JP4390417B2 - Organic laminated member, color conversion member and manufacturing method thereof - Google Patents
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- JP4390417B2 JP4390417B2 JP2002017062A JP2002017062A JP4390417B2 JP 4390417 B2 JP4390417 B2 JP 4390417B2 JP 2002017062 A JP2002017062 A JP 2002017062A JP 2002017062 A JP2002017062 A JP 2002017062A JP 4390417 B2 JP4390417 B2 JP 4390417B2
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Description
【０００１】
【発明の属する技術分野】
本発明は、有機積層部材とその製造方法、特に好適には有機ＥＬカラーディスプレイに使用される色変換部材とその製造方法に関する。
【０００２】
【従来の技術】
パターニングした有機物層を積層してなる有機積層部材は様々な分野で用いられているが、そのうちの１つに有機ＥＬディスプレイなどのカラーディスプレイに用いられる蛍光体層と外光遮断層（カラーフィルター）を積層した色変換部材がある。このような色変換部材（外光遮断層および蛍光体層）は、例えば特開平９−１１５６６８号公報や1998 SID International Symposium Digest of Technical Papers/Vol XXIX、p.7-10に開示されている。
【０００３】
このような色変換部材を用いた有機ＥＬディスプレイは、典型的には、青色発光有機ＥＬ素子を、任意の蛍光変換材料（ＣＣＭ材料）を用いることにより緑色および赤色に変換し、ＲＧＢの３色を取り出すことによりフルカラー化を行う。現在既に青色発光ＥＬ素子が実用化レベルの性能を有しており、これを光源にしたＧ、Ｒの蛍光発光に関しても、高効率なものが得られている。この方式による有機ＥＬカラーディスプレイは、ＥＬ素子が単色で済み、一般的なフォトリソグラフィー法により色変換部材が形成できるので、ＥＬ材料の利用効率が高く、高精細化が容易で、生産性も高いという長所がある。そして、蛍光体層に入り込む外光により蛍光体層が励起され、ＥＬ素子の非発光状態においても蛍光体層が蛍光を発生して、コントラストが低下してしまう問題を解消するため、前記文献に開示されているように、蛍光体層の外側（外光の入射側）に、蛍光体層の励起波長を遮断し、かつ、蛍光波長を透過する外光遮断層を配置して、コントラストの向上を図り、発光色の色純度を向上させることが行われている。
【０００４】
しかしながら、このような色変換方式において用いられる色変換部材において、積層された外光遮断層と蛍光体層が混ざり込み、外光遮断層成分が、ＥＬ素子の発光または蛍光を吸収して、色変換性能を著しく低下させる場合があった。また、外光遮断層内に蛍光体層成分が混ざり込むと、外光により蛍光体層成分が蛍光を発するため、コントラストを低下させる場合があった。さらに、このような色変換方式において用いられる色変換部材を一般的なフォトリソグラフィー法により作製する際には、外光遮断層については、少なくともＲ，Ｇの２回、ならびに蛍光体層についてＲ，Ｇの２回、計４回（パターンの数だけ）のフォトリソグラフィーを行なうことになる。このフォトリソグラフィー工程は、感材塗布、乾燥、露光、現像、焼成を行なうものであるので、蛍光体層と外光遮断層を併用した色変換部材を作製するとき、結果的に製造工程数が非常に多くなる。したがって、工程数、歩留まり、生産性、コストの面での問題が生じ、フォトリソグラフィー工程数の減少が望まれている。
【０００５】
【発明が解決しようとする課題】
本発明は上記の課題を解決するものであり、本発明の目的は、有機積層部材、特にフルカラー有機ＥＬディスプレイ等に用いられる色変換部材に関し、高性能な色変換性能を有する色変換部材を提供することである。
【０００６】
また、本発明の目的は、少ない工程数で、安定的に微細なパターンを形成でき、有機積層部材、特にフルカラー有機ＥＬディスプレイ等に用いられる色変換部材の生産性を著しく向上できる製造方法を提供することである。
【０００７】
本発明の目的はさらに、そのような色変換部材を用いたフルカラー有機ＥＬディスプレイを提供することである。
【０００８】
【課題を解決するための手段】
本発明者は、複数の層が、互いの機能を妨げず、高性能な機能を発揮する有機積層部材の構成、および、その効率的な製造法を見出し本発明を完成させた。
【０００９】
したがって本発明の有機積層部材の製造方法は、基材と、前記基材上に少なくとも第１有機物層と第２有機物層とが順次積層された有機物層とからなる有機積層部材の製造方法であって、前記第１有機物層と第２有機物層とを単一のフォトリソグラフィー工程によってパターニングすることを特徴とする方法である。
【００１０】
また、本発明の有機積層部材は、基材と、前記基材上に少なくとも第１有機物層と第２有機物層とが順次積層された有機物層とからなる有機積層部材であって、前記第１有機物層と第２有機物層とが作成時に互いに混ざり合わない材料から構成されていることを特徴とするものである。
【００１１】
【発明の実施の形態】
有機積層部材の製造方法
本発明の有機積層部材の製造方法は、基材と、前記基材上に少なくとも第１有機物層と第２有機物層とが順次積層された有機物層とからなる有機積層部材の製造方法であって、前記第１有機物層と第２有機物層とを単一のフォトリソグラフィー工程によってパターニングすることを特徴としている。この方法においては、積層される有機物層は２層以上あれば何層でもよく、有機物層の間に、保護層など任意の層が積層されていてもよい。さらに単一のフォトリソグラフィー工程によってパターニングされる有機物層は、これらの積層された有機物層の全てでも一部でもよく、２層以上あれば何層でもよく、単一のフォトリソグラフィー工程でパターニングされる有機物層の間に、無機化合物等、任意の層が積層されていてもよい。
【００１２】
ここで、単一のフォトグラフィー工程とは、塗布、乾燥、露光、現像および／またはエッチングの工程を含む一連の工程を意味する。この工程内には、適宜、焼成工程が含まれていてもよい。なお、単一とはいっても、例えば、層毎に異なる薬液を用いて現像することも含まれる。具体的には例えば、第１液を塗布、乾燥後、続いて第２液を塗布、乾燥して、以後の露光、現像、エッチング、焼成工程について再度塗布、乾燥工程に戻ることなく工程を進められることを含む。より具体的には例えば、塗布▲１▼→乾燥▲１▼→塗布▲２▼→乾燥▲２▼→露光→現像（▲１▼→現像▲２▼）→エッチング（▲１▼→エッチング▲２▼）→焼成という工程が挙げられる。
【００１３】
色変換部材の製造方法
また、本発明の色変換部材の製造方法は、基材と、前記基材上に少なくとも第１有機物層と第２有機物層とが順次積層された有機物層とからなる有機積層部材の製造方法であって、前記第１有機物層と第２有機物層とを単一のフォトリソグラフィー工程によってパターニングすることを特徴とする方法において、
前記第１有機物層が蛍光体層であり、前記第２有機物層が前記蛍光体層の励起波長を遮断し、かつ、蛍光体層の蛍光波長を透過する外光遮断層である、または、 前記第２有機物層が蛍光体層であり、前記第１有機物層が外光遮断層である方法である。
【００１４】
この方法においては、少なくとも、基材／外光遮断層／蛍光体層または基材／蛍光体層／外光遮断層の積層順であれば、その他に任意の層がいずれの位置に積層されていてもよい。また、この任意の層は上記の単一のフォトリソグラフィー工程によってパターニングされる層であってもされない層であってもよい。
【００１５】
図１は、本発明の色変換部材の製造工程の例を説明する図である。図１（ａ）の透明基材１上に、図１（ｂ）のようにブラックマトリクス２を形成する。その後、図１（ｃ）のように青色外光遮断層３を塗布し、さらに、図１（ｄ）のように青色蛍光体層４を塗布し、図１（ｅ）のようにパターン露光・現像を行う。同様に緑色外光遮断層３’、緑色蛍光体層４’、赤色外光遮断層３”、赤色蛍光体層４”を形成すると図１（ｆ）のようになり、さらに図１（ｇ）のようにオーバーコート５を形成して色変換部材が完成する。
【００１６】
これに対し図２は従来の色変換部材の製造工程の例を説明する図である。図２（ａ）の透明基材１上に、図２（ｂ）のようにブラックマトリクス２を形成する。その後、図２（ｃ）のように青色外光遮断層３をパターニングし、ついで図２（ｄ）のように緑色外光遮断層３’をパターニングし、さらに、図２（ｅ）のように赤色外光遮断層３”をパターニングする。その後、図２（ｆ）のように青色蛍光体層４をパターニングし、ついで図２（ｇ）のように緑色蛍光体層４’をパターニングし、さらに図２（ｈ）のように赤色蛍光体層４”をパターニングする。そして図２（ｉ）のようにオーバーコート５を形成して色変換部材が完成する。
【００１７】
このような色変換部材の製造においては、従来の製造法では、露光・現像によるパターニングの回数が、３色の外光遮断層毎に３回と３色の蛍光体層毎の３回、合計６回必要であるのに対し、本発明の製造方法では、外光遮断層と蛍光体層を一括して、さらに保護層を設けるときには保護層も一括してパターニングするため、露光・現像の回数が合計でも３回と少なくすることができ優れている。
【００１８】
有機積層部材
本発明の有機積層部材は、基材と基材上に少なくとも第１有機物層と第２有機物層とが順次積層された有機物層とからなる有機積層部材であって、第１有機物層と第２有機物層とが作成時に互いに混ざり合わない材料から構成されている。好ましくは第１有機物層と第２有機物層との間に作成時に第１有機物層と第２有機物層とが混ざり合うことを防止する保護層を設けることができる。また、本発明の有機積層部材の製造方法により製造されたものであれば本発明の有機積層部材である。また、好ましくは有機物層が、基材上に平面的に分離配置されているものとすることができる。
【００１９】
色変換部材
本発明の有機積層部材は、好適には色変換部材とすることができる。
【００２０】
色変換部材は、本発明の有機積層部材において、第１有機物層が蛍光体層であり、第２有機物層が蛍光体層の励起波長を遮断し、かつ、蛍光体層の蛍光波長を透過する外光遮断層とする、または、第２有機物層が蛍光体層であり、第１有機物層を外光遮断層とすることで得ることができる。
【００２１】
ここで、蛍光体層は、蛍光体層側に配置されたＥＬ素子などの光源からの光を吸収し、より長波長の光に蛍光変換する層である。
【００２２】
また、外光遮断層は、侵入する外光の蛍光体励起波長を吸収し、かつ、蛍光体層からの蛍光を透過させることにより、コントラスト特性を向上させる層である。外光遮断層は、必要に応じて、蛍光色の色純度を向上させる役割も行う。
【００２３】
色変換部材においては、従来のように外光遮断層と蛍光体層との界面において、両者の材料が混ざり合っている場合、外光遮断層成分が、ＥＬ素子の発光または蛍光体層の蛍光を吸収して、色変換性能を著しく低下させてしまう。また、外光遮断層内に蛍光体層成分が混ざり込むと、外光により蛍光体層成分が蛍光を発するため、著しくコントラストを低下させてしまう。
【００２４】
したがって、本発明ではこれら外光遮断層と蛍光体層は、前述の有機物層と同様に、作成時に互いに混ざり合わない材料から形成する。好ましくは例えば、外光遮断層を水溶液から形成し、色変換フィルターを有機溶媒の溶液から形成することや、外光遮断層を有機溶媒の溶液から形成し、色変換フィルターを水溶液から形成することができる。
【００２５】
この色変換部材と有機ＥＬ素子とを組み合わせて、カラーディスプレイとすることもできる。
【００２６】
有機物層
本発明における有機物層は、有機物を含むものであれば特に限定されることはなく、基材上に形成された第１有機物層と第１有機物層上に形成する第２有機物層から少なくともなることができる。そして、第１有機物層と第２有機物層とを、作成時に互いに混ざり合わない材料から形成する。
【００２７】
本発明における「作成時に互いに混ざり合わない」とは、第１有機物層形成時、第２有機物層形成時およびパターニング時、焼成時を含め最終工程終了まで互いに混ざり合わず、作成終了後に機能が損なわれていないことを意味する。
【００２８】
また、別の好ましい態様としては、第１有機物層と第２有機物層との間に、互いが混ざり合うことを防止するための保護層が設けられている。
【００２９】
本発明において、混ざり合わないとは、例えば固形化された第１有機物層が第２有機物層を形成するための塗液にこの製造方法において溶出し、その結果両層の界面を不均一に著しく乱さないことを意味する。
【００３０】
互いに混ざり合わないような第１有機物層と第２有機物層の組み合わせとしては、例えば表面張力の差が大きな材料の組合わせや、水に可溶な材料と有機溶媒に可溶な材料との組合わせを挙げることができる。表面張力の大小関係は、簡易的には水接触角の大小関係で判断することができる。
【００３１】
具体的には、水溶性ポリマー（例えば、ポリビニルアルコール、ポリビニルピロリドン、ヒドロキシエチルセルロース、カルボキシメチルセルロース、ヒドロキシエチル（メタ）アクリレート重合体、ポリアクリル酸等）のような極性基を有する樹脂膜表面の水接触角は２０〜３０°程度の値を示し、アクリル酸エステル樹脂膜表面の水接触角は５０〜７０°程度の値を示す。このように、水接触角が好ましくは２０°以上異なる材料の組合わせを選定することにより、互いに混ざり合わないようにすることができる。
【００３２】
また、どちらも有機溶媒に可溶な系で混ざり合わない材料としては、ポリアミック酸樹脂、ポリイミド樹脂、ポリアミド樹脂と、アクリル酸エステル樹脂、アクリル酸−アクリル酸エステル共重合体、ポリケイ皮酸ビニル、環化ゴム、環状ポリオレフィン、ノボラック樹脂、または、アクリル酸エステル樹脂と、環化ゴム、環状ポリオレフィンとの組み合せのように、有機溶媒に対する溶解性が異なる樹脂を挙げることができる。
【００３３】
より具体的には、第２有機物層を溶解する溶媒（例えば溶媒１００ｇに対する溶質の溶解量の百分率である溶解度が１％以上）にて、第１有機物層が溶解しない、または溶解しにくい（例えば溶解度が１％未満）という有機物層の組合わせが好ましい。例えば、第１有機物層にポリアミック酸樹脂を用い、第２有機物層にアクリル酸−アクリル酸エステル共重合体を用いた場合、ポリアミック酸樹脂は、アクリル酸−アクリル酸エステル共重合体を溶解するエステル系溶媒には溶解しない。また、第１有機物層にアクリル酸エステル樹脂を用い、第２有機物層に環状ポリオレフィンを用いた場合、アクリル酸−アクリル酸エステル共重合体は、環状ポリオレフィンを溶解する炭化水素系溶媒には溶解しない。このような組み合わせにより、第１有機物層と第２有機物層は混ざり合わないことになる。
【００３４】
保護層
第１有機物層と第２有機物層との塗布液の表面張力差が余りない場合、例えば両者の水接触角差が２０°未満の場合や、第１有機物層と第２有機物層のある特定の溶媒に対する溶解性が類似している場合には、好適には第１有機物層と第２有機物層との間に保護層を設けることにより、二つの有機物層を混ざり合わないようにすることができる。二つの有機物層が混ざり合いにくい場合であっても、保護層を設けることは構わない。
【００３５】
保護層として用いる材料としては、第１および／もしくは第２有機物層表面の水接触角との差が好ましくは２０°以上あること、または、第１および／もしくは第２有機物層の溶媒に溶解しないことが望ましい。２０°未満の場合、または、第１および第２有機物層の溶媒に溶解する場合には、第１有機物層と保護層、または保護層と第２有機物層とが互いに混ざり合い、所望の特性が発現することを妨げるからである。また、保護層は、好ましくは第１有機物層および／または第２有機物層で用いるパターニング液（現像液）でパターニングされるものとすることができる。
【００３６】
保護層に用いる材料としては、例えば第１有機物層および第２有機物層として、有機溶媒に可溶なアクリル系樹脂を用いる場合には、水溶性ポリマー層を用いることにより、各層が互いに混ざり合うことを防止することができる。
【００３７】
また、保護層に用いる材料として、無機化合物も挙げることができる。例えば、金等の金属、酸化錫、酸化インジウム、酸化ケイ素、酸化アルミニウム、酸化チタン、酸化イットリウム、酸化ゲルマニウム、酸化亜鉛、酸化マグネシウム、酸化カルシウム、ホウ酸、酸化ストロンチウム、酸化バリウム、酸化鉛、ジルコニア、窒化ケイ素、窒化酸化ケイ素、フッ化カルシウム等の１種または２種以上の無機酸化物、無機窒化物が挙げられる。
【００３８】
保護層は、外光遮断層や蛍光体層の色変換部材の機能を有してもよく、さらには色変換部材の特性を向上させる機能を有してもよい。具体的には、顔料分散系外光遮断膜の分光特性を補正するものとして、染料系色素を含有する保護層を設けてもよい。色変換部材の特性を向上させない場合には、可視光領域において透過率が高い方（５０％以上）が望ましい。
【００３９】
ここで、複数の有機物層が混ざりあっているか否かは、積層した層の断面を観察するか、それぞれの層成分を分光的または化学的に分析することにより判定することができる。具体的には、層断面の光学顕微鏡観察や、ＳＥＭ（Scanning Electron Microscopy）観察にて、層界面が明確なこと、または、層の成分をＡＥＳ（Auger Electron Microscopy）、ＥＰＭＡ、ＸＰＳ、ダイナミックシムス、トフシムス等の分光分析、層材料をＩＲ、ＮＭＲ、ＵＶ−Ｖｉｓ、ＩＣＰ等の化学分析により膜界面に層成分が混在しない場合に有機物層が混ざりあっていないと判断できる。また、色変換部材の特性を乱さない閾値としては、白色または青色などの特定光源を用いた透過率測定や放射輝度測定において、特性を５０％以上低下させないものとすることもできる。
【００４０】
基材
本発明において基材は、有機積層部材または色変換部材に強度を付与するために設けられるものであり、材料は特に限定されるものではない。色変換部材に用いる場合であって、基材が光取り出し側に設けられる場合では、少なくとも可視光線のうち取り出される光が透過するものであれば限定されず、光源光を受けて蛍光体層に光を透過させるべき部位に設けられる場合は、少なくとも光源光を透過すれば限定されず、光源からみて光取り出し側と反対面に基材が設けられる場合には、基材にAlやAgなどの薄膜を設け反射率の高い基材とすることができる。
【００４１】
また、基材は任意に設定する使用レジストの焼成温度において、変形を伴う軟化をせず、溶融しないものとする。さらにこの温度において変質したり、光取り出し効率が低下しない基材が望ましい。例えば、アルカリガラス、無アルカリガラス、石英ガラスなどのガラス基板や、ポリエーテルサルフォンフィルムなとの１５０℃以上のガラス転移温度を有するフィルム基材が好ましい。
【００４２】
有機ＥＬ素子と組み合わせて使用する場合、水分および酸素による有機ＥＬ素子発光部の非発光領域（ダークスポット）の成長に伴う発光特性の低下を抑制するため、基材は水蒸気バリア性および酸素バリア性に優れた基材が好ましい。具体的には、水蒸気透過率が４０℃／１００％ＲＨ測定下で、１０−３ｇ／（ｍ２・ｄａｙ・ａｔｏｍ）以下、酸素透過率が２５℃／９０％ＲＨ測定下で、１０−２ｃｃ／（ｍ２・ｄａｙ・ａｔｏｍ）以下であることが望ましい。
【００４３】
【実施例】
実施例１
（基材）
縦５０ｍｍ、横５０ｍｍ、厚さ０．７ｍｍのガラス基板（日本電気硝子株式会社製ＯＡ−１０）を準備した。
【００４４】
（外光遮断層の製膜）
上記ガラス基板上に外光遮断層として、赤色カラーフィルター材料（新日鉄化学株式会社製Ｖ２５９Ｒ：３０％アントラキノン系顔料含有アクリル酸エステル系光硬化型レジスト）をスピンコート塗布し、クリーンオーブン中８０℃で１５分間プリベイク（ＰＢ）を行なった。
【００４５】
（保護層の製膜）
この上にＰＶＡ−ｓｂｑ水溶液（大日本印刷株式会社製：ポリビニルアルコール系光硬化型レジスト）をスピンコート塗布し、真空クリーンオーブン中８０℃で１５分間プリベイク（ＰＢ）を行なった。
【００４６】
（蛍光体層の製膜）
次に、クマリン６：０．０３ｍｏｌ／ｋｇ（固形分中）、ローダミン６Ｇ：１重量％（固形分中）、ローダミンＢ：１重量％（固形分中）になるように、それぞれをアクリル酸エステル系光硬化型レジスト（新日鉄化学株式会社製Ｖ２５９ＰＡ／ＰＨ５、５０％固形分濃度）中に混合して、赤色蛍光材料（固形分４５％、溶媒：プロピレングルコールメチルエーテルアセテート）を調製した。
【００４７】
次に、先の保護層上に、赤色蛍光材料をスピンコート塗布し、同様にプリベイクを行なった。
【００４８】
（露光・現像）
続いて、この積層膜を、露光機（光源：高圧水銀灯）を用いて、Ｌ／Ｓ＝５０μｍ／１００μｍのストライプパターンが得られる石英製クロムマスクを介して、露光量が１５００ｍＪ／ｃｍ２（波長３６５ｎｍにおける積算量）となる条件でパターン露光し、０．５重量％水酸化カリウム水溶液を用いて室温で１分間揺動現像した。
【００４９】
（ポストベーク）
続いてクリーンオーブン中１８０℃で３０分間焼成（ＰＯＢ）を行うことにより、外光遮断層／保護層／蛍光体層のパターン基板を得た。このときの積層膜の膜厚は約１２μｍであった。
【００５０】
実施例２
（基材）
実施例１と同様な基材を用意した。
【００５１】
（外光遮断層の製膜）
上記ガラス基板上に外光遮断層として、赤色カラーフィルター材料（３０％アントラキノン系顔料含有ＰＶＡ−ｓｂｑ水系分散液（ＰＶＡ−ｓｂｑ：大日本印刷株式会社製ポリビニルアルコール系光硬化型レジスト）をスピンコート塗布し、クリーンオーブン中８０℃で１５分間プリベイク（ＰＢ）を行なった。
【００５２】
（蛍光体層の製膜）
実施例１と同様に行った。
【００５３】
（露光・現象）
実施例１と同様に行った。
【００５４】
（ポストペーク）
続いてクリーンオーブン中１８０℃で３０分間焼成（ＰＯＢ）を行うことにより、外光遮断層／蛍光体層のパターン基板を得た。このときの積層膜の膜厚は約１０μｍであった。
【００５５】
実施例３
（基材）
実施例１と同様な基材を用意した。
【００５６】
（外光遮断層の製膜）
上記ガラス基板上に外光遮断層として、赤色カラーフィルター材料（３０％アントラキノン系顔料含有ポリアミック酸分散液（ポリアミック酸：東レ株式会社製ＳＰ９１０）をスピンコート塗布し、クリーンオーブン中１４０℃で１５分間プリベイク（ＰＢ）を行なった。
【００５７】
（蛍光体層の製膜）
実施例１と同様に行った。
【００５８】
（露光・現像）
続いて、この積層膜を、露光機（光源：高圧水銀灯）を用いて、Ｌ／Ｓ＝５０μｍ／１００μｍのストライプパターンが得られる石英製クロムマスクを介して、露光量が１５００ｍＪ／ｃｍ２（波長３６５ｎｍにおける積算量）となる条件でパターン露光し、０．５重量％水酸化カリウム水溶液を用いて室温で１分間揺動現像した。
【００５９】
（ボストペーク）
続いてクリーンオーブン中１８０℃で３０分間焼成（ＰＯＢ）を行うことにより、外光遮断層／蛍光体層のパターン基板を得た。このときの積層膜の膜厚は約１０μｍであった。
【００６０】
比較例１
保護膜を製膜しなかったこと以外は実施例１と同様にして、外光遮断層／蛍光体層パターン基板を得た。このときの積層膜の膜厚は約１０μｍであった。
【００６１】
比較例２
（基材）
実施例１と同様な基材を用意した。
【００６２】
（外光遮断層の製膜、パターニング）
外光遮断層として、赤色カラーフィルター材料（新日鉄化学株式会社製Ｖ２５９Ｒ：３０％アントラキノン系顔料含有アクリル酸エステル系光硬化型レジスト）をスピンコート塗布し、クリーンオーブン中８０℃で１５分間プリベイク（ＰＢ）を行なった。次に、これを露光機（光源：高圧水銀灯）を用いて、Ｌ／Ｓ＝５０μｍ／１００μｍのストライプパターンが得られる石英製クロムマスクを介して、露光量が１５００ｍＪ／ｃｍ２（波長３６５ｎｍにおける積算量）となる条件でパターン露光し、０．５重量％水酸化カリウム水溶液を用いて室温で１分間揺動現像した。
【００６３】
続いてクリーンオーブン中１８０℃で３０分間焼成（ＰＯＢ）を行うことにより、外光遮断層パターン基板を得た。このときの外光遮断層の膜厚は約１μｍであった。
【００６４】
（蛍光体層の製膜、パターニング）
次に、クマリン６：０．０３ｍｏｌ／：ｋｇ（固形分中）、ローダミン６Ｇ：１重量％（固形分中）、ローダミンＢ：１重量％（固形分中）になるように、それぞれをアクリル酸エステル系光硬化型レジスト（新日鉄化学株式会社製Ｖ２５９ＰＡ／ＰＨ５．５０％固形分濃度）中に混合して、赤色蛍光材料（固形分４５％、溶媒：プロピレングルコールメチルエーテルアセテート）を調製した。
【００６５】
次に、先の外光遮断層パターン上に、赤色蛍光材料をスピンコート塗布し、同様にプリベイクを行なった。
【００６６】
続いて、この積層膜を、アライメント機能を有する露光機（光源：高圧水銀灯）を用いて、Ｌ／Ｓ＝５０μｍ／１００μｍのストライプパターンが得られる石英製クロムマスクを介して、露光量が１５００ｍＪ／ｃｍ２（波長３６５ｎｍにおける積算量）となる条件で、先の外光遮断層パターンに重ねるように位置合わせを行い、パターン露光し、０．５重量％水酸化カリウム水溶液を用いて室温で１分間揺動現像した。
【００６７】
続いてクリーンオーブン中１８０℃で３０分間焼成（ＰＯＢ）を行うことにより、外光遮断層／蛍光体層のパターン基板を得た。このときの積層膜の膜厚は約１０μｍであった。
【００６８】
このように、外光遮断層／蛍光体層のパターン基板を得るのに、２回のフォトリソ工程を行う必要があるのに対し、実施例は１回の工程でよく、工程数が実施例に比べて多いのは明らかである。
【００６９】
これらの実施例、比較例の製造条件を表１に示す。
【表１】
評価
これらの実施例、比較例について以下のような評価を行った。
【００７１】
（分光特性評価）
上記の方法で作製した基板の蛍光体層面を下にして、青色励起光源（ピーク波長４７０ｎｍ、半値幅５０ｎｍの青色ＬＥＤ）に重ね、１００μｍのライン部分から基板の外光遮断層側に取り出される赤色光のスペクトルを顕微分光測定装置（顕微鏡：ニコン株式会社製、分光器：大塚電子株式会社製ＭＣＰＤ−２０００）により測定した。
【００７２】
一方、基板を重ねない状態での青色励起光源自体の発光スペクトルを測定した。
【００７３】
以上により得られたスペクトルと等色関数との演算から輝度および色度（ＣＩＥ１９３１）を算出した。
【００７４】
色変換部材の評価指標として、以下の式に従い、輝度変換効率を算出した。
【００７５】
輝度変換効率＝（基板を重ねたときの輝度）／（青色ＬＥＤの輝度）
なお、青色ＬＥＤを青色有機ＥＬ素子に置き換えても、同等の色変換部材の評価ができた。
【００７６】
（パターン形成評価）
上記の方法で作製した基板の断面形状を光学顕微鏡および走査型電子顕微鏡（ＳＥＭ）により観察した。
【００７７】
これらの評価結果を表２に示した。
【表２】
以上の結果から、比較例１および２の従来プロセスにおける色変換部材と比較して、実施例の色変換部材は輝度変換効率が向上した。
【００７９】
また、工程数の著しく減少した外光遮断層／蛍光体層を含む色変換部材の製造が可能であることが実証された。
【００８０】
また本発明の色変換部材は、パターン露光を行なうことによりフルカラーディスプレイに適用することが可能である。
【００８１】
【発明の効果】
本発明によって、有機積層部材、特にフルカラー有機ＥＬディスプレイ等に用いられる色変換部材の性能を向上できる。また、製造工程数を減らし、安定的に微細なパターンを形成でき、著しく生産性を向上できる製造方法を提供でき、その結果、歩留まり、生産性、コストの面での改善ができる。さらにそのような色変換部材を用いたフルカラー有機ＥＬディスプレイを提供できる。
【図面の簡単な説明】
【図１】本発明の色変換部材の製造方法例を説明する図である。
【図２】従来の色変換部材の製造方法例を説明する図である。
【符号の説明】
１ 透明基材
２ ブラックマトリクス
３ 青色外光遮断層
３’緑色外光遮断層
３”赤色外光遮断層
４ 青色蛍光体層
４’緑色蛍光体層
４”赤色蛍光体層
５ オーバーコート[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an organic laminated member and a manufacturing method thereof, and more particularly to a color conversion member used for an organic EL color display and a manufacturing method thereof.
[0002]
[Prior art]
Organic laminated members made by laminating patterned organic layers are used in various fields, one of which is a phosphor layer and an external light blocking layer (color filter) used for color displays such as organic EL displays. There is a color conversion member laminated. Such color conversion members (external light blocking layer and phosphor layer) are disclosed in, for example, Japanese Patent Application Laid-Open No. 9-115668 and 1998 SID International Symposium Digest of Technical Papers / Vol XXIX, p.7-10.
[0003]
An organic EL display using such a color conversion member typically converts a blue light emitting organic EL element into green and red by using an arbitrary fluorescence conversion material (CCM material), and three colors of RGB. Full color is achieved by taking out. Currently, blue light-emitting EL elements have a practical level of performance, and high-efficiency G and R fluorescent light emission using the blue light-emitting EL elements has been obtained. An organic EL color display using this method requires only a single color EL element, and a color conversion member can be formed by a general photolithography method. Therefore, the use efficiency of EL material is high, high definition is easy, and productivity is high. There is an advantage. In order to solve the problem that the phosphor layer is excited by external light entering the phosphor layer and the phosphor layer generates fluorescence even in a non-light emitting state of the EL element, and the contrast is lowered. As disclosed, an external light blocking layer that blocks the excitation wavelength of the phosphor layer and transmits the fluorescence wavelength is arranged outside the phosphor layer (external light incident side) to improve contrast. In order to improve the color purity of the emitted color.
[0004]
However, in the color conversion member used in such a color conversion method, the laminated external light blocking layer and the phosphor layer are mixed, and the external light blocking layer component absorbs the light emission or fluorescence of the EL element, so that the color In some cases, the conversion performance was significantly reduced. In addition, when the phosphor layer component is mixed in the external light blocking layer, the phosphor layer component emits fluorescence due to the external light, which may reduce the contrast. Furthermore, when a color conversion member used in such a color conversion method is manufactured by a general photolithography method, the external light blocking layer is at least R and G twice, and the phosphor layer is R, Two times of G, a total of four times (by the number of patterns) are performed. Since this photolithography process involves the application of photosensitive material, drying, exposure, development, and baking, when producing a color conversion member using both a phosphor layer and an external light blocking layer, the number of manufacturing processes is consequently reduced. Become very much. Therefore, problems in terms of the number of processes, yield, productivity, and cost arise, and a reduction in the number of photolithography processes is desired.
[0005]
[Problems to be solved by the invention]
The present invention solves the above problems, and an object of the present invention relates to a color conversion member used for an organic laminated member, particularly a full-color organic EL display, and the like, and provides a color conversion member having high-performance color conversion performance. It is to be.
[0006]
Another object of the present invention is to provide a production method that can stably form a fine pattern with a small number of steps and can significantly improve the productivity of an organic laminated member, particularly a color conversion member used for a full color organic EL display. It is to be.
[0007]
It is another object of the present invention to provide a full color organic EL display using such a color conversion member.
[0008]
[Means for Solving the Problems]
The present inventor has found the structure of an organic laminated member in which a plurality of layers exhibit high-performance functions without interfering with each other's functions, and has completed the present invention.
[0009]
Therefore, the method for producing an organic laminated member of the present invention is a method for producing an organic laminated member comprising a substrate and an organic layer in which at least a first organic layer and a second organic layer are sequentially laminated on the substrate. Then, the first organic material layer and the second organic material layer are patterned by a single photolithography process.
[0010]
The organic laminated member of the present invention is an organic laminated member comprising a base material and an organic material layer in which at least a first organic material layer and a second organic material layer are sequentially laminated on the base material. The organic material layer and the second organic material layer are made of materials that do not mix with each other at the time of creation.
[0011]
DETAILED DESCRIPTION OF THE INVENTION
Method for producing organic laminated member
The method for producing an organic laminated member of the present invention is a method for producing an organic laminated member comprising a substrate and an organic layer in which at least a first organic layer and a second organic layer are sequentially laminated on the substrate. The first organic layer and the second organic layer are patterned by a single photolithography process. In this method, the number of organic layers to be stacked may be any number as long as it is two or more, and an arbitrary layer such as a protective layer may be stacked between the organic layers. Further, the organic material layer patterned by a single photolithography process may be all or a part of these stacked organic material layers, and may be any number of layers of two or more, and is patterned by a single photolithography process. Arbitrary layers, such as an inorganic compound, may be laminated | stacked between the organic substance layers.
[0012]
Here, the single photography process means a series of processes including coating, drying, exposure, development and / or etching processes. This step may include a firing step as appropriate. In addition, even if it says that it is single, for example, developing using a different chemical for each layer is also included. Specifically, for example, after applying and drying the first liquid, subsequently applying and drying the second liquid, the subsequent exposure, development, etching, and baking processes are performed again without returning to the application and drying processes. Including being done. More specifically, for example, coating (1)-> drying (1)-> coating (2)-> drying (2)-> exposure-> development ((1)-> development (2))-> etching ((1)-> etching -2) ▼) → The step of firing can be mentioned.
[0013]
Method for producing color conversion member
Moreover, the manufacturing method of the color conversion member of this invention is a manufacturing method of the organic laminated member which consists of a base material and the organic substance layer in which the 1st organic substance layer and the 2nd organic substance layer were laminated | stacked sequentially on the said base material. In the method, the first organic layer and the second organic layer are patterned by a single photolithography process.
The first organic layer is a phosphor layer, and the second organic layer is an external light blocking layer that blocks the excitation wavelength of the phosphor layer and transmits the fluorescence wavelength of the phosphor layer, or In this method, the second organic layer is a phosphor layer, and the first organic layer is an external light blocking layer.
[0014]
In this method, at least any other layer is laminated in any position as long as the lamination order of the substrate / external light blocking layer / phosphor layer or the substrate / phosphor layer / external light blocking layer is reached. May be. The arbitrary layer may be a layer patterned or not patterned by the single photolithography process.
[0015]
FIG. 1 is a diagram for explaining an example of the manufacturing process of the color conversion member of the present invention. A
[0016]
On the other hand, FIG. 2 is a diagram for explaining an example of a manufacturing process of a conventional color conversion member. A
[0017]
In the production of such a color conversion member, in the conventional production method, the number of times of patterning by exposure / development is 3 times for each of the three external light blocking layers and 3 times for each of the three color phosphor layers. In contrast, the manufacturing method of the present invention requires six times of exposure and development because the external light blocking layer and the phosphor layer are collectively patterned, and when the protective layer is further provided, the protective layer is also patterned. However, the total can be reduced to 3 times, which is excellent.
[0018]
Organic laminated material
The organic laminated member of the present invention is an organic laminated member comprising an organic material layer in which at least a first organic material layer and a second organic material layer are sequentially laminated on the substrate, and the first organic material layer and the second organic material layer. The organic layer is made of a material that does not mix with each other at the time of creation. Preferably, a protective layer can be provided between the first organic material layer and the second organic material layer to prevent the first organic material layer and the second organic material layer from being mixed at the time of production. Moreover, if it was manufactured by the manufacturing method of the organic laminated member of this invention, it will be the organic laminated member of this invention. Moreover, it is preferable that the organic material layer be arranged in a plane on the substrate.
[0019]
Color conversion member
The organic laminated member of the present invention can be preferably a color conversion member.
[0020]
In the organic layered member of the present invention, the color conversion member is the first organic layer is a phosphor layer, the second organic layer blocks the excitation wavelength of the phosphor layer, and transmits the fluorescence wavelength of the phosphor layer. It can be obtained by using an external light blocking layer, or by forming the second organic layer as a phosphor layer and the first organic layer as an external light blocking layer.
[0021]
Here, the phosphor layer is a layer that absorbs light from a light source such as an EL element arranged on the phosphor layer side and converts the light into light having a longer wavelength.
[0022]
The external light blocking layer is a layer that improves the contrast characteristics by absorbing the phosphor excitation wavelength of the invading external light and transmitting the fluorescence from the phosphor layer. The external light blocking layer also plays a role of improving the color purity of the fluorescent color as necessary.
[0023]
In the color conversion member, when both materials are mixed at the interface between the external light blocking layer and the phosphor layer as in the prior art, the external light blocking layer component is the light emission of the EL element or the fluorescence of the phosphor layer. The color conversion performance is significantly reduced. Further, when the phosphor layer component is mixed in the external light blocking layer, the phosphor layer component emits fluorescence due to the external light, so that the contrast is remarkably lowered.
[0024]
Therefore, in the present invention, the external light blocking layer and the phosphor layer are formed of materials that do not mix with each other at the time of production, like the organic layer described above. Preferably, for example, the external light blocking layer is formed from an aqueous solution and the color conversion filter is formed from an organic solvent solution, or the external light blocking layer is formed from an organic solvent solution and the color conversion filter is formed from an aqueous solution. Can do.
[0025]
A color display can be formed by combining the color conversion member and the organic EL element.
[0026]
Organic layer
The organic material layer in the present invention is not particularly limited as long as it contains an organic material, and includes at least a first organic material layer formed on the substrate and a second organic material layer formed on the first organic material layer. Can do. And a 1st organic substance layer and a 2nd organic substance layer are formed from the material which is not mixed mutually at the time of creation.
[0027]
In the present invention, “does not mix with each other at the time of creation” means that they do not mix with each other until the end of the final process including the first organic layer formation, the second organic layer formation, patterning, and firing, and the function is impaired after the completion of the creation. Means not.
[0028]
In another preferred embodiment, a protective layer is provided between the first organic layer and the second organic layer to prevent them from mixing with each other.
[0029]
In the present invention, the term “not mixed” means that, for example, the solidified first organic material layer elutes in the coating liquid for forming the second organic material layer in this manufacturing method, and as a result, the interface between the two layers is significantly uneven. It means not disturbing.
[0030]
Examples of combinations of the first organic layer and the second organic layer that do not mix with each other include, for example, a combination of materials having a large difference in surface tension, or a combination of a material soluble in water and a material soluble in an organic solvent. A combination can be mentioned. The magnitude relationship between the surface tensions can be determined simply by the magnitude relationship between the water contact angles.
[0031]
Specifically, water contact on the surface of a resin film having a polar group such as a water-soluble polymer (for example, polyvinyl alcohol, polyvinyl pyrrolidone, hydroxyethyl cellulose, carboxymethyl cellulose, hydroxyethyl (meth) acrylate polymer, polyacrylic acid, etc.) The angle shows a value of about 20 to 30 °, and the water contact angle on the acrylic ester resin film surface shows a value of about 50 to 70 °. Thus, by selecting a combination of materials whose water contact angles are preferably different from each other by 20 ° or more, they can be prevented from being mixed with each other.
[0032]
In addition, as materials that are soluble in organic solvents and not mixed with each other, polyamic acid resin, polyimide resin, polyamide resin, acrylic ester resin, acrylic acid-acrylic ester copolymer, polyvinyl cinnamate, Examples thereof include resins having different solubility in organic solvents, such as a combination of a cyclized rubber, a cyclic polyolefin, a novolac resin, or an acrylate resin, and a cyclized rubber and a cyclic polyolefin.
[0033]
More specifically, in the solvent that dissolves the second organic layer (for example, the solubility that is a percentage of the dissolved amount of the solute with respect to 100 g of the solvent is 1% or more), the first organic layer is not dissolved or hardly dissolved (for example, A combination of organic layers with a solubility of less than 1% is preferred. For example, when a polyamic acid resin is used for the first organic layer and an acrylic acid-acrylic acid ester copolymer is used for the second organic material layer, the polyamic acid resin is an ester that dissolves the acrylic acid-acrylic acid ester copolymer. It is not soluble in system solvents. Further, when an acrylic ester resin is used for the first organic layer and a cyclic polyolefin is used for the second organic layer, the acrylic acid-acrylic ester copolymer does not dissolve in the hydrocarbon solvent that dissolves the cyclic polyolefin. . By such a combination, the first organic layer and the second organic layer are not mixed.
[0034]
Protective layer
When there is not much difference in the surface tension of the coating liquid between the first organic layer and the second organic layer, for example, when the difference in water contact angle between them is less than 20 °, or when there is a certain specific between the first organic layer and the second organic layer If the solubility in the solvent is similar, a protective layer is preferably provided between the first organic layer and the second organic layer, so that the two organic layers can be prevented from being mixed. . Even when the two organic layers are difficult to mix, a protective layer may be provided.
[0035]
The material used as the protective layer preferably has a difference of 20 ° or more from the water contact angle on the surface of the first and / or second organic layer, or does not dissolve in the solvent of the first and / or second organic layer. It is desirable. When it is less than 20 ° or when it is dissolved in the solvent of the first and second organic layers, the first organic layer and the protective layer, or the protective layer and the second organic layer are mixed with each other, and the desired characteristics are obtained. This is because it prevents the expression. The protective layer can be patterned with a patterning solution (developer) used in the first organic layer and / or the second organic layer.
[0036]
As a material used for the protective layer, for example, when an acrylic resin soluble in an organic solvent is used as the first organic layer and the second organic layer, the layers are mixed with each other by using a water-soluble polymer layer. Can be prevented.
[0037]
Moreover, an inorganic compound can also be mentioned as a material used for a protective layer. For example, metals such as gold, tin oxide, indium oxide, silicon oxide, aluminum oxide, titanium oxide, yttrium oxide, germanium oxide, zinc oxide, magnesium oxide, calcium oxide, boric acid, strontium oxide, barium oxide, lead oxide, zirconia , Silicon nitride, silicon nitride oxide, calcium fluoride and the like, or one or more inorganic oxides and inorganic nitrides.
[0038]
The protective layer may have a function of the color conversion member of the external light blocking layer or the phosphor layer, and may further have a function of improving the characteristics of the color conversion member. Specifically, a protective layer containing a dye pigment may be provided to correct the spectral characteristics of the pigment dispersion external light blocking film. In the case where the characteristics of the color conversion member are not improved, it is desirable that the transmittance is higher (50% or more) in the visible light region.
[0039]
Here, whether or not a plurality of organic layers are mixed can be determined by observing the cross section of the stacked layers or analyzing each layer component spectroscopically or chemically. Specifically, a layer interface is clear by optical microscope observation of a layer cross-section or SEM (Scanning Electron Microscopy) observation, or the components of the layer are AES (Auger Electron Microscopy), EPMA, XPS, Dynamic Sims, It can be determined that the organic material layer is not mixed when the layer component is not mixed at the film interface by spectroscopic analysis such as Tofusims or the like and chemical analysis such as IR, NMR, UV-Vis, and ICP. In addition, as a threshold value that does not disturb the characteristics of the color conversion member, the characteristics may not be reduced by 50% or more in transmittance measurement and radiance measurement using a specific light source such as white or blue.
[0040]
Base material
In this invention, a base material is provided in order to provide intensity | strength to an organic laminated member or a color conversion member, and material is not specifically limited. In the case where the base material is provided on the light extraction side when used for a color conversion member, it is not limited as long as the extracted light of at least visible light is transmitted. When it is provided at a site where light should be transmitted, it is not limited as long as it transmits light from the light source. When a base material is provided on the surface opposite to the light extraction side when viewed from the light source, the base material such as Al or Ag is used. A thin film can be provided to provide a highly reflective base material.
[0041]
Further, the base material is not softened with deformation and does not melt at the baking temperature of the resist used arbitrarily set. Furthermore, a base material that does not deteriorate at this temperature and does not lower the light extraction efficiency is desirable. For example, a glass substrate such as alkali glass, alkali-free glass, or quartz glass, or a film substrate having a glass transition temperature of 150 ° C. or higher such as a polyethersulfone film is preferable.
[0042]
When used in combination with an organic EL element, the base material has a water vapor barrier property and an oxygen barrier property in order to suppress a decrease in light emission characteristics accompanying the growth of a non-light emitting region (dark spot) of the organic EL element light emitting portion due to moisture and oxygen. A substrate excellent in the thickness is preferable. Specifically, the water vapor transmission rate is 10 ° C. under 40 ° C./100% RH measurement.-3g / (m2(Day / atom) or less, the oxygen transmission rate is 10 at 25 ° C./90% RH measurement.-2cc / (m2(Day / atom) or less.
[0043]
【Example】
Example 1
(Base material)
A glass substrate (OA-10 manufactured by Nippon Electric Glass Co., Ltd.) having a length of 50 mm, a width of 50 mm, and a thickness of 0.7 mm was prepared.
[0044]
(Formation of external light blocking layer)
A red color filter material (V259R manufactured by Nippon Steel Chemical Co., Ltd .: 30% anthraquinone pigment-containing acrylate ester-based photocurable resist) is spin-coated on the glass substrate as an external light blocking layer, and then at 80 ° C. in a clean oven. Pre-baking (PB) was performed for 15 minutes.
[0045]
(Formation of protective layer)
A PVA-sbq aqueous solution (manufactured by Dai Nippon Printing Co., Ltd .: polyvinyl alcohol-based photocurable resist) was spin-coated thereon, and prebaked (PB) at 80 ° C. for 15 minutes in a vacuum clean oven.
[0046]
(Formation of phosphor layer)
Next, each of the acrylates was coumarin 6: 0.03 mol / kg (in solids), rhodamine 6G: 1% by weight (in solids), rhodamine B: 1% by weight (in solids). A red fluorescent material (solid content 45%, solvent: propylene glycol methyl ether acetate) was prepared by mixing in a photo-curable resist (V259PA / PH5, 50% solid content concentration manufactured by Nippon Steel Chemical Co., Ltd.).
[0047]
Next, a red fluorescent material was spin-coated on the protective layer and prebaked in the same manner.
[0048]
(Exposure / Development)
Subsequently, the exposure amount of the laminated film is 1500 mJ / cm through a quartz chrome mask from which a stripe pattern of L / S = 50 μm / 100 μm is obtained using an exposure machine (light source: high pressure mercury lamp).2Pattern exposure was performed under the conditions of (integrated amount at a wavelength of 365 nm), followed by rocking development for 1 minute at room temperature using a 0.5 wt% aqueous potassium hydroxide solution.
[0049]
(Post bake)
Subsequently, baking (POB) was performed at 180 ° C. for 30 minutes in a clean oven to obtain a pattern substrate of an external light blocking layer / protective layer / phosphor layer. The film thickness of the laminated film at this time was about 12 μm.
[0050]
Example 2
(Base material)
A base material similar to that in Example 1 was prepared.
[0051]
(Formation of external light blocking layer)
Spin coating of red color filter material (30% anthraquinone pigment containing PVA-sbq aqueous dispersion (PVA-sbq: polyvinyl alcohol photocurable resist made by Dai Nippon Printing Co., Ltd.)) as an external light blocking layer on the glass substrate. This was applied and prebaked (PB) for 15 minutes at 80 ° C. in a clean oven.
[0052]
(Formation of phosphor layer)
The same operation as in Example 1 was performed.
[0053]
(Exposure / Phenomenon)
The same operation as in Example 1 was performed.
[0054]
(Postpaque)
Subsequently, baking (POB) was performed at 180 ° C. for 30 minutes in a clean oven to obtain a pattern substrate of an external light blocking layer / phosphor layer. At this time, the thickness of the laminated film was about 10 μm.
[0055]
Example 3
(Base material)
A base material similar to that in Example 1 was prepared.
[0056]
(Formation of external light blocking layer)
A red color filter material (30% anthraquinone pigment-containing polyamic acid dispersion (polyamic acid: SP910 manufactured by Toray Industries, Inc.)) was spin-coated on the glass substrate as an external light blocking layer, and the resultant was cleaned at 140 ° C. for 15 minutes in a clean oven. Pre-baking (PB) was performed.
[0057]
(Formation of phosphor layer)
The same operation as in Example 1 was performed.
[0058]
(Exposure / Development)
Subsequently, the exposure amount of the laminated film is 1500 mJ / cm through a quartz chrome mask from which a stripe pattern of L / S = 50 μm / 100 μm is obtained using an exposure machine (light source: high pressure mercury lamp).2Pattern exposure was performed under the conditions of (integrated amount at a wavelength of 365 nm), followed by rocking development for 1 minute at room temperature using a 0.5 wt% aqueous potassium hydroxide solution.
[0059]
(Boostake)
Subsequently, baking (POB) was performed at 180 ° C. for 30 minutes in a clean oven to obtain a pattern substrate of an external light blocking layer / phosphor layer. At this time, the thickness of the laminated film was about 10 μm.
[0060]
Comparative Example 1
An external light blocking layer / phosphor layer pattern substrate was obtained in the same manner as in Example 1 except that the protective film was not formed. At this time, the thickness of the laminated film was about 10 μm.
[0061]
Comparative Example 2
(Base material)
A base material similar to that in Example 1 was prepared.
[0062]
(Formation of external light blocking layer, patterning)
As an external light blocking layer, a red color filter material (V259R manufactured by Nippon Steel Chemical Co., Ltd .: 30% anthraquinone pigment-containing acrylate ester photocurable resist) was applied by spin coating, and pre-baked (PB) at 80 ° C. for 15 minutes in a clean oven. ). Next, using an exposure machine (light source: high-pressure mercury lamp), the exposure dose is 1500 mJ / cm through a quartz chromium mask from which a stripe pattern of L / S = 50 μm / 100 μm is obtained.2Pattern exposure was performed under the conditions of (integrated amount at a wavelength of 365 nm), followed by rocking development for 1 minute at room temperature using a 0.5 wt% aqueous potassium hydroxide solution.
[0063]
Subsequently, baking (POB) was performed at 180 ° C. for 30 minutes in a clean oven to obtain an external light blocking layer pattern substrate. The film thickness of the external light blocking layer at this time was about 1 μm.
[0064]
(Phosphor layer formation, patterning)
Next, acrylic acid was used so that coumarin 6: 0.03 mol /: kg (in solid content), rhodamine 6G: 1 wt% (in solid content), rhodamine B: 1 wt% (in solid content), respectively. A red fluorescent material (solid content 45%, solvent: propylene glycol methyl ether acetate) was prepared by mixing in an ester photocurable resist (V259PA / PH 5.50% solid content concentration manufactured by Nippon Steel Chemical Co., Ltd.).
[0065]
Next, a red fluorescent material was spin-coated on the external light blocking layer pattern and prebaked in the same manner.
[0066]
Subsequently, the exposure dose of this laminated film is 1500 mJ / through a quartz chrome mask from which a stripe pattern of L / S = 50 μm / 100 μm can be obtained using an exposure machine (light source: high pressure mercury lamp) having an alignment function. cm2Alignment is performed so as to overlap the previous external light blocking layer pattern under the condition of (integrated amount at wavelength 365 nm), pattern exposure is performed, and rocking is performed for 1 minute at room temperature using a 0.5 wt% potassium hydroxide aqueous solution. Developed.
[0067]
Subsequently, baking (POB) was performed at 180 ° C. for 30 minutes in a clean oven to obtain a pattern substrate of an external light blocking layer / phosphor layer. At this time, the thickness of the laminated film was about 10 μm.
[0068]
As described above, in order to obtain the pattern substrate of the external light blocking layer / phosphor layer, the photolithography process needs to be performed twice. In contrast, the embodiment may be performed once, and the number of steps is the same as the embodiment. It is clear that there are many more.
[0069]
The production conditions of these examples and comparative examples are shown in Table 1.
[Table 1]
Evaluation
These Examples and Comparative Examples were evaluated as follows.
[0071]
(Spectral characteristic evaluation)
With the phosphor layer surface of the substrate produced by the above method facing down, it is superimposed on a blue excitation light source (blue LED with a peak wavelength of 470 nm and a half-value width of 50 nm), and is extracted from the 100 μm line portion to the outside light blocking layer side of the substrate The spectrum of light was measured with a microspectrophotometer (microscope: manufactured by Nikon Corporation, spectrometer: MCPD-2000 manufactured by Otsuka Electronics Co., Ltd.).
[0072]
On the other hand, the emission spectrum of the blue excitation light source itself in a state where the substrates were not stacked was measured.
[0073]
Luminance and chromaticity (CIE 1931) were calculated from the calculation of the spectrum and the color matching function obtained as described above.
[0074]
As an evaluation index of the color conversion member, luminance conversion efficiency was calculated according to the following formula.
[0075]
Luminance conversion efficiency = (luminance when the substrates are stacked) / (luminance of blue LED)
Even when the blue LED was replaced with a blue organic EL element, an equivalent color conversion member could be evaluated.
[0076]
(Pattern formation evaluation)
The cross-sectional shape of the substrate manufactured by the above method was observed with an optical microscope and a scanning electron microscope (SEM).
[0077]
The evaluation results are shown in Table 2.
[Table 2]
From the above results, the luminance conversion efficiency of the color conversion member of the example was improved as compared with the color conversion member in the conventional processes of Comparative Examples 1 and 2.
[0079]
In addition, it was demonstrated that it is possible to manufacture a color conversion member including an external light blocking layer / phosphor layer with a significantly reduced number of steps.
[0080]
The color conversion member of the present invention can be applied to a full color display by performing pattern exposure.
[0081]
【The invention's effect】
According to the present invention, the performance of an organic laminated member, particularly a color conversion member used for a full color organic EL display or the like can be improved. In addition, it is possible to provide a manufacturing method that can reduce the number of manufacturing steps, stably form a fine pattern, and remarkably improve productivity, and as a result, improve yield, productivity, and cost. Furthermore, a full color organic EL display using such a color conversion member can be provided.
[Brief description of the drawings]
FIG. 1 is a diagram illustrating an example of a method for producing a color conversion member of the present invention.
FIG. 2 is a diagram illustrating an example of a conventional method for producing a color conversion member.
[Explanation of symbols]
1 Transparent substrate
2 Black matrix
3 Blue light blocking layer
3 'green light blocking layer
3 "red light blocking layer
4 Blue phosphor layer
4 'green phosphor layer
4 "red phosphor layer
5 Overcoat
Claims (9)
前記第１有機物層と前記第２有機物層とを、作成時に互いに混ざり合わない材料を用い、前記第１有機物層については水溶液から形成し、前記第２有機物層については有機溶媒の溶液から形成し、前記第１有機物層と第２有機物層とを単一のフォトリソグラフィー工程によってパターニングすることを特徴とする、色変換部材の製造方法。A method for producing a color conversion member comprising a base material and an organic material layer in which at least a first organic material layer and a second organic material layer are sequentially laminated on the base material,
The first organic layer and the second organic layer are made of a material that does not mix with each other at the time of creation , the first organic layer is formed from an aqueous solution, and the second organic layer is formed from an organic solvent solution. The method for producing a color conversion member, wherein the first organic material layer and the second organic material layer are patterned by a single photolithography process.
前記第１有機物層と前記第２有機物層とを、作成時に互いに混ざり合わない材料を用い、前記第１有機物層については有機溶媒の溶液から形成し、前記第２有機物層については水溶液から形成し、前記第１有機物層と第２有機物層とを単一のフォトリソグラフィー工程によってパターニングすることを特徴とする、色変換部材の製造方法。A method for producing a color conversion member comprising a base material and an organic material layer in which at least a first organic material layer and a second organic material layer are sequentially laminated on the base material,
The first organic layer and the second organic layer are made of materials that do not mix with each other at the time of creation , the first organic layer is formed from an organic solvent solution, and the second organic layer is formed from an aqueous solution. The method for producing a color conversion member, wherein the first organic material layer and the second organic material layer are patterned by a single photolithography process.
前記第１有機物層と前記第２有機物層との間に、作成時に前記第１有機物層および／または前記第２有機物層と混ざり合わない材料からなる保護層を水溶液から形成して設け、前記第１有機物層と前記第２有機物層とが作成時に互いに混ざり合うことを防止する、色変換部材の製造方法。A method for producing a color conversion member comprising: a base material; and at least a first organic material layer and a second organic material layer are laminated on the base material, and patterning them by a single photolithography process,
In between the first organic layer second organic layer, it disposed to form a protective layer made of a material immiscible with the first organic layer and / or the second organic layer at creation from an aqueous solution, the first The manufacturing method of the color conversion member which prevents that 1 organic substance layer and the said 2nd organic substance layer mutually mix at the time of preparation.
前記第１有機物層と前記第２有機物層との間に作成時に前記第１有機物層と前記第２有機物層とが混ざり合うことを防止する、水溶性ポリマーから作成された、保護層が設けられていることを特徴とする、色変換部材。A color conversion member comprising a base material and an organic material layer in which at least a first organic material layer and a second organic material layer are sequentially laminated and patterned on the base material,
A protective layer made of a water-soluble polymer is provided between the first organic material layer and the second organic material layer to prevent the first organic material layer and the second organic material layer from being mixed at the time of production. A color conversion member characterized by comprising:
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