JP5679565B2 - 透明導電膜、透明導電膜付き基材、及びそれを用いた有機エレクトロルミネッセンス素子 - Google Patents
透明導電膜、透明導電膜付き基材、及びそれを用いた有機エレクトロルミネッセンス素子 Download PDFInfo
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- JP5679565B2 JP5679565B2 JP2011053424A JP2011053424A JP5679565B2 JP 5679565 B2 JP5679565 B2 JP 5679565B2 JP 2011053424 A JP2011053424 A JP 2011053424A JP 2011053424 A JP2011053424 A JP 2011053424A JP 5679565 B2 JP5679565 B2 JP 5679565B2
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- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 1
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- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
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Images
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H10K71/80—Manufacture or treatment specially adapted for the organic devices covered by this subclass using temporary substrates
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Description
金属細線として、公知論文「Materials Chemistry and Physics vol.114 p333-338 “Preparation of Ag nanorods with high yield by polyol process”」に準じて銀ナノワイヤを作製した。この場合、銀ナノワイヤの平均直径を50nmとし、銀ナノワイヤの平均長さを5μmとした。
上記の銀ナノワイヤ3質量部とセルロース樹脂1質量部とを水を分散媒として混合した。それにより、固形分4.0%の金属細線を含む第1の透明樹脂層の材料を作製した。
三菱化学株式会社製シリコーン樹脂MS51(酸化物換算51%)9.8質量部をイソプロピルアルコール(以下、IPAという)85.2質量部に溶解した。次に、このシリコーン樹脂とIPAとの混合液に、0.1H硝酸5質量部を加えてよく混合した後、25℃の恒温雰囲気下において1時間撹拌混合した。それにより、固形分5%の第1の多孔質層の材料を作製した。
三菱化学株式会社製シリコーン樹脂MS51(酸化物換算51%)5.88質量部をIPA82.54質量部に溶解した。次に、このシリコーン樹脂とIPAとの混合液にITOナノ粒子(シーアイ化成株式会社製、固形分30%のIPA分散液)6.67質量部を添加した。さらに、このITOナノ粒子が添加されたシリコーン樹脂とIPAとの混合液に0.1H硝酸5質量部を加えてよく混合した後、25℃の恒温雰囲気下において1時間撹拌混合した。それにより、固形分5%の第2の多孔質層の材料を作製した。
三菱化学株式会社製シリコーン樹脂MS51(酸化物換算51%)9.8質量部をIPA85.2質量部に溶解した。次に、このシリコーン樹脂とIPAとの混合液に0.1Hアンモニア5質量部を加えてよく混合した後、25℃の恒温雰囲気下において1時間撹拌混合した。それにより、固形分5%の第3の多孔質層の材料を作製した。
ポリ(3,4−エチレンジオキシチオフェン)1質量部とポリアニオンポリ(スチレンスルホン酸塩)2.5質量部とを水を分散媒として混合した。それにより、固形分3.5%の導電性高分子を含む第2の透明樹脂層の材料を作製した。
基材として、コーニング社製無アルカリガラスNo.1737(波長が500nmの光の屈折率が1.50〜1.53)を用意した。次に、この基材上に、スピンコート法により、予め作製した金属細線を含む第1の透明樹脂層の材料を厚さが100nmとなるように塗布し、100℃で5分間加熱した。それにより、基材上に第1の透明樹脂層を形成した。次に、第1の透明樹脂層上に、第1の多孔質層の材料を厚さが30nmとなるように塗布し、100℃で5分間加熱した。それにより、第1の透明樹脂層上に水との接触角が30度である多孔質層を形成した。次に、多孔質層上に、第2の透明樹脂層の材料を厚さが100nmとなるように塗布し、100℃で5分間加熱した。それにより、多孔質層上に、第2の透明樹脂層を形成した。こうして、実施例1のサンプルを作製した。
第1の多孔質層の材料の代わりに、第2の多孔質層の材料を用いて、孔径が10nmであり、水に対する接触角が60度である第2の多孔質層を形成した点を除いて、上記実施例1と同様にして、実施例2のサンプルを作製した。
基材上に第1の多孔質層の材料を厚さが300nmとなるように塗布した点を除いて、上記実施例1と同様にして、実施例3のサンプルを作製した。
第1の多孔質層の材料の代わりに、第3の多孔質層の材料を用いて、孔径が300nmであり、水に対する接触角が30度である第3の多孔質層を形成した点を除いて、上記実施例1と同様にして、実施例4のサンプルを作製した。
離型フィルム上に、実施例1と同様にして、順次、第1の透明樹脂層と、第1の多孔質層と、第2の透明樹脂層と、を形成した。次に、この離型フィルム、第1の透明樹脂層、第1の多孔質層、第2の透明樹脂層から成る積層体をガラス基板上に転写した。こうして、実施例5のサンプルを作製した。
実施例1のサンプル上に株式会社同人化学研究所製N,N−ジフェニル−N,N−ビス3−メチル−フェニル−1,1−ジフェニル−4,4ジアミンを真空蒸着した。これにより、実施例1のサンプル上に正孔輸送層を形成した。この場合、正孔輸送層の厚さを50nmとした。次に、正孔輸送層上に株式会社同人化学研究所製アルミキノリノール錯体(トリス(8−ヒドロキノリン)アルミニウム)を真空蒸着した。これにより、正孔輸送層上に有機発光層を形成した。この場合、有機発光層の厚さを50nmとした。次に、有機発光層上にアルミニウムを真空蒸着した。これにより、有機発光層上にアルミニウムから成る導体層を形成した。こうして、実施例1のサンプルを陽極とする有機EL素子を作製した。
有機EL素子の陽極として、実施例2のサンプルを用いた点を除いて、上記実施例6と同様にして、実施例7のサンプルを作製した。
有機EL素子の陽極として、実施例3のサンプルを用いた点を除いて、上記実施例6と同様にして、実施例8のサンプルを作製した。
有機EL素子の陽極として、実施例4のサンプルを用いた点を除いて、上記実施例6と同様にして、実施例9のサンプルを作製した。
有機EL素子の陽極として、実施例5のサンプルを用いた点を除いて、上記実施例6と同様にして、実施例10のサンプルを作製した。
第1の多孔質層と第2の透明樹脂層とを形成しなかった点を除いて、上記実施例1と同様にして、比較例1のサンプルを作製した。
第1の多孔質層を形成しなかった点を除いて、上記実施例1と同様にして、比較例2のサンプルを作製した。
第1の多孔質層の代わりに、スパッタ法により孔径が0.1mmの二酸化ケイ素(SiO2)を形成した点を除いて、上記実施例1と同様にして、比較例3のサンプルを作製した。
有機EL素子の陽極として、比較例1のサンプルを用いた点を除いて、上記実施例6と同様にして、比較例4のサンプルを作製した。
有機EL素子の陽極として、比較例2のサンプルを用いた点を除いて、上記実施例6と同様にして、比較例5のサンプルを作製した。
有機EL素子の陽極として、比較例3のサンプルを用いた点を除いて、上記実施例6と同様にして、比較例6のサンプルを作製した。
三菱化学株式会社製ロレスタEP MCP−T360を用いて各サンプルの表面抵抗値を測定した。
株式会社島津製作所製ナノサーチ顕微鏡SFT−3500を用いて、測定視野を縦30μm及び横30μmとして、各サンプルの表面粗さを測定した。
各サンプルの透明導電膜の表面の状態を目視により観察した。
有機EL素子に逆電圧(発光させる際に流す電流と逆向き)を5[V]印加し、有機EL素子は点灯するか否かを調べた。
可能である。例えば、基材2上に、第2の透明樹脂層9と、第3の透明樹脂層10とが順次積層され、第1の透明樹脂層8が、水に対して可溶な樹脂を含んでもよい。つまり、水に対して可溶な上層の透明樹脂層を塗布により形成する場合に、それが下層の透明樹脂層と混合しないように、それらの間に水に対して不溶な又は耐水性を持つ樹脂を含む透明樹脂層を設けたものであればよい。また、透明導電膜3は、液晶ディスプレイ、プラズマディスプレイ、又は太陽有機電池等の透明電極として用いることができる。
2 基材
6 透明導電膜付き基材
7 金属細線(金属ナノワイヤ又はカーボンナノチューブ)
8 第1の透明樹脂層
9 第2の透明樹脂層
10 第3の透明樹脂層
Claims (9)
- 金属細線又はカーボン系繊維状材料を含む第1の透明樹脂層と、
導電性高分子を含む第2の透明樹脂層と、
前記第1の透明樹脂層と前記第2の透明樹脂層との間に設けられる第3の透明樹脂層と、を備え、
前記第1の透明樹脂層及び前記第2の透明樹脂層の少なくとも一方は、水に対して可溶な樹脂を含み、
前記第3の透明樹脂層は、水に対して不溶な又は耐水性を持つ樹脂を含むことを特徴とする透明導電膜。 - 前記金属細線は、金属ナノワイヤであることを特徴とする請求項1に記載の透明導電膜。
- 前記カーボン系繊維状材料は、カーボンナノチューブであることを特徴とする請求項1に記載の透明導電膜。
- 前記第3の透明樹脂層は、多孔質層として形成され、
前記第3の透明樹脂層の孔径は、0.5nm以上1μm以下であることを特徴とする請求項1乃至請求項3のいずれか一項に記載の透明導電膜。 - 前記第3の透明樹脂層の厚さは、5nm以上1μm以下であることを特徴とする請求項1乃至請求項4のいずれか一項に記載の透明導電膜。
- 前記第3の透明樹脂層の表面における水に対する接触角は、75°以下であることを特徴とする請求項1乃至請求項5のいずれか一項に記載の透明導電膜。
- 前記第3の透明樹脂層は、シリコーン樹脂から成るバインダーを含むことを特徴とする
請求項1乃至請求項6のいずれか一項に記載の透明導電膜。 - 基材上に請求項1乃至請求項7のいずれか一項に記載の透明導電膜が形成されたことを特徴とする透明導電膜付き基材。
- 請求項8に記載の透明導電膜付き基材を備えたことを特徴とする有機エレクトロルミネッセンス素子。
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US13/812,013 US9017807B2 (en) | 2011-03-10 | 2012-02-07 | Transparent conductive film, substrate with transparent conductive film, and organic electroluminescence element using the same |
CN201280002256.5A CN103068573B (zh) | 2011-03-10 | 2012-02-07 | 透明导电膜、带透明导电膜的基材及使用其的有机电致发光元件 |
PCT/JP2012/052695 WO2012120949A1 (ja) | 2011-03-10 | 2012-02-07 | 透明導電膜、透明導電膜付き基材、及びそれを用いた有機エレクトロルミネッセンス素子 |
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US20140170427A1 (en) * | 2012-12-13 | 2014-06-19 | Carestream Health, Inc. | Anticorrosion agents for transparent conductive film |
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WO2015025792A1 (ja) * | 2013-08-22 | 2015-02-26 | 昭和電工株式会社 | 透明電極及びその製造方法 |
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