/10—Organic polymers or oligomers
    • H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
    • H10K85/114—Poly-phenylenevinylene; Derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/191—Deposition of organic active material characterised by provisions for the orientation or alignment of the layer to be deposited
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/10—Organic polymers or oligomers
    • H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
    • H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Manufacturing & Machinery (AREA)
  • Electroluminescent Light Sources (AREA)
  • Luminescent Compositions (AREA)
  • Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
  • Illuminated Signs And Luminous Advertising (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Led Devices (AREA)
  • Control Of Indicators Other Than Cathode Ray Tubes (AREA)
  • Control Of El Displays (AREA)
  • Heating, Cooling, Or Curing Plastics Or The Like In General (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)

Description

【発明の詳細な説明】
【０００１】
【発明の属する技術分野】本発明は、エレクトロルミネ
センス装置に関し、一層詳細には、発光層が半導体であ
るエレクトロルミネセンス素子（ＥＬ）を含み、それぞ
れ前記半導体のバンドギャップが異なるエレクトロルミ
ネセンス素子を組み合わせてディスプレイ等の如き表示
装置を構成するエレクトロルミネセンス装置およびその
製造方法に関する。
【０００２】
【従来の技術】エレクトロルミネセンス素子（ＥＬ）
は、電界の影響により発光するよう構成されている。こ
のような半導体における物理的過程に対する一般的な作
用は、半導体の相対する電極から半導体に注入される電
子−正孔対の放射結合を通して行われる。その一例を挙
げると、ＧａＰおよびあるいは、同様なIII 族の元素と
Ｖ族の元素の組み合わせからなる半導体を基礎として構
成されている。
【０００３】これらの素子は、効果的且つ広範囲に利用
されているものの、その大きさが非常に微小であるため
に大面積ディスプレイに使用するに際しては、困難を伴
うばかりか不経済でもある。
【０００４】大面積ディスプレイへの使用が可能な代替
品の材料は幾種類か知られているが、無機半導体の一つ
であるＺｎＳ（硫化亜鉛）が好適である。しかしなが
ら、この系には信頼性に薄いという、問題が存在する。
【０００５】有機材料の一つとしては、アントラセン
（ａｎｔｈｒａｃｅｎｃ）、ペリレン（ｐｅｒｙｌｅｎ
ｅ）、そしてコロネン（ｃｏｒｏｎｅｎｅ）のようなシ
ンプルな芳香族分子単体（ｓｉｍｐｌｅ ａｒｏｍａｔ
ｉｃ ｍｏｌｅｃｕｌｅｓ）がエレクトロルミネセンス
素子（ＥＬ）の材料として用いられていることが知られ
ている。
【０００６】これらの材料の実用上の問題点としては、
ＺｎＳと同様に、それらが信頼性を欠くばかりか、これ
らの有機層と電流注入電極層（ｃｕｒｒｅｎｔ−ｉｎｊ
ｅｃｔｉｎｇ ｅｌｅｃｔｒｏｄｅ ｌａｙｅｒｓ）と
の接合性に問題がある。
【０００７】アントラセン（ａｎｔｈｒａｃｅｎｅ）を
利用したエレクトロルミネセンス素子は、米国特許３，
６２１，３２１号に開示されている。この素子は、多量
の電力を消費し、且つその電力消費量に比して発光が少
ないという不都合を有している。
【０００８】前記開示の素子の改善を試みるべく、米国
特許４，６７２，２６５号には、発光層を二層からなる
構造としたエレクトロルミネセンス素子（ＥＬ）が記載
されている。
【０００９】しかしながら、前記二層構造に用いられる
物質は、前述の不都合な有機材料である。
【００１０】
【発明が解決しようとする課題】本発明は、前記の不都
合を未然に回避するか、若しくは少なくとも前記不都合
を低減化することを可能とするエレクトロルミネセンス
装置およびその製造方法を提供することを目的とする。
【００１１】
【課題を解決するための手段】本発明の一能様によれ
ば、エレクトロルミネセンス装置を構成する素子が少な
くとも共役ポリマーが用いられる高密度で薄いポリマー
膜から構成される半導体層と、前記半導体層の第１の表
面と接する第１接触層と、前記半導体層の第２の表面と
接する第２接触層とを有する。
【００１２】本発明は、好適な接触層から電荷移動体
（ｃｈａｒｇｅ ｃａｒｒｉｅｒｓ）が半導体層に注入
されることより発光することを応用した共役ポリマー半
導体に発見の基礎をおいている。
【００１３】高分子重合体は知られている。例えば、そ
れらは、光学変調器（ｏｐｔｉｃａｌ ｍｏｄｕｌａｔ
ｏｒ）に用いられ、欧州特許出願０２９４０６１号で検
討されている。この場合には、第１の電極と第２の電極
の間に位置する変調のためのアクティブ層としてポリア
セチレンが用いられている。光学変調効果を発生させる
アクティブ層に空間電荷領域を形成するように、一つの
電極とアクティブ層との間に絶縁層を設ける必要があ
る。空間電荷層の存在が発光に寄与する電子−正孔対
（ｅｌｅｃｔｏｒ−ｈｏｌｅ ｐａｉｒｓ）の形成を妨
げるため、エレクトロルミネセンス素子には不向きであ
る。いずれにせよ、欧州特許出願０２９４０６１号に開
示されているエレクトロルミネセンス素子では、光学変
調効果の破壊に関しては、全く望ましくない。
【００１４】本発明に係る装置を構成する素子は、共役
ポリマー（ＣｏｎｉｕｇａｔｅｄＰｏｌｙｍｅｒ）がポ
リポリ（ｐ−フエニレンビニレン）〔ＰＰＶ〕であるの
が好ましく、第１の電荷注入接触層（ｆｉｒｓｔ ｃｈ
ａｒｇｅ ｉｎｊｅｃｔｉｏｎ ｃｏｎｔａｃｔ ｌａ
ｙｅｒ）は、一側の表面に薄い酸化物層が形成されたア
ルミニウムの薄層からなり、半導体層の第１の表面は前
記酸化物層と接し、そして第２の電荷注入接触層（ｓｅ
ｃｏｎｄ ｃｈａｒｇｅ ｉｎｊｅｃｔｉｏｎ ｃｏｎ
ｔａｃｔ ｌａｙｅｒ）はアルミニウムまたは金の薄層
である。
【００１５】その他の実施態様では、共役ポリマーはＰ
ＰＶであり、第１接触層がアルミニウム、若しくはマグ
ネシウムと銀の合金で、第２接触層（ｓｅｃｏｎｄ ｃ
ｏｎｔａｃｔ ｌａｙｅｒ）は、酸化インジウムであ
る。
【００１６】さらに別の実施態様では、共役ポリマーは
ＰＰＶであり、接触層の一つは非晶質シリコンからな
り、他方の接触層は、アルミニウム、金、マグネシウム
−銀合金、酸化インジウムなる群のうちから選択され
る。
【００１７】これらの実施態様は、第１接触層あるいは
第２接触層のうちのいずれかを基板に積層し、ＰＰＶの
薄層を付与し、そして、その上に前記積層されなかった
接触層を積層する。
【００１８】好適には、ポリマー膜は、概ね１０ｎｍか
ら５μｍの範囲の均一な厚さを有し、共役ポリマーは１
ｅＶから３．５ｅＶの範囲で半導体バンドギャップを有
する。その上、電界発光するポリマー膜の共役ポリマー
の大きさは、膜内の共役ポリマーにおける電荷の浸透移
動が十分なされるものである。
【００１９】共役ポリマーとは、ポリマーの主骨格に沿
って非極在π電子を有するポリマーを意味する。
【００２０】そのようなポリマーは、例えば、Ｒ．Ｈ．
フレンドにより、Ｊｏｕｒｎａｌｏｆ Ｍｏｌｅｃｕｌ
ａｒ Ｅｌｅｃｔｒｏｎｉｅｓ４（１９８８）Ｊａｎｕ
ａｒｙ−Ｍａｒｃｈ，Ｎｏ．１，の３７頁から４６頁で
検討されている。
【００２１】本発明の基礎となるメカニズムは、以下の
とおりである。すなわち、正の接触層は、ポリマー膜に
正の電荷キャリヤを注入し、負の接触層は、ポリマー膜
に負の電荷キャリヤを注入する。この場合、正の接触層
は高い仕事関数を有することが、また負の接触層は低い
仕事関数を有するように構成される。従って、負の接触
層は、例えば、金属あるいはドープ半導体（ａ ｄｏｐ
ｅｄ ｓｅｍｉｃｏｎｄｕｃｔｏｒ）のような電子注入
材料（ｅｌｅｃｔｒｉｃ─ｉｎｊｅｃｔｉｎｇｍａｔｅ
ｒｉａｌ）から構成され、ポリマー半導体層と接して、
外部電位を印加されて負電位を生じる時、電子のポリマ
ー半導体層への注入がなされる。正の接触層は、例え
ば、金属やドープ半導体のような正孔注入材料（ｈｏｌ
ｅ−ｉｎｇｅｃｔｉｎｇ ｍａｔｅｒｉａｌ）から構成
され、ポリマー半導体層とし、外部電位を印加されてポ
リマー半導体層に一般に正孔と呼ばれる正の電荷が注入
される。
【００２２】所謂、“緻密な”ポリマー膜とは、実質的
に空間が排除されたポリマー膜を意味する。
【００２３】少なくとも一つの接触層は、電子注入材
（ｅｌｅｃｔｒｉｃ─ｉｎｊｅｃｔｉｎｇ ｍａｔｅｒ
ｉａｌ）に加えて、有機材料を含むことが可能である。
【００２４】共役ポリマーの膜は、好適には、単一の共
役ポリマーから構成される。またあるいは、共役ポリマ
ーからなる膜は、共役ポリマーの混合物から構成される
ことも可能である。
【００２５】ポリマー膜のさらに好適な特徴は以下の通
りである。 （ｉ）ポリマーは酸素、湿度に対して化学的に安定であ
ること。 （ii）ポリマー膜は、下地層との間の良好な接着性、温
度上昇あるいは圧力圧迫を原因とする亀裂の発生に対す
る阻止能力、縮み、膨張、再結晶あるいは他の形態変化
への抵抗性を有するべきである。
【００２６】次に、本発明に係るエレクトロルミネセン
ス装置およびその製造方法についてその実施態様を挙げ
て図面を参照しながら説明する。
【００２７】共役ポリマー膜は、好適には、下記式のポ
リ（ｐ−フエニレンビニレン）［ＰＰＶ］であり、下記
式において、フェニレン環は、各々独立してアルキル基
（好適にはメチル基）、アルコキシ基（好適にはメトキ
シ基若しくはエトキシ基）、ハロゲン（好適には塩素若
しくは臭素）のなかから選択される一あるいはそれ以上
数の置換基であってよい。
【００２８】ポリ（ｐ−フエニレンビニレン）［ＰＰ
Ｖ］から誘導されるその他の共役ポリマーもまた、本発
明に係るエレクトロルミネセンス素子のポリマー膜とし
て適当に使用される。
【００２９】
【化２】
【００３０】以下に前記その他の共役ポリマーの典型的
例を示す。 （ｉ）式１のフェニレン環を縮合環系に置き換える例え
ば、フェニレン環に代えてアントラセンあるいはナフタ
レン環系に置換することによって得られる、以下のよう
な構造を示すポリマー。
【００３１】
【化３】
【００３２】
【化４】
【００３３】
【化５】
【００３４】これらの多環系もまた前記フェニレン環と
同様に１あるいはそれ以上の数の置換基を有してもよ
い。 （ii）フェニレン環をフラン環のような複素環系に置換
することによって得られる、以下の構造を示すポリマ
ー。
【００３５】
【化６】
【００３６】前記と同様に、前記フラン環も一あるいは
それ以上の数の置換基を有してもよい。 （iii) 各々のフェニレン環（若しくは前記（ｉ）ある
いは（ii）においてに与えられた他の環系）に結合した
ビニレン部分の数を増やすことによって得られる、以下
のような構造示すポリマー。
【００３７】
【化７】
【００３８】
【化８】
【００３９】
【化９】
【００４０】前記構造式において、ｙは２、３、４、
５、６、７を示す。
【００４１】さらにまた、これらの環系は前記種々の置
換基を有してもよい。
【００４２】これらのさまざまなＰＰＶ誘導体は、全て
のスペクトルを確実に網羅するために異なった波長を放
射するエレクトロルミネセンスの構造が得られるので、
異なった様々な半導体のエネルギーギャップを有し、こ
れらを組み合わせてエレクトロルミネセンス装置を構成
する。
【００４３】共役ポリマー膜は、前駆体ポリマーを化学
的方法あるいは熱処理によって得ることができる。前記
方法のうち後者の場合においては、共役ポリマーに変質
させる前に、必要に応じて前処理することができる。
【００４４】前記の各種のＰＰＶ誘導体膜は、適当なス
ルホニウム前駆体を使用することにより同様に導電性基
板に付与することができる。
【００４５】一般に、好適には、スルホニウム塩前駆体
（II）よりも有機溶媒への溶解度が高いポリマー前駆体
を用いるが有利な場合がある。
【００４６】ポリ（フエニレンビニレン）の膜は、図１
に示されるような反応図式に基いた方法により、導電性
基板上に付与される。スルホニウム塩単量体（II）は、
水溶液、水エタノール混液、若しくはメタノール中で前
駆体ポリマー（III)に合成される。そのような前駆体ポ
リマー（III)は、ホトレジスト処理のために半導体産業
で用いられている一般的なスピンーコーティング技術に
より導電性基板上に付与することができる。その結果生
じた前駆体ポリマー（III)は、通例２００℃から３５０
℃での加熱処理によりポリフエニレンビニレン（Ｉ）に
転化される。
【００４７】単量体（II）の化学合成、その前駆体（II
I)への重合、そしてＰＰＶのための熱転化のために必要
な詳細な条件は、文献、例えば、Ｄ．Ｄ．Ｃ．Ｂｒａｄ
ｌｅｙによるＪ．Ｐｈｙｓ．Ｄ（Ａｐｐｌｉｅｄ Ｐｈ
ｙｓｉｃｓ）、２０、１３８９（１９８７）およびＪ．
Ｄ．Ｓｔｅｎｇｅｒ Ｓｍｉｔｈ、Ｒ．Ｗ．Ｌｅｎｚと
Ｇ．ＷｅｇｎｅｒによるＰｏｌｙｍｅｒ、３０、１０４
８（１９８９）に記載されている。
【００４８】ポリ（フェニレンビニレン）膜は、１０ｎ
ｍから１０μｍの厚さが得られることが知られている。
これらのＰＰＶ膜は、ごくわずなピンホールしかみられ
ない。ＰＰＶ膜は、約２．５ｅＶ（５００ｎｍ）の半導
体エネルギーギャップを有する。
【００４９】それ以外の適当な共役ポリマーの膜を形成
する材料は、ポリ（フェニレン）である。
【００５０】この材料は、５、６−ジヒドロキシシクロ
ヘキサ−１、３−ジエンの生化学的に製造される誘導体
を出発物質として製造される。このポリ（フェニレン）
の製造は、Ｂａｌｌａｒｄ ｅｔ ａｌ、Ｊ．Ｃｈｅ
ｍ．Ｃｏｍｍ．９５４（１９８３）により詳細に記載さ
れている。
【００５１】ポリマー前駆体溶液は、導電性基板上に薄
い膜としてスピンコートされ、そして、その後、通例１
４０℃から２４０℃の範囲で熱処理されて共役ポリ（フ
ェニレン）ポリマーに転換される。
【００５２】ビニル若しくはジエン単量体の共重合もま
たフェニレンコポリマーを得ることができる。
【００５３】それ以外の種類の共役ポリマーの膜に必要
とされ使用できる材料として、例えば、以下のようなも
のが含まれる。 （ａ）ポリ（４、４’−ジフェニレンジフェニルビニレ
ン）［ＰＤＰＶ］は、両方のビニレンの炭素がフェニル
環により置換されている。それは、薄い膜を形成できる
ように普通の有機溶媒に解ける。 （ｂ）ポリ（１、４−フェニレン−１−ジフェニルビニ
レンとポリ（１、４−フェニレンジフェニルビニレン）
ポリマーはＰＰＶと類似物質であり、それぞれ一つある
いは両方のビニレンの炭素がフェニル基と置換されてい
る。それらは各々有機溶媒に解け薄い膜として被覆され
る。 （ｃ）有機溶媒中に溶解可能であり、長い主鎖を有する
アルキル（アルキルはオクチルと等しいかそれ以上に長
い）についてはポリ（３−アルキルチオフェン）ポリマ
ー（アルキルは、プロピル、ブチル、ペンチル、ヘキシ
ル、ヘプチル、オクチル、デシル、ウンデシル、ドデシ
ルのいずれか一つ）は溶融加工可能である。 （ｄ）ポリ（３−アルキルピロール）ポリマーは（３−
アルキルチオフェン）ポリマーと類似であることが予想
される。 （ｅ）ブチルよりも大きなアルキルを有するポリ（２、
５−ジアルコキシ−ｐ−フェニレンビニレン）ポリマー
は溶解加工可能である。 （ｆ）ポリ（フェニルアセチレン）は主鎖中の水素原子
がフェニル基に置換されたポリアセチレンの誘導体であ
る。この置換によって、材料は加工可能である。
【００５４】必要とされ使用可能なポリマーとそれによ
って導電性基板（電荷注入接触層）に必要とされるポリ
マーからなる薄い均一な膜が容易に得られるように、他
のポリマーとの共役ポリマーが混合されたポリマーブレ
ンドが使用されることもある。
【００５５】共役ポリマーの膜を形成するのに、そのよ
うなコポリマーまたはポリマーブレンドを用いる時、前
記共役ポリマーの膜を併せ有するエレクトロルミネセン
ス素子の活性部位は、コポリマーあるいはポリマーブレ
ンドのパーコレイション開始物質と同じかそれ以上に大
きい多量の共役ポリマー部位を含まなければならない。
【００５６】半導体電界発光層は、異なったバンドギャ
ップあるいは多種類の電荷のバンドギャップのポリマー
層から形成されている。
【００５７】
【実施例】［実施例１］ 図２および図３を参照しながらエレクトロルミネセンス
素子（ＥＬ）の構造を以下に説明する。
【００５８】ガラス基板、例えば、約１ｍｍのシリコン
あるいは、ホウケイ酸塩ガラス１の上面に、第１の電荷
注入接触層２を形成した。電荷注入接触層２は、約２０
ｎｍの厚さの層を作るためのシャドウマスクによりアル
ミニウムを熱蒸着させて形成した。前記シャドウマスク
によりパターンが形成され、前記パターンは、縦の長さ
が１５ｍｍで２ｍｍの間隙を有して平行に並ぶ幅２ｍｍ
の一連の細長い小片状である。。アルミニウム電荷注入
接触層を、薄い表面酸化物層３を形成するために空気に
さらした。このようにして電荷注入接触層を形成した。
【００５９】２５ｇのメタノールに１ｇのポリマーが溶
解されたＰＰＶの前駆体のメタノール溶液を、前記の結
合基板にスピンコーティングした。これは、結合基板の
表面の全体にポリマーの塗布がなされ、軸の回転速度が
５０００ｒ．ｐ．ｍ．で回転して行なわれた。その結
果、得られた基板とポリマー前駆体層は、真空オーブン
中で３００℃の温度で加熱された。この加熱処理によっ
てポリマー前駆体はＰＰＶに変換された。得られたＰＰ
Ｖ膜４は１００から３００ｎｍの厚さであった。必要最
低限の膜の厚さは２０ｎｍ程度である。しかしながら、
２０ｎｍから１μｍの範囲の厚さであってもよい。
【００６０】次に、第２の電荷注入接触層５を、ＰＰＶ
膜の上に金あるいはアルミニウムを蒸着させて形成し
た。シャドウマスクを用いて、ＰＰＶ膜の表面上におい
てパターンを形成し、縦の長さが１５ｍｍで２ｍｍの間
隙を有して平行に並ぶ幅２ｍｍの一連の細長い小片を得
た。第２の電荷注入接触層の厚さは、２０から３０ｎｍ
の範囲であった。このようにして正孔注入接触層を形成
した。
【００６１】電荷注入接触層のうち少なくとも一つは、
エレクトロルミネセンス素子（ＥＬ）の水平面に垂直に
発光をなすために透明、若しくは半透明であることが望
ましい。この実施例では金、若しくはアルミニウムの層
が３０ｍｍ以下の厚さである時になされる。ＰＰＶ層の
厚さが約２００ｎｍの素子であって強力なエレクトロル
ミネセンス素子（ＥＬ）のためのしきい値電圧は、約４
０ボルトである。この電圧は、２×１０6 Ｖｃｍ -1 の
しきい電界を付与することになる。半透明の電極を通し
てなされる電流密度２ｍＡ／ｃｍ2 の発光がある。この
実施例のエレクトロルミネセンス素子（ＥＬ）のレスポ
ンスタイムは、非常に短く、そして１０マイクロセカン
ドより速い。エレクトロルミネセンス素子（ＥＬ）は、
空気中では、特別な用心をすることなく使用され、機能
低下の兆候はなにも示さない。
【００６２】素子から出力された光を、格子モノクロメ
ータにより分光し、シリコン光起電力セルで検出し、室
温２０℃で計測し光学通路を有する低温保持装置に素子
を保持した。その結果を図４に示す。エレクトロルミネ
センス素子（ＥＬ）のスペクトルは、ピークが温度によ
ってその位置をわずかにシフトして０．１５ｅＶだけ異
なって６９０ｎｍから５００ｎｍ（１．８ｅＶから２．
４ｅＶ）のスペクトル範囲で発光する。
【００６３】エレクトロルミネセンス素子（ＥＬ）層と
比べて低い仕事関数を有し電子注入層として用いるのに
適した他の材料は、（非結晶あるいは結晶性）のｎ−ド
ープシリコン、酸化膜を有するシリコン、純粋、若しく
は金などの他の金属との合金であるアルカリ、およびア
ルカリ土類金属類である。“ｎタイプドープ”共役ポリ
マーの薄層を、金属層と電界発光ポリマー層との間に入
れることができる。
【００６４】エレクトロルミネセンス素子（ＥＬ）層と
比べて高い仕事関数を有し正孔注入層として用いるのに
適した他の材料は、インジウム／スズ酸化物、白金、ニ
ッケル、パラジウム、および黒鉛である。また、電気化
学的に重合されたポリピロール、ポリチオフェン等の
“ｐタイプドープ”共役ポリマーの薄膜を金属層とエレ
クトロルミネセンスポリマー層の間に入れることができ
る。
【００６５】前記材料は、以下のように付与することが
できる。すなわち、白金のような融点温度が特に高い金
属を除いた殆どの金属は、蒸着により付着させることが
できる。インジウム／錫の酸化物を含む全ての合金は、
ＤＣまたはＲＦスパッタリング法を用いて、付着させる
ことができる。 「実施例２」 この例は、一連の層から構成される。先ず、透明な酸化
インジウムからなる所定の層が、抵抗率が５×１０-4Ω
ｃｍとなるように形成する。インジウムターゲットから
一般的に０．１１ｎｍ／ｓｅｃで、一般に２×１０-4ｍ
ｂａｒの酸素圧力を付与しながらイオンビームのスパッ
タリングを含む工程により基板上に設ける。
【００６６】一般に単位面積あたり約５０Ωの抵抗比シ
ートは、１００ｎｍの厚さによりもたらされる。そのよ
うな膜は、可視スペクトル部で光学透過係数は、９０％
以上である。
【００６７】ＰＰＶ膜は、実施例１に記載の方法によ
り、酸化インジウム層上に配設される。アルミニウム接
触層は、５０ｎｍの厚さを有するように蒸着により最後
に形成される。この構造で、酸化インジウム接触層が正
の接触層として働き、アルミニウム接触層は、負の接触
層として働く。発光は、酸化インジウム層を通過する。 「実施例３」この構造体の制作は、実施例２の上部金属
接触層までは近似して行われる。ここで、負接触層とし
て機能する上部接触層は、ＡｇおよびＭｇの合金を蒸着
させることで形成した。蒸着は、ＡｇおよびＭｇの粉末
を、容器内で１：１０のモル比で混合したものを加熱し
て行われ、主として５０ｎｍの厚さの層が形成された。
【００６８】Ｍｇは、仕事関数が小さいので、負極の物
質として用いるのが望ましい。Ａｇを加えて合金とする
のは、ポリマー層に対する金属膜の固着を良くし、酸化
を抑制するためである。この例における電流／電圧特性
およびエレクトロルミネセンス特性は、前記実施例２に
記載のものと略同じである。 「実施例４」これらの構造体は、負極として機能する非
晶質シリコーン水素合金層と、正極として機能する酸化
インジウムの層とで制作される。ガラス基板は、Ａｌま
たはＣｒを蒸着させて得られる金属接触層を有する。非
晶質シリコーン水素合金層は、以下に詳細に示す高周波
加熱（ＲＦ）スパッタリングによって形成された。
【００６９】ＲＦスパッタリング装置は、２つのターゲ
ットと液体窒素冷却ゲッタを有し、８ｃｍのターゲット
基板で作用する。チャンバは、５×１０-8ｍｂａｒのベ
ース圧力に設定される。マグネトロンのターゲットは、
厚さ３ｍｍのｎ−ドープＳｉウエハ層を担持させる。タ
ーゲットは、試料に関して１乃至２時間プレスパッタリ
ングを行うことで浄化される。このようにして用意され
た基板は、厚さ３ｃｍのＣｕおよびＡｌの基板温度が２
５０乃至３００°Ｃとなるように加熱される。基板は、
約６ｒｐｍで回転される。スパッタリングのガスとして
は、０．００７乃至０．０１３ｍｂａｒの圧力でＨ2 ３
０％を含むＡｒが用いられ、蒸着の間、連続的にチャン
バに供給される。ＲＦのパワーとしては、２Ｗの反射出
力を有する２５０Ｗが使用される。付着は、厚さ１μｍ
の膜厚に対して１．５時間付着を行う場合に、主として
１２ｎｍ／分である。
【００７０】生成された非晶質Ｓｉは、赤茶色を呈し、
直流抵抗率が５×１０6 乃至５×１０8 Ωｃｍである。
【００７１】ＰＰＶの層は、実施例１に示したように、
非晶質シリコン−水素層に加えられた。そして、実施例
２に示した手順でＰＰＶ層に直接した酸化インジウム層
を形成した。
【００７２】上記の手順を用いて制作された面積１４ｍ
ｍ2 、シリコン−水素層の厚さ１μｍ、ＰＰＶの層の厚
さ４０ｎｍ、酸化インジウム層の厚さ２５０ｎｍの構造
体に関して得られた結果を図７および図８に示す。図７
は、順バイアス（酸化インジウム層を正極とする）をか
けた場合の素子の電流／電圧特性を示す。また、図８
は、電流に対する発光量の変化を示す。電荷の注入およ
び発光は、約１７Ｖより開始される。そして、この閾値
を越えた電流値の上昇は、例えば、図５に示すように、
シリコン−水素層がない場合に比較してなだらかであ
る。
【００７３】この形状の構造体は、逆バイアス（シリコ
ン−水素接触層に対して酸化インジウム層を負極とす
る）をかけた場合に、弱い電界発光を示す。従って、順
バイアスをかけることが望ましい。 「実施例５」実施例４に示す構造体の最上層である酸化
インジウム層は、半透明のＡｕまたはＡｌと置き換え
た。構造体の最上層は、厚さ約２０ｎｍからなる発光を
示す層として形成された。これらの素子は、上述した各
実施例と同様の特性を示した。
【００７４】実施例４の製造方法は、実施例２および実
施例３に示した接触層にも適用することができる。
【００７５】シリコン／水素層および酸化インジウム層
を形成する方法はそれ自体公知である。シリコンの場
合、これは、シランのグロー放電と蒸着を含む。付着方
法は、蒸着、ＲＦおよび直流スパッタリングでもよい。
【００７６】電荷注入接触層の厚さの選択は、用いられ
る付着技術と、接触層における所望の光学的透明度によ
って決定される。電荷注入の容易性は、電荷注入接触層
を複合層として構成することで改善される。この複合層
は、正孔および電子を夫々注入するため、酸化および還
元共役ポリマーの薄膜層を含む。これらの特別な共役ポ
リマー層は、活性状態の電界発光ポリマーと同様であっ
てよい。このような物質をドープする方法は、この分野
においては良く知られており、「導電性ポリマーハンド
ブック」（ティ．ジェイ．スコッテイム（Ｔ．Ｊ．Ｓｋ
ｏｔｈｅｉｍ））に良く書かれている。
【００７７】少なくとも１つの電荷注入接触層は、素子
の平面に垂直に発光させるため透明または半透明とする
べきであるが、それは素子の平面内で放射が要求されな
い場合には必ずしも必要なものではない。
【００７８】製造されるエレクトロルミネセンス素子の
サイズの限界は、スピンコーティンに使用することがで
きる基板のサイズによって決定される。例えば、このよ
うにして、直径１５ｃｍのシリコンウエファのコーティ
ングが行われる。さらに、広い面積のコーティングを行
うためには、ドローコーティングの技術が用いられる。
従って、平方メートルの面積を有する共役ポリマーを用
いたエレクトロルミネセンス素子の製造もできる。
【００７９】ＰＰＶを含む共役ポリマーの少なくとも、
いくつかは非常に高い温度で蒸着される金属層の付着、
または、活性電界光領域を限定するためのフォトリソグ
ラフィの工程で得られ、非晶質シリコン層の蒸着のよう
な前工程に対して、耐性を有する。ＰＰＶの場合、基板
に前駆体ポリマーを用いる方法では、スピンコーティン
グまたはドローコーティングのいずれかによるのが適当
であるが、共役ポリマーとエレクトロルミネセンス素子
のタイプによって、スピンコーティング、ドローコーテ
ィングおよび溶融工程の全てを基板上に共役ポリマーを
付着するのに使用することができる。
【００８０】エレクトロルミネセンス素子は、電界発光
効果を用いる種々の用途に適用される。従来より、半導
体ＬＥＤが使用されていたところに用いられる。また、
液晶が使用されていたところにも用いられる。エレクト
ロルミネセンス素子は数多くの特性を有している。
【００８１】前記の如き素子を組み込むエレクトロルミ
ネセンス装置は、視角が拡張される。さらに、広面積の
エレクトロルミネセンス装置は、大面積液晶ディスプレ
イが遭遇する基板の平面性についての問題点を克服する
ことができる。エレクトロルミネセンス装置は、テレビ
ジョンやコンピュータディスプレイのように、マトリッ
クス方式のディスプレイに対して特に好適である。マト
リックス方式のディスプレイに適用されるエレクトロル
ミネセンス装置の一例を図３に示す。ここでは、電荷注
入接触層が、半導体層のいずれか一方の側部において、
一方の接触層が他方の接触層に対して直交するようにし
て筋状に形成される。ディスプレイの画素としての個々
エレクトロルミネセンス素子すなわち半導体層の領域の
マトリックスのアドレス指定は、下方の電荷注入接触層
と上方の電荷注入層とを特定することで達成される。さ
らに、エレクトロルミネセンス素子は、応答速度が速い
ため、テレビジョンの受像機に適する。特に、発光の色
を共役ポリマーの選択および半導体のバンドギャップの
選択によって制御することができる。従って、緑、赤、
青を混色してなるカラーディスプレイは、エレクトロル
ミネセンス素子の共役ポリマーの配置によって制御が可
能となる。
【図面の簡単な説明】
【図１】共役ポリマーを配設するための反応図式を示す
図である。
【図２】本発明に係るエレクトロルミネセンス素子の概
略図である。
【図３】本発明に係るエレクトロルミネセンス素子の概
略図である。
【図４】図２並びに図３に記載されたエレクトロルミネ
センス素子の出力を示すグラフである。
【図５】本発明の他の実施例に係る電界発光素子のそれ
ぞれ電流対発光および出力強度対印加電圧を示すグラフ
である。
【図６】本発明の他の実施例に係る電界発光素子のそれ
ぞれ電流対発光および出力強度対印加電圧を示すグラフ
である。
【図７】本発明のさらに他の実施例に係るそれぞれの電
流出力および電界発光強度を示すグラフである。
【図８】本発明のさらに他の実施例に係るそれぞれの電
流出力および電界発光強度を示すグラフである。
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ Ｈ０５Ｂ 33/22 Ｈ０５Ｂ 33/22 Ｃ 33/26 33/26 Ｚ (72)発明者 バローグス ジェルミー ヘンリー アメリカ合衆国、ニューヨーク00516 コールドスプリング パーソネイジ ス トリート 11 (72)発明者 ブラッドリー ドナル ドナット コー ナー イギリス国、ケンブリッジ シービー３ ０ディー５チャーチル カレッジ（番 地なし) (56)参考文献 特開 昭61−37887（ＪＰ，Ａ) 特開 昭59−194393（ＪＰ，Ａ) 特開 平２−160894（ＪＰ，Ａ) 特開 昭62−44986（ＪＰ，Ａ) 特開 昭63−7804（ＪＰ，Ａ) 特開 平３−244630（ＪＰ，Ａ) 特開 昭59−199746（ＪＰ，Ａ) 特開 昭60−11528（ＪＰ，Ａ) 米国特許3621321（ＵＳ，Ａ) 欧州公開294061（ＥＰ，Ａ１) (58)調査した分野(Int.Cl.7，ＤＢ名) H05B 33/14

Claims (25)

    (57)【特許請求の範囲】
  1. 【請求項１】複数の共役ポリマーからなる緻密なポリマ
    ー膜の形状を呈し発光色を制御する異なる半導体バンド
    ギャップを有する半導体層と、素子に電界をかけること
    によって第１のタイプの電荷キャリヤが前記半導体層に
    放出されるように選択された第１の接触層と、前記素子
    に電界をかけることによって第２のタイプの電荷キャリ
    ヤが前記半導体層に放出されるように選択された第２の
    接触層とからなり、前記共役ポリマーは発光色を制御す
    る半導体バンドギャップを有し、前記半導体層のポリマ
    ー膜は、該半導体層を横断して前記第１と第２の接触層
    の間に電界をかけたときに前記第１の接触層に対して第
    ２の接触層を正にすべく前記第１と第２の電荷キャリヤ
    が前記半導体層の中に注入されて共役ポリマー電荷キャ
    リヤ対を形成するように結合されて放射して崩壊するこ
    とにより、前記共役ポリマーから発光が行われるほどに
    十分に低い濃度の外部電荷キャリヤを有することを特徴
    とするエレクトロルミネセンス装置。
  2. 【請求項２】請求項１記載のエレクトロルミネセンス装
    置において、共役ポリマーが式 【化１】 ［式中、フェニレン環は、必要に応じてアルキル（好適
    にはメチル）、アルコキシ（好適にはメトキシまたはエ
    トキシ）、ハロゲン（好適には塩素または臭素）または
    ニトロの中からそれぞれ独立して選択される一つあるい
    はそれ以上の置換基を有していてもよい］のポリ（ｐ−
    フェニレンビニレン） [ＰＰＶ] であるエレクトロルミ
    ネセンス素子を有することを特徴とするエレクトロルミ
    ネセンス装置。
  3. 【請求項３】請求項１または２記載のエレクトロルミネ
    センス装置において、前記ポリマー膜は１０ｎｍから５
    μｍの実質的に均一な厚さからなるエレクトロルミネセ
    ンス素子を有することを特徴とするエレクトロルミネセ
    ンス装置。
  4. 【請求項４】請求項１乃至３のいずれかに記載のエレク
    トロルミネセンス装置において、共役ポリマーが１ｅＶ
    から３．５ｅＶの範囲内で半導体のバンドギャップを有
    するエレクトロルミネセンス素子を有することを特徴と
    するエレクトロルミネセンス装置。
  5. 【請求項５】請求項１乃至４のいずれかに記載のエレク
    トロルミネセンス装置において、ポリマー膜のエレクト
    ロルミネセンス領域において共役ポリマーの割合はフイ
    ルムに存在する共役ポリマーにあってキャリヤを移動さ
    せるために十分な浸透しきい値を有するものであるエレ
    クトロルミネセンス素子を有することを特徴とするエレ
    クトロルミネセンス装置。
  6. 【請求項６】請求項１乃至５のいずれかに記載のエレク
    トロルミネセンス装置において、第１の電荷キャリヤの
    注入接触層は薄い酸化層を形成したアルミニウムからな
    る一つの薄い表面層を有し、半導体層の第１の表面が前
    記酸化層と接触しているエレクトロルミネセンス素子を
    有することを特徴とするエレクトロルミネセンス装置。
  7. 【請求項７】請求項１乃至６のいずれかに記載のエレク
    トロルミネセンス装置において、第１の接触層はアルミ
    ニウム、若しくはマグネシウムと銀の合金からなるグル
    ープから選択されるエレクトロルミネセンス素子を有す
    ることを特徴とするエレクトロルミネセンス装置。
  8. 【請求項８】請求項６記載のエレクトロルミネセンス装
    置において、第２の電荷キャリヤ注入接触層はアルミニ
    ウムと金からなるグループから選択されるエレクトロル
    ミネセンス素子を有することを特徴とするエレクトロル
    ミネセンス装置。
  9. 【請求項９】請求項１乃至８のいずれかに記載のエレク
    トロルミネセンス装置において、第１と第２の電荷キャ
    リヤ注入接触層は少なくとも一つが半透明体であるエレ
    クトロルミネセンス素子を有することを特徴とするエレ
    クトロルミネセンス装置。
  10. 【請求項１０】請求項７記載のエレクトロルミネセンス
    装置において、第２の接触層は酸化インジウム若しくは
    酸化インジウムスズであるエレクトロルミネセンス素子
    を有することを特徴とするエレクトロルミネセンス装
    置。
  11. 【請求項１１】請求項１乃至５のいずれかに記載のエレ
    クトロルミネセンス装置において、第１の接触層は非晶
    質シリコンからなり、第２の接触層はアルミニウム、金
    および酸化インジウムから構成されるグループから選択
    されるエレクトロルミネセンス素子を有することを特徴
    とするエレクトロルミネセンス装置。
  12. 【請求項１２】請求項１乃至１１のいずれかに記載のエ
    レクトロルミネセンス装置において、少なくとも第１と
    第２の電荷キャリヤ注入接触層の一つは支持基板に接触
    しているエレクトロルミネセンス素子を有することを特
    徴とするエレクトロルミネセンス装置。
  13. 【請求項１３】請求項９記載のエレクトロルミネセンス
    装置において、支持基板は石英ガラスからなるエレクト
    ロルミネセンス素子を有することを特徴とするエレクト
    ロルミネセンス装置。
  14. 【請求項１４】請求項１乃至１３のいずれかに記載のエ
    レクトロルミネセンス装置において、エレクトロルミネ
    センス素子によってアレイを形成し、前記第１と第２の
    電荷キャリヤ注入接触層が前記アレイに選択的にアドレ
    スすることを許容すべく配列されているエレクトロルミ
    ネセンス素子を有することを特徴とするエレクトロルミ
    ネセンス装置。
  15. 【請求項１５】発光色を制御する異なる半導体バンドギ
    ャップを有する複数の共役ポリマーからなる緻密なポリ
    マー膜層の形状の半導体層を有し、ポリマー膜として前
    駆体ポリマーの層を基板上に付着させる工程と、前記付
    着された前駆体ポリマーを高温に加熱して共役ポリマー
    に生成する工程と、第１の接触層の薄層を前記半導体層
    の第１の表面と接して設け、第２の接触層の薄層を前記
    半導体層の第２の表面と接して設ける工程とからなり、
    前記ポリマー膜は、第２の接触層を第１の接触層に対し
    て正にするように前記半導体層の第１及び第２の接触層
    間に電界をかけることにより電荷キャリヤが前記半導体
    層に注入されて、前記半導体層から発光がなされる十分
    に低い濃度の外部電荷キャリヤを有することを特徴とす
    るエレクトロルミネセンス装置の製造方法。
  16. 【請求項１６】請求項１５記載の製造方法において、先
    ず、支持基板上に前記第１の電荷注入接触層を付着させ
    て複合基板を形成し、前記第１の電荷注入接触層上にポ
    リマー膜として前記前駆体ポリマーを付着させ、次に複
    合基板及び前駆体ポリマーをポリマー膜中に前記共役ポ
    リマーを生成する高温に加熱し、最後に前記第２の電荷
    注入接触層をポリマー膜上に設けてエレクトロルミネセ
    ンス素子を形成し、該エレクトロルミネセンス素子を組
    み合わせることを特徴とするエレクトロルミネセンス装
    置の製造方法。
  17. 【請求項１７】請求項１５または１６記載の製造方法に
    おいて、前駆体を構成するポリマーは可溶体で且つポリ
    マー膜としてスピンコーティングにより前記基板上に設
    けられてエレクトロルミネセンス素子を形成し、該エレ
    クトロルミネセンス素子を組み合わせることを特徴とす
    るエレクトロルミネセンス装置の製造方法。
  18. 【請求項１８】請求項１５乃至１７のいずれかに記載の
    製造方法において、前記前駆体ポリマーはポリ（ｐ−フ
    ェニレンビニレン）［ＰＰＶ］のための前駆体ポリマー
    からなるエレクトロルミネセンス素子を形成し、該エレ
    クトロルミネセンス素子を組み合わせることを特徴とす
    るエレクトロルミネセンス装置の製造方法。
  19. 【請求項１９】請求項１５乃至１８のいずれかに記載の
    製造方法において、前記ポリマー膜は１０ｎｍから５μ
    ｍの範囲において均一な厚さからなるエレクトロルミネ
    センス素子を形成し、該エレクトロルミネセンス素子を
    組み合わせることを特徴とするエレクトロルミネセンス
    装置の製造方法。
  20. 【請求項２０】請求項１５乃至１９のいずれかに記載の
    製造方法において、第１の電荷キャリヤ注入接触層はア
    ルミニウムの薄い層からなり、一つの表面が薄い酸化層
    を形成し、前記第１の電荷キャリヤ注入接触層の薄い酸
    化層が前記半導体層の第１の表面と接触するように設け
    ることによりエレクトロルミネセンス素子を形成し、該
    エレクトロルミネセンス素子を組み合わせることを特徴
    とするエレクトロルミネセンス装置の製造方法。
  21. 【請求項２１】請求項１５乃至２０のいずれかに記載の
    製造方法において、前記第２の電荷キャリヤ注入接触層
    はアルミニウムと金からなるグループから選択されるこ
    とによりエレクトロルミネセンス素子を形成し、該エレ
    クトロルミネセンス素子を組み合わせることを特徴とす
    るエレクトロルミネセンス装置の製造方法。
  22. 【請求項２２】請求項１５乃至１９のいずれかに記載の
    製造方法において、第１の接触層はアルミニウムとマグ
    ネシウム／銀の合金からなるグループから選択され、且
    つ第２の接触層は酸化インジウムであるエレクトロルミ
    ネセンス素子を形成し、該エレクトロルミネセンス素子
    を組み合わせることを特徴とするエレクトロルミネセン
    ス装置の製造方法。
  23. 【請求項２３】請求項１５乃至１９のいずれかに記載の
    製造方法において、前記第１の接触層はアモルファスシ
    リコンからなり、第２の接触層はアルミニウム、金、お
    よび酸化インジウムからなるグループから選択されるこ
    とによりエレクトロルミネセンス素子を形成し、該エレ
    クトロルミネセンス素子を組み合わせることを特徴とす
    るエレクトロルミネセンス装置の製造方法。
  24. 【請求項２４】請求項１５乃至２３のいずれかに記載の
    製造方法において、前記第１と第２の電荷キャリヤ注入
    接触層は蒸着によって設けられることによりエレクトロ
    ルミネセンス素子を形成し、該エレクトロルミネセンス
    素子を組み合わせることを特徴とするエレクトロルミネ
    センス装置の製造方法。
  25. 【請求項２５】請求項１５乃至２４のいずれかに記載の
    製造方法において、前記支持基板が石英ガラスであるエ
    レクトロルミネセンス素子を形成し、該エレクトロルミ
    ネセンス素子を組み合わせることを特徴とするエレクト
    ロルミネセンス装置の製造方法。
JP11615997A 1989-04-20 1997-04-18 エレクトロルミネセンス装置およびその製造方法 Expired - Lifetime JP3239991B2 (ja)

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ATE117834T1 (de) 1995-02-15
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CA2030785C (en) 2000-05-30
EP0423283B1 (en) 1995-01-25
JP3249971B2 (ja) 2002-01-28
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