JP6074215B2 - 有機エレクトロルミネッセンス表示素子の製造方法 - Google Patents
有機エレクトロルミネッセンス表示素子の製造方法 Download PDFInfo
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- JP6074215B2 JP6074215B2 JP2012225064A JP2012225064A JP6074215B2 JP 6074215 B2 JP6074215 B2 JP 6074215B2 JP 2012225064 A JP2012225064 A JP 2012225064A JP 2012225064 A JP2012225064 A JP 2012225064A JP 6074215 B2 JP6074215 B2 JP 6074215B2
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- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- NQSMEZJWJJVYOI-UHFFFAOYSA-N Methyl 2-benzoylbenzoate Chemical compound COC(=O)C1=CC=CC=C1C(=O)C1=CC=CC=C1 NQSMEZJWJJVYOI-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004696 Poly ether ether ketone Substances 0.000 description 1
- 229930182556 Polyacetal Natural products 0.000 description 1
- 239000004962 Polyamide-imide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920000265 Polyparaphenylene Polymers 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- UUQQGGWZVKUCBD-UHFFFAOYSA-N [4-(hydroxymethyl)-2-phenyl-1h-imidazol-5-yl]methanol Chemical compound N1C(CO)=C(CO)N=C1C1=CC=CC=C1 UUQQGGWZVKUCBD-UHFFFAOYSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000005370 alkoxysilyl group Chemical group 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
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- 150000001721 carbon Chemical group 0.000 description 1
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- 239000006229 carbon black Substances 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
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- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 125000005578 chrysene group Chemical group 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
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- 238000006731 degradation reaction Methods 0.000 description 1
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
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Description
上記導電材料に含まれている硬化性化合物は特に限定されない。上記硬化性化合物として、従来公知の硬化性化合物が使用可能である。上記硬化性化合物は1種のみが用いられてもよく、2種以上が併用されてもよい。
上記導電材料は、硬化剤を含む。該硬化剤は、熱硬化剤を含んでいてもよく、光硬化開始剤を含んでいてもよい。該硬化剤は、カチオン発生剤を含む。該カチオン発生剤として従来公知のカチオン発生剤が使用可能である。また、本発明では、カチオン発生剤は、導電材料を光硬化のみさせるための光カチオン発生剤として用いるのではなく、導電材料を少なくとも熱硬化させるための熱カチオン発生剤として用いることが好ましい。さらに、本発明では、カチオン発生剤は、導電材料を光硬化させるための光カチオン発生剤として用いるのではなく、導電材料を熱硬化させるための熱カチオン発生剤として用いることがより好ましい。上記カチオン発生剤は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記導電性粒子は、導電性の表面に導電部を有していればよい。該導電部は導電層であることが好ましい。図3に、導電性粒子の一例を断面図で示すように、導電性粒子11は、基材粒子12と、基材粒子12の表面上に配置された導電層13とを備えていてもよい。導電性粒子は、全体が導電部である金属粒子であってもよい。なかでも、コストを低減したり、導電性粒子の柔軟性を高くして、電極間の導通信頼性を高めたりする観点からは、基材粒子と、基材粒子の表面上に配置された導電層とを有する導電性粒子が好ましい。
上記導電材料は、有機粒子を含むことが好ましい。該有機粒子はゲル化剤として作用する。上記有機粒子は、常温において導電材料中で膨潤し、導電材料の粘度を適度に向上させる。さらに、上記有機粒子は、導電材料の硬化中に粘度の低下を抑制する作用を有する。また、上記有機粒子を無機フィラーと組み合わせて用いることにより、基板を減圧雰囲気下で貼り合わせる場合でも、硬化物にボイドが生じ難くなる。上記有機粒子は、1種のみが用いられてもよく、2種以上が併用されてもよい。
上記導電材料を製造する方法は特に限定されず、例えば、ホモディスパー、ホモミキサー、万能ミキサー、プラネタリウムミキサー、ニーダー、3本ロール等の混合機を用いて、硬化性成分と導電性粒子と必要に応じて他の成分とを混合する方法が挙げられる。
(1)導電材料の調製:
ビスフェノールA変性エポキシ樹脂(DIC社製「EPICLON EXA−4850−150」)40重量部、及びビスフェノールFエポキシ樹脂(DIC社製「EXA−835LV」)30重量部に、カチオン発生剤であるSI−60L(三新化学社製のサンエイド)3重量部と、光硬化性化合物であるエポキシアクリレート(ダイセル・サイテック社製「EBECRYL3702」)20重量部と、光硬化開始剤であるアシルホスフィンオキサイド系化合物(チバ・ジャパン社製「DAROCUR TPO」)1重量部と、フィラーである平均粒子径0.25μmのシリカ10重量部と、平均粒子径10μmの導電性粒子A4重量部とを添加し、遊星式攪拌機を用いて2000rpmで5分間攪拌することにより、導電ペーストを得た。
有機EL素子を備えており、L/Sが50μm/50μm、長さ1mmのアルミニウム電極パターンが上面に形成された有機EL基板(第1の基板)を用意した。また、L/Sが50μm/50μm、長さ2mmのアルミニウム電極パターンが下面に形成された封止基板(第2の基板)を用意した。
導電ペースト層の加熱温度を100℃から120℃に変更したこと以外は実施例1と同様にして、有機EL表示素子を得た。
上記第2の基板を積層する前に光の照射を行い、光の照射後に速やかに上記第2の基板を積層したこと以外は実施例1と同様にして、有機EL表示素子を得た。
熱硬化性化合物の種類を、ビスフェノールA変性エポキシ樹脂(DIC社製「EPICLON EXA−4850−150」)から、フェノールノボラック型エポキシ樹脂(DIC社製「EPICLON N−770」)に変更したこと以外は実施例1と同様にして、導電ペーストを得た。得られた導電ペーストを用いて、実施例1と同様にして、有機EL表示素子を得た。
カチオン発生剤の種類を、SI−60L(三新化学社製のサンエイド)から、CXC−1612(K−pure社製のK−pure CXC)に変更したこと以外は実施例1と同様にして、導電ペーストを得た。得られた導電ペーストを用いて、実施例1と同様にして、有機EL表示素子を得た。
カチオン発生剤であるSI−60Lを添加せずに、熱硬化剤(イミダゾール化合物、四国化成工業社製「2P−4MZ」)15重量部を添加したこと以外は、実施例1と同様にして、異方性導電ペーストを得た。得られた導電ペーストを用いて、実施例1と同様にして、有機EL表示素子を得た。
導電性粒子Aの粒子径を60μmに変更ししたこと以外は実施例1と同様にして、導電ベーストを得た。また、上記第1の基板の電極をL/Sが500μm/500μm、長さ20mmのアルミニウム電極パターンに変更し、封止基板(第2の基板)の電極を、L/Sが500μm/500μm、長さ20mmのITO電極パターンに変更し、上記第1の基板上に、作製直後の導電ペーストを幅1.5mm、厚さ120μmとなるようにディスペンサーを用いて塗工したこと以外は、実施例1と同様にして、有機EL表示素子を得た。
(1)導電材料の調製:
光硬化性化合物であるエポキシアクリレート(ダイセル・サイテック社製「EBECRYL3702」)と、光硬化開始剤であるアシルホスフィンオキサイド系化合物(チバ・ジャパン社製「DAROCUR TPO」)とを配合しなかったこと以外は実施例1と同様にして、導電ペーストを得た。
実施例1と同じ第1,第2の基板を用意した。上記第1の基板上に、作製直後の導電ペーストを幅1.5mm、厚さ40μmとなるようにディスペンサーを用いて塗工し、導電ペースト層を形成した。次に、導電ペースト層上に上記第2の基板を、電極同士が対向するように積層した。その後、大橋製作所社製「BD−02」を用い、導電ペースト層の温度が100℃(本圧着温度)となるように加熱圧着ヘッドの温度を調整しながら、上記第2の基板の上面に加圧圧着ヘッドを載せ、1MPaの圧力をかけて100℃で15分間導電ペースト層を硬化させ、有機EL表示素子を得た。比較例1では、光の照射を行わなかった。
(1)ボイドの有無
得られた有機EL表示素子において、導電材料層が硬化した接続部にボイドが生じているか否かを観察した。ボイドの有無を下記の基準で判定した。
○:ボイドなし
△:ボイドはあるものの、電極幅及び電極間幅よりも大きいボイドはない
×:電極幅又は電極間幅よりも大きいボイドがある
得られた有機EL表示素子の上下の電極間の接続抵抗をそれぞれ、4端子法により測定した。100箇所の接続抵抗の平均値を算出した。なお、電圧=電流×抵抗の関係から、一定の電流を流した時の電圧を測定することにより接続抵抗を求めることができる。得られた有機EL表示素子における電極間の導通信頼性を下記の基準で判定した。
○○:3Ω未満
○:3Ω以上、4Ω未満
△:4Ω以上、5Ω未満
×:5Ω以上
2…第1の基板
2a…第1の電極
3…接続部
3A…導電材料層
3B…Bステージ化された導電材料層
4…第2の基板
4a…第2の電極
5…導電性粒子
11…導電性粒子
12…基材粒子
13…導電層
Claims (6)
- 有機エレクトロルミネッセンス表示素子用基板である第1の基板の表面に、硬化性成分と導電性粒子とを含む導電材料により導電材料層を配置する工程と、
前記導電材料層の前記第1の基板側とは反対側の表面に、有機エレクトロルミネッセンス表示素子用基板である第2の基板を配置する工程と、
前記導電材料層に光を照射し、かつ前記導電材料層を加熱して、前記導電材料層を光硬化及び熱硬化させて、前記第1,第2の基板を電気的に接続している接続部を形成する工程とを備え、
前記硬化性成分が、硬化性化合物とカチオン発生剤とを含み、
前記カチオン発生剤の作用により、前記導電材料層を熱硬化させる、有機エレクトロルミネッセンス表示素子の製造方法。 - 120℃を超える温度に加熱せずに、120℃以下の温度に加熱して、前記導電材料層を熱硬化させる、請求項1に記載の有機エレクトロルミネッセンス表示素子の製造方法。
- 前記導電材料層に光を照射した後に前記導電材料層を加熱するか、又は前記導電材料層を加熱した後に前記導電材料層に光を照射する、請求項1又は2に記載の有機エレクトロルミネッセンス表示素子の製造方法。
- 前記第1の基板が表面に第1の電極を有し、
前記第2の基板が表面に第2の電極を有し、
前記第1の電極と前記第2の電極とを、前記導電性粒子により電気的に接続する、請求項1〜3のいずれか1項に記載の有機エレクトロルミネッセンス表示素子の製造方法。 - 前記第1の基板と前記第2の基板とが、有機エレクトロルミネッセンス素子を備える有機エレクトロルミネッセンス基板と封止基板とである、請求項1〜4のいずれか1項に記載の有機エレクトロルミネッセンス表示素子の製造方法。
- 100℃を超える温度に加熱せずに、100℃以下の温度に加熱して、前記導電材料層を熱硬化させる、請求項1〜5のいずれか1項に記載の有機エレクトロルミネッセンス表示素子の製造方法。
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