JP6503674B2 - 樹脂積層体、それを用いた有機el素子基板、カラーフィルター基板及びそれらの製造方法ならびにフレキシブル有機elディスプレイ - Google Patents
樹脂積層体、それを用いた有機el素子基板、カラーフィルター基板及びそれらの製造方法ならびにフレキシブル有機elディスプレイ Download PDFInfo
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- JP6503674B2 JP6503674B2 JP2014200266A JP2014200266A JP6503674B2 JP 6503674 B2 JP6503674 B2 JP 6503674B2 JP 2014200266 A JP2014200266 A JP 2014200266A JP 2014200266 A JP2014200266 A JP 2014200266A JP 6503674 B2 JP6503674 B2 JP 6503674B2
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
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- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 8
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
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- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 6
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- 150000008064 anhydrides Chemical class 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
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- 238000009835 boiling Methods 0.000 description 5
- WKDNYTOXBCRNPV-UHFFFAOYSA-N bpda Chemical compound C1=C2C(=O)OC(=O)C2=CC(C=2C=C3C(=O)OC(C3=CC=2)=O)=C1 WKDNYTOXBCRNPV-UHFFFAOYSA-N 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 5
- 150000001805 chlorine compounds Chemical class 0.000 description 5
- 125000006159 dianhydride group Chemical group 0.000 description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 5
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 5
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- 125000003545 alkoxy group Chemical group 0.000 description 4
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- 238000004040 coloring Methods 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 4
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 4
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- RLUCXJBHKHIDSP-UHFFFAOYSA-N propane-1,2-diol;propanoic acid Chemical compound CCC(O)=O.CC(O)CO RLUCXJBHKHIDSP-UHFFFAOYSA-N 0.000 description 4
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 3
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 3
- FYBFGAFWCBMEDG-UHFFFAOYSA-N 1-[3,5-di(prop-2-enoyl)-1,3,5-triazinan-1-yl]prop-2-en-1-one Chemical compound C=CC(=O)N1CN(C(=O)C=C)CN(C(=O)C=C)C1 FYBFGAFWCBMEDG-UHFFFAOYSA-N 0.000 description 3
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- FFJVMNHOSKMOSA-UHFFFAOYSA-N trimethoxy-[1-(oxiran-2-ylmethoxy)butyl]silane Chemical compound CCCC([Si](OC)(OC)OC)OCC1CO1 FFJVMNHOSKMOSA-UHFFFAOYSA-N 0.000 description 1
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- ZQPNGHDNBNMPON-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)butyl]silane Chemical compound CO[Si](OC)(OC)CCC(C)OCC1CO1 ZQPNGHDNBNMPON-UHFFFAOYSA-N 0.000 description 1
- ZOWVSEMGATXETK-UHFFFAOYSA-N trimethoxy-[4-(7-oxabicyclo[4.1.0]heptan-4-yl)butyl]silane Chemical compound C1C(CCCC[Si](OC)(OC)OC)CCC2OC21 ZOWVSEMGATXETK-UHFFFAOYSA-N 0.000 description 1
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- FVHPPQILUTTWCV-UHFFFAOYSA-N undecane-1,3,7,9-tetracarboxylic acid Chemical compound CCC(C(O)=O)CC(C(O)=O)CCCC(C(O)=O)CCC(O)=O FVHPPQILUTTWCV-UHFFFAOYSA-N 0.000 description 1
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Description
第1の樹脂層の透過色度座標が0.300≦x≦0.310及び0.305≦y≦0.315の範囲にあることで、樹脂積層体を通して視認される透過光を白色に近い色調とすることができる。この透過色度座標は0.305≦x≦0.310及び0.310≦y≦0.315の範囲にあることが好ましい。ここで、「透過色度座標」とは、C光源、2度視野で測定したCIE1931表色系における透過色度の座標のことをいう。
第1の樹脂層は、その透過色度座標を上記範囲とするため、着色剤を含有することが好ましい。着色剤としては、例えば、有機顔料、無機顔料、又は染料が挙げられるが、透過光の色調調整のためには、青色顔料、青色染料、紫色顔料又は紫色染料が好ましい。
第1の樹脂層に含まれる樹脂としては、熱硬化性樹脂、熱可塑性樹脂、アルカリ可溶性樹脂等、特に限定されないが、ビニルエーテル樹脂、アクリル樹脂、ポリシロキサン樹脂、ポリイミド樹脂、ポリアミド樹脂、ポリヒドロキシスチレン樹脂、ノボラック樹脂等が好ましい。また、樹脂積層体にパターニングを施す場合には、アルカリ可溶性基を有する樹脂が好ましい。アルカリ可溶性基を有することにより、簡便にパターン加工が可能となる。アルカリ可溶性基に特に制限はないが、カルボキシル基、シラノール基及びフェノール性水酸基が、導入容易性の観点から好ましい。また、第1の樹脂層と、第2の樹脂層とを、一回の露光及び現像により一括でパターン加工して得ることが容易となる。
第1の樹脂層は、少なくとも上記各成分が溶解した溶液を用いて作製することができる。以下、その溶液を「樹脂組成物」という。第1の樹脂層を形成するための樹脂組成物は、感光性樹脂組成物であってもかまわないし、ポジ型又はネガ型のどちらであってもかまわない。
本発明の透明樹脂積層体を構成する、第2の樹脂層はポリイミド樹脂を含有する。
本発明において第2の樹脂層に含まれるポリイミド樹脂は、特に制限はなく、一般的に、下記一般式(2)で表されるポリイミド樹脂を用いることができる。これは例えば下記一般式(3)で表されるポリイミド前駆体をイミド閉環(イミド化反応)させることで得られる。イミド化反応の方法としては特に限定されず、熱イミド化や化学イミド化が挙げられる。中でも、ポリイミド樹脂膜の耐熱性、可視光領域での透明性の観点から、熱イミド化が好ましい。
第2の樹脂層は、熱架橋剤を含有していてもよい。熱架橋剤としては、エポキシ化合物やアルコキシメチル基またはメチロール基を少なくとも2つ有する化合物が好ましい。これらの基を少なくとも2つ有することで、樹脂および同種分子と縮合反応して架橋構造体が形成され、加熱処理後の硬化膜の機械強度や耐薬品性を向上させることができる。
第2の樹脂層は、無機フィラーを含有していてもよい。無機フィラーとしては、シリカ微粒子、アルミナ微粒子、チタニア微粒子、ジルコニア微粒子などが挙げられる。
第2の樹脂層は、ポリイミド前駆体および上記成分のうち必要なものが溶解した溶液を用いて作製することができる。この樹脂組成物に用いられる溶媒としては、N−メチル−2−ピロリドン、N−エチル−2−ピロリドン、ガンマブチロラクトン、1,3−ジメチル−2−イミダゾリジノン、1,3−ジエチル−2−イミダゾリジノン、N,N’−ジプロピルエチレンジアミン、N,N’−ジイソプロピルエチレンジアミン、N,N’−ジブチルエチレンジアミン、N,N−ジメチルホルムアミド、N,N−ジメチルアセトアミド、ジメチルスルホキシドなどの極性の非プロトン性溶媒、テトラヒドロフラン、ジオキサン、プロピレングリコールモノメチルエーテルなどのエーテル類、アセトン、メチルエチルケトン、ジイソブチルケトン、ジアセトンアルコールなどのケトン類、酢酸エチル、プロピレングリコールモノメチルエーテルアセテート、乳酸エチルなどのエステル類、トルエン、キシレンなどの芳香族炭化水素類などを単独、または2種以上使用することができる。
本発明の樹脂積層体は、その片側に有機EL素子を備えた有機EL素子基板や、その片側にブラックマトリクス及び着色画素を備えたカラーフィルター基板として利用できる。これらは、それぞれ有機EL素子やブラックマトリクス及び着色画素が備えられた側とは反対側に支持基板を備えていてもよい。有機EL素子やブラックマトリクス及び着色画素が備えられる側は、樹脂積層体のうち第1の樹脂層側であることが好ましい。
また、本発明の樹脂積層体は少なくとも下記(1)〜(3)の工程を含む製造方法で作製することができる。
(1)支持基板上にポリイミド前駆体を含有する樹脂組成物を塗布して塗布膜X1を得る工程。
(2)前記塗布膜X1またはその焼成膜上に、樹脂組成物を塗布して塗布膜Y1を得る工程。
(3)前記塗布膜X1と、前記塗布膜Y1とをそれぞれ焼成して、樹脂積層体を得る工程。
本発明の樹脂積層体を利用した有機EL素子は、前記(1)〜(3)の工程に加え、更に下記の工程を経て製造することができる。
(4)前記樹脂積層体上に、有機EL素子を形成する工程。
(5)支持基板から前記樹脂積層体を剥離する工程。
本発明の樹脂積層体を利用したカラーフィルターは、前記(1)〜(3)の工程に加え、更に下記の工程を経て製造することができる。
(4)前記樹脂積層体上に、ブラックマトリックスを形成する工程。
(5)前記樹脂積層体上に、着色画素を形成する工程。
(6)支持基板から前記樹脂積層体を剥離する工程。
酸無水物、ジアミンおよび溶剤の例としては、前述のポリイミド樹脂で挙げたものを用いることができる。
本発明の樹脂積層体は、液晶ディスプレイ、有機ELディスプレイ、電子ペーパーといった表示デバイス、カラーフィルター、タッチパネル、太陽電池、CMOSなどの受光デバイス等に使用することができる。特にこれらの表示デバイスや受光デバイスを、折り曲げ可能なフレキシブルデバイスとして活用する上で、本発明の樹脂積層体が好ましく用いられる。
無アルカリガラス(ガラス厚み0.7mm)上に形成された第1の樹脂層、又は第2の樹脂層の、XYZ表色系色度図における透過色度座標を大塚電子(株)製、顕微分光光度計“MCPD−2000”を用いて測定した。
A(非常に良好:◎):a*、b*の値が、0≦|a*|≦0.5かつ0≦|b*|≦0.5
B(良好:○):a*、b*の値が、0≦|a*|≦1.0かつ0.5<|b*|≦1.0、又は0.5<|a*|≦1.0かつ0≦|b*|≦1.0
C(可:△):a*、b*の値が、0≦|a*|≦1.5かつ1.0<|b*|≦1.5、又は1.0<|a*|≦1.5かつ0≦|b*|≦1.5
D(不良:×):a*、b*の値が、|a*|>1.5又は|b*|>1.5。
紫外可視分光光度計((株)島津製作所製 MultiSpec1500)を用いて、透明樹脂積層体基板の400nmにおける光透過率を測定した。
樹脂積層体を、オーブンを用いて、大気中300℃で10分間加熱させた後、大塚電子(株)製“MCPD−2000”を用いて、C光源(L*a*b*)色空間を測定し、(1)で測定された値からの変化量から以下のように耐熱性を判定した。
A(非常に良好:◎):a*、b*の値が、0≦|a*|≦0.5かつ0≦|b*|≦0.5
B(良好:○):a*、b*の値が、0≦|a*|≦1.0かつ0.5<|b*|≦1.0、又は0.5<|a*|≦1.0かつ0≦|b*|≦1.0
C(可:△):a*、b*の値が、0≦|a*|≦1.5かつ1.0<|b*|≦1.5、又は1.0<|a*|≦1.5かつ0≦|b*|≦1.5
D(不良:×):a*、b*の値が、|a*|>1.5又は|b*|>1.5。
フレキシブル有機ELディスプレイを白色表示したときの色目を目視で観察し、視認性を以下のように判定した。
A(○):白色に見える
B(△):やや着色しているように見えるが、気にならない程度の白色に見える
C(×):明らかに着色しており、白色とは言えない。
メチルトリメトキシシラン13.62g(0.1モル)、フェニルトリメトキシシラン118.98g(0.6モル)、3−トリメトキシシリルプロピルコハク酸39.39g(0.15モル)、γ−メタクリルオキシプロピルトリメトキシシラン35.16g、ダイアセトンアルコール(DAA)140.87gを500mLの三口フラスコに仕込み、室温で攪拌しながら水59.4gにリン酸0.106g(仕込みモノマーに対して0.05重量%)を溶かしたリン酸水溶液を30分かけて添加した。その後、フラスコを40℃のオイルバスに浸けて30分攪拌した後、オイルバスを30分かけて115℃まで昇温した。昇温開始1時間後に溶液の内温が100℃に到達し、そこから45分過熱攪拌した(内温は100℃以上、110℃以下)。反応中に副生成物であるメタノール、水が合計89g留出した。得られたポリシロキサンのダイアセトンアルコール溶液が、ポリマー濃度が40重量%となるようにダイアセトンアルコールを加えてシロキサン樹脂溶液(a1)を得た。得られたポリマーの重量平均分子量は7500であった。
メチルトリメトキシシラン40.86g(0.3mol)、フェニルトリメトキシシラン99.15g(0.50mol)、2−(3,4−エポキシシクロヘキシル)エチルトリメトキシシラン49.28g(0.20mol)及びDAA189.29gを500mLのフラスコに仕込み、40℃のオイルバスに漬けて撹拌しながら、水54.0g(加水分解に必要な理論量)にリン酸0.39g(仕込みモノマーに対して0.2重量部)を溶かしたリン酸水溶液を滴下ロートで10分かけて添加した。40℃で1時間撹拌した後、オイルバス温度を70℃に設定して1時間撹拌し、さらにオイルバスを30分かけて115℃まで昇温した。昇温開始1時間後に溶液の内温が100℃に到達し、そこから2時間加熱撹拌した(内温は100〜110℃)。反応中に副生成物であるメタノール、水が合計120g留出した。得られたポリシロキサンのDAA溶液に、ポリマー濃度が40wt%となるようにDAAを加え、シロキサン樹脂溶液(a2)を得た。得られたポリマーの重量平均分子量は4500であった。
500mLのフラスコに2,2‘−アゾビス(イソブチロニトリル)を3g、プロピレングリコールメチルエーテルアセテートを50g仕込んだ。その後、メタクリル酸を30g、スチレンを22,48g、シクロヘキシルメタクリレートを25.13g仕込み、室温でしばらく攪拌し、フラスコ内を窒素置換した後、70℃で5時間過熱攪拌した。次に、得られた溶液にメタクリル酸グリシジルを15g、ジメチルベンジルアミンを1g、p−メトキシフェノールを0.2g、プロピレングリコールモノメチルエーテルアセテートを100g添加し、90℃で4時間過熱攪拌した。得られたアクリル樹脂溶液は、固形分濃度が40重量%になるようにプロピレングリコールモノメチルアセテートを加えて、アクリル樹脂溶液(a3)を得た。アクリル樹脂の重量平均分子量は13500、酸価は100mgKOH/gであった。
乾燥窒素気流下、200mL4つ口フラスコに3,3’,4,4’−オキシフタル酸二無水物16.6478g(53.7mmol)、trans−1,4−ジアミノシクロへキサン6.1375g(53.7mmol)、N−メチル−2−ピロリドン100gを入れて65℃で加熱撹拌した。6時間後、冷却してポリイミド前駆体溶液(I)を得た。
trans−1,4−ジアミノシクロヘキサンを、2,2’−ビス(トリフルオロメチル)ベンジジン17.2055g(53.7mmol)に代えること以外は、合成例4と同様にして、ポリイミド前駆体溶液(II)を得た。
3,3’,4,4’−オキシフタル酸二無水物を、1,2,4,5−シクロヘキサンテトラカルボン酸二無水物12.0288g(53.7mmol)に代えること以外は、合成例5と同様にして、ポリイミド前駆体溶液(III)を得た。
(合成例7:ポリイミド前駆体溶液(IV)の合成)
3,3’,4,4’−オキシフタル酸二無水物を、3,3’,4,4’−ビフェニルテトラカルボン酸15.8137g(53.7mmol)に代えること以外は、合成例4と同様にして、ポリイミド前駆体溶液(IV)を得た。
4,4’−ジアミノフェニルエーテル(0.30モル当量)、パラフェニレンジアミン(0.65モル当量)およびビス(3−アミノプロピル)テトラメチルジシロキサン(0.05モル当量)を、850gのγ−ブチロラクトンおよび850gのN−メチル−2−ピロリドンと共に仕込み、3,3’,4,4’−オキシジフタルカルボン酸二無水物(0.9975モル当量)を添加し、80℃で3時間反応させた。無水マレイン酸(0.02モル当量)を添加し、更に80℃で1時間反応させ、ポリイミド前駆体溶液(V)(樹脂の濃度20重量%)を得た。
PB15:6 100g、分散剤としてbic chemie社“BYK2001”40g及びプロピレングリコールモノメチルアセテート860gを、直径0.3mmのジルコニアビーズ1000gとともにホモジナイザーを用いて、7000rpmで30分間分散処理後、ジルコニアビーズを濾過により除去し、顔料分散液(d1)を得た。
PB15:6をPV23に代えること以外は、顔料分散液(d1)の作製と同様にして、顔料分散液(d2)を得た。
PB15:6 100gを、PB15:6 65g及びPV23 35gに代えること以外は、顔料分散液(d1)の作製と同様にして、顔料分散液(d3)を得た。
PV23をAR289に代えること以外は、顔料分散液(d3)の作製と同様にして、顔料分散液(d4)を得た。
合成例7のポリイミド前駆体溶液(V)250gに、50gのカーボンブラック(MA100;三菱化学(株)製)および200gのN−メチル−2−ピロリドンを混合し、ダイノーミルKDL−Aを用いて、直径0.3mmのジルコニアビーズを使用して、3200rpmで3時間の分散処理を行い、黒色樹脂分散液を得た。
ピグメントレッドPR177、8.05gを3−メチル−3−メトキシブタノール50gとともに仕込み、ホモジナイザーを用い、7000rpmで5時間分散後、ガラスビーズを濾過し、除去した。アクリル共重合体溶液(ダイセル化学工業(株)製“サイクロマー”P、ACA−250、43wt%溶液)70.00g、多官能モノマーとしてペンタエリスリトールテトラメタクリレート30.00g、光重合開始剤として“イルガキュア”369、15.00gにシクロペンタノン260.00gを加えた濃度20重量%の感光性アクリル樹脂溶液(AC)134.75gを加え、感光性赤レジストを得た。同様にして、ピグメントグリーンPG38とピグメントイエローPY138からなる感光性緑レジスト、ピグメントブルーPB15:6からなる感光性青レジストを得た。
[1]着色樹脂組成物の調製
黄色灯下にて、シロキサン樹脂溶液(a1)25.0g、ジペンタエリスリトールヘキサアクリレート10.0g、1,2−オクタンジオン,1−[4−(フェニルチオ)−2−(o―ベンゾイルオキシム)]1.0g、BYK−333(ビックケミー・ジャパン(株)製)0.02g、プロピレングリコールモノメチルアセテート33.0g、ジアセトンアルコール31.0g、顔料分散液(d1)0.10gを混合し、攪拌した。続いて、0.45μmのフィルターで濾過を行い、着色樹脂組成物(A1)を得た。
50mm×70mm×0.7mm厚の無アルカリガラス上に、スピンコーターを用いて調製例1のポリイミド前駆体溶液(I)を、キュア後の膜厚が10μmになるように塗布した。その後140℃のホットプレートで4分間セミキュアを行い、塗布膜を得た。
上記で作製した樹脂積層体に調製例5で作製した黒色樹脂組成物をスピン塗布し、ホットプレートで130℃、10分間乾燥し、黒色の樹脂塗膜を形成した。ポジ型フォトレジスト(シプレー社製、“SRC−100”)をスピン塗布、ホットプレートで120℃、5分間プリベークし、超高圧水銀灯を用いて100mJ/cm2紫外線照射してマスク露光した後、2.38%のテトラメチルアンモニウムヒドロキシド水溶液を用いて、フォトレジストの現像と黒色の樹脂塗膜のエッチングを同時に行い、パターンを形成、メチルセロソルブアセテートでレジスト剥離し、ホットプレートで280℃、10分間加熱させることでイミド化させ、ポリイミド樹脂にカーボンブラックを分散した樹脂ブラックマトリクス4を形成した。ブラックマトリクスの厚さを測定したところ、1.4μmであった。
[3]で得られた、ブラックマトリクスがパターン加工された樹脂積層体に、熱処理後のブラックマトリクス開口部での膜厚が2.0μmになるようにスピナーの回転数を調整し、調製例6で調整した感光性赤レジストを樹脂積層体上に塗布、ホットプレートで100℃、10分間プリベークすることにより、赤色着色層を得た。次に、キャノン(株)製、紫外線露光機“PLA−5011”を用い、ブラックマトリクス開口部とブラックマトリクス上の一部の領域についてアイランド状に光が透過するクロム製フォトマスクを介して、100mJ/cm2(365nmの紫外線強度)で露光した。露光後に0.2%のテトラメチルアンモニウムヒドロキシド水溶液からなる現像液に浸漬を行い現像し、続いて純水洗浄後、230℃のオーブンで30分間加熱処理し、赤画素5Rを作製した。同様にして、調製例6で調整した感光性緑レジストからなる緑画素5G、感光性青レジストからなる青画素5Bを作製し、ガラス基板上に作製されたカラーフィルターを(図1)得た。
図2を参照する。上記[3]の方法で作製した樹脂積層体の第1の樹脂層3上に、プラズマCVD法を用いてSiOから成る無機ガスバリア膜13を製膜した。その後、ボトムゲート型のTFT12を形成し、このTFTを覆う状態でSi3N4から成る絶縁膜(図示せず)を形成した。次に、この絶縁膜に、コンタクトホールを形成した後、このコンタクトホールを介してTFTに接続される配線(高さ1.0μm、図示せず)を絶縁膜上に形成した。この配線は、TFT間または、後の工程で形成される有機EL素子とTFTとを接続するためのものである。
得られた平坦化層6上に、有機EL素子を形成した。まず、平坦化層上に、ITOからなる第一電極7を、コンタクトホールを介して配線(図示せず)に接続させて形成した。その後、レジストを塗布、プリベークし、所望のパターンのマスクを介して露光し、現像した。このレジストパターンをマスクとして、ITOエッチャント用いたウエットエッチングにより第一電極のパターン加工を行った。その後、レジスト剥離液(モノエタノールアミンとジエチレングリコールモノブチルエーテルの混合液)を用いて該レジストパターンを剥離した。剥離後の基板を水洗し、200℃で30分間加熱脱水して平坦化層付き電極基板を得た。平坦化層の厚さ寸法変化は、剥離液処理前に対して加熱脱水後で1%未満であった。こうして得られた第一電極は、有機EL素子の陽極に相当する。
上記[3]で得られたガラス基板付きカラーフィルターと、上記[7]で得られたガラス基板付き白色発光型有機EL素子を、粘着層を介して貼り合わせた。続いて、エキシマレーザー(波長308nm)をガラス基板側から照射することにより、ガラス基板からカラーフィルターと白色発光型有機EL素子を剥離し、フレキシブル有機ELディスプレイを作製した。
使用する顔料分散液(d1)0.10gを、顔料分散液(d2)0.50gに代えること以外は、実施例1[1]と同様に行い、着色樹脂組成物(A2)を得た。続いて、着色樹脂組成物(A2)を、キュア後の膜厚が0.2μmになるようにスピンコーターで塗布すること以外は、実施例1[2]と同様にして、膜厚10.2μmの樹脂積層体を得た。
使用する顔料分散液(d1)0.10gを、顔料分散液(d3)0.50gに代えること以外は、実施例1[1]と同様に行い、着色樹脂組成物(A3)を得た。続いて、着色樹脂組成物(A3)を、キュア後の膜厚が0.4μmになるようにスピンコーターで塗布すること以外は、実施例1[2]と同様にして、膜厚10.4μmの樹脂積層体を得た。
使用する顔料分散液(d3)を、顔料分散液(d4)に代えること以外は、実施例3と同様に行い、着色樹脂組成物(A4)、膜厚11μmの樹脂積層体、フレキシブル有機ELディスプレイを得た。得られたフレキシブル有機ELディスプレイについて、上記の方法で視認性評価を行った。
シロキサン樹脂溶液(a1)をアクリル樹脂溶液(a3)に代えること以外は、実施例1[1]着色樹脂組成物の調製、と同様にして、着色樹脂組成物(A5)を得た。続いて、着色樹脂組成物(A5)を、キュア後の膜厚が0.1μmになるようにスピンコーターで塗布すること以外は、実施例1[2]と同様にして、膜厚10.1μmの樹脂積層体を得た。 得られた樹脂積層体について、上記の方法で色度測定、光透過率測定および耐熱性試験を行った。その後、実施例1[3]〜[7]と同様にして、フレキシブル有機ELディスプレイを作製した。得られたフレキシブル有機ELディスプレイについて、上記の方法で視認性評価を行った。
シロキサン樹脂溶液(a1)をシロキサン樹脂溶液(a2)に代えること以外は、実施例3と同様にして、着色樹脂組成物(A6)、膜厚10.4μmの樹脂積層体、フレキシブル有機ELディスプレイを得た。得られた樹脂積層体について、上記の方法で色度測定、光透過率測定および耐熱性試験を行った。また、得られたフレキシブル有機ELディスプレイについて、上記の方法で視認性評価を行った。
ポリイミド前駆体溶液(I)をポリイミド前駆体溶液(II)に代えること以外は、実施例3と同様にして、膜厚10μmのポリイミド樹脂を含有する第2の樹脂層(P2)および膜厚0.4μmのポリシロキサン樹脂を含有する第1の樹脂層(A1)からなる膜厚10.4μmの樹脂積層体を得た。得られた樹脂積層体について、上記の方法で色度測定、光透過率測定および耐熱性試験を行った。その後、実施例1[3]〜[7]と同様にして、フレキシブル有機ELディスプレイを得た。得られたフレキシブル有機ELディスプレイについて、上記の方法で視認性評価を行った。
ポリイミド前駆体溶液(II)をポリイミド前駆体溶液(III)に代えること、および着色樹脂組成物(A3)を、キュア後の膜厚が0.3μmになるようにスピンコーターで塗布すること以外は、実施例3と同様にして、膜厚10μmのポリイミド樹脂を含有する第2の樹脂層(P3)および膜厚0.3μmのポリシロキサン樹脂を含有する第1の樹脂層(A3)からなる膜厚10.3μmの樹脂積層体およびフレキシブル有機ELディスプレイを得た。得られた樹脂積層体について、上記の方法で色度測定、光透過率測定および耐熱性試験を行った。また、得られたフレキシブル有機ELディスプレイについて、上記の方法で視認性評価を行った。
ポリイミド前駆体溶液(I)をポリイミド前駆体溶液(IV)に代えること以外は、実施例3と同様にして、膜厚10μmのポリイミド樹脂を含有する第2の樹脂層(P4)および膜厚0.4μmのポリシロキサン樹脂を含有する第1の樹脂層(A3)からなる膜厚10.4μmの樹脂積層体を得た。得られた樹脂積層体について、上記の方法で色度測定、光透過率測定および耐熱性試験を行った。その後、実施例1[3]〜[7]と同様にして、フレキシブル有機ELディスプレイを得た。得られたフレキシブル有機ELディスプレイについて、上記の方法で視認性評価を行った。
実施例1[2]第1の樹脂層(2層目)の作製を行わないこと以外は、実施例1と同様にして、塗布膜(P1)、フレキシブル有機ELディスプレイを得た。
顔料分散液を添加しないこと以外は、実施例1と同様にして、樹脂組成物(A8)、続けて膜厚10.2μmの樹脂積層体、フレキシブル有機ELディスプレイを得た。
2 第2の樹脂層
3 第1の樹脂層
4 ブラックマトリックス
5R 赤色画素
5G 緑色画素
5B 青色画素
6 平坦化層
7 第一電極
8 絶縁層
9W 白色有機EL発光層
10 第二電極
11 封止膜
12 TFT層
13 ガスバリア層
Claims (12)
- 第1の樹脂層と、ポリイミド樹脂を含有する第2の樹脂層を有する、2層以上の樹脂積層体であって、前記第1の樹脂層が、ポリシロキサン樹脂と、青色顔料および紫色顔料から選ばれる着色剤とを含み、前記着色剤が2種類以上含まれており、波長400nmにおける透過率が90%以上であり、第1の樹脂層の、XYZ表色系色度図における透過色度座標が0.300≦x≦0.310及び0.305≦y≦0.315の範囲にあることを特徴とする、樹脂積層体。
- 前記第1の樹脂層が、感光性樹脂を含有する、請求項1に記載の樹脂積層体。
- 請求項1〜3のいずれかに記載の樹脂積層体の片側に、有機EL素子を備えた、有機EL素子基板。
- 前記樹脂積層体の、有機EL素子を備えた側とは反対側に支持基板を備えた、請求項4記載の有機EL素子基板。
- 請求項1〜3のいずれかに記載の樹脂積層体の片側に、ブラックマトリクス及び着色画素を備えた、カラーフィルター基板。
- 前記樹脂層体の、ブラックマトリクス及び着色画素を備えた側とは反対側に支持基板を備えた、請求項6記載のカラーフィルター基板。
- 少なくとも下記(1)〜(5)の工程を含む、請求項4記載の有機EL素子基板の製造方法。
(1)支持基板上に、ポリイミド前駆体を含有する樹脂組成物を塗布して塗布膜X1を得る工程。
(2)前記塗布膜X1上またはその焼成膜に樹脂組成物を塗布して塗布膜Y1を得る工程。
(3)前記塗布膜X1と前記塗布膜Y1とをそれぞれ加熱して、樹脂積層体を得る工程。
(4)前記樹脂積層体上に、有機EL素子を形成する工程。
(5)支持基板から前記樹脂積層体を剥離する工程。 - 前記塗布膜Y1を得るための樹脂組成物が感光性樹脂を含有し、前記塗布膜Y1を得る工程の後、塗布膜Y1を露光及び現像する工程を含む、請求項8記載の有機EL素子基板の製造方法。
- 少なくとも下記(1)〜(6)の工程を含む、請求項6記載のカラーフィルター基板の製造方法。
(1)支持基板上に、ポリイミド前駆体を含有する樹脂組成物を塗布して塗布膜X1を得る工程。
(2)前記塗布膜X1またはその焼成膜上に樹脂組成物を塗布して塗布膜Y1を得る工程。
(3)前記塗布膜X1と前記塗布膜Y1とをそれぞれ加熱して、樹脂積層体を得る工程。
(4)前記樹脂積層膜上に、ブラックマトリクスを形成する工程。
(5)前記樹脂積層膜上に、着色画素を形成する工程。
(6)支持基板から前記樹脂積層体を剥離する工程。 - 前記塗布膜Y2を得る工程の後、塗布膜Y2を露光及び現像する工程を含む、請求項10記載のカラーフィルター基板の製造方法。
- 請求項4記載の有機EL素子基板と、請求項6記載のカラーフィルター基板と、を備えたフレキシブル有機ELディスプレイ。
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