JP5690098B2 - 銀ナノ粒子から低プロセス温度で高導電性構造体を形成するための新規なプロセス及び高導電性構造体 - Google Patents
銀ナノ粒子から低プロセス温度で高導電性構造体を形成するための新規なプロセス及び高導電性構造体 Download PDFInfo
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- JP5690098B2 JP5690098B2 JP2010181695A JP2010181695A JP5690098B2 JP 5690098 B2 JP5690098 B2 JP 5690098B2 JP 2010181695 A JP2010181695 A JP 2010181695A JP 2010181695 A JP2010181695 A JP 2010181695A JP 5690098 B2 JP5690098 B2 JP 5690098B2
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- highly conductive
- silver
- heating
- containing nanoparticles
- Prior art date
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- H05K3/00—Apparatus or processes for manufacturing printed circuits
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- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- H05K1/097—Inks comprising nanoparticles and specially adapted for being sintered at low temperature
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- H—ELECTRICITY
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
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Description
<1> 複数の銀含有ナノ粒子を含む液体組成物を堆積させて基板上に組成物構造体を形成する工程;
前記組成物構造体を加熱して高導電性構造体を形成する工程;ならびに
加熱工程の温度を低下させるために前記組成物構造体に組成物薬剤を付与する工程であって、前記組成物薬剤が、前記堆積工程、前記堆積工程の後であって前記加熱工程より前の工程、および前記加熱工程から選択される工程において付与される、組成物薬剤を付与する工程
を含む、高導電性構造体を形成する方法。
前記組成物構造体を140℃以下の温度で加熱する工程;ならびに
前記組成物構造体に酸性組成物を付与して高導電性構造体を形成する工程であって、前記酸性組成物が、前記堆積工程、前記堆積工程の後であって前記加熱工程より前の工程、および前記加熱工程からなる群から選択される工程において付与される、酸性組成物を付与する工程
を含む、<1>又は<2>に記載の方法。
前記1つまたは複数の組成物構造体を120℃以下の温度でアニールする工程;ならびに
前記1つまたは複数の組成物構造体に酸性組成物を付与して1つまたは複数の高導電性構造体を形成する工程であって、前記酸性組成物が、前記堆積工程、前記堆積工程の後であって前記加熱工程より前の工程、および前記加熱工程からなる群から選択される工程において塗布される、酸性組成物を付与する工程、
を含む、<1>〜<3>のいずれか1つに記載の方法。
前記有機アミンが、ブチルアミン、ペンチルアミン、ヘキシルアミン、ヘプチルアミン、オクチルアミン、ノニルアミン、デシルアミン、ヘキサデシルアミン、ウンデシルアミン、ドデシルアミン、トリデシルアミン、テトラデシルアミン、ジアミノペンタン、ジアミノヘキサン、ジアミノヘプタン、ジアミノオクタン、ジアミノノナン、ジアミノデカン、ジアミノオクタン、ジプロピルアミン、ジブチルアミン、ジペンチルアミン、ジヘキシルアミン、ジヘプチルアミン、ジオクチルアミン、ジノニルアミン、ジデシルアミン、ヘキシルデカンアミン、メチルプロピルアミン、エチルプロピルアミン、プロピルブチルアミン、エチルブチルアミン、エチルペンチルアミン、プロピルペンチルアミン、ブチルペンチルアミン、トリブチルアミン、トリヘキシルアミン、およびこれらの混合物からなる群から選択される、<4>に記載の方法。
前記高導電性構造体の厚さが50nm〜10μmであり、電気伝導率が1,000S/cm超である、高導電性構造体。
対照サンプルおよび本発明の導電性サンプルの両方に、ヘキシルデカンアミンで安定化させた銀含有ナノ粒子を用いた。トルエン溶媒中に15wt%のヘキシルデカンアミン安定化銀含有ナノ粒子が含まれるように対照サンプルの液体組成物を調製し、例示的な基板としての複数のスライドガラス上にスピンコーティングした。塗布した材料をホットプレート上で、それぞれ約110℃、約120℃、または約140℃の各温度で約10分間アニールした。この対照サンプルの形成中では、塗布されたまたはアニールされたサンプルを処理するための組成物薬剤は用いなかった。
本実施例では実施例1のプロセスおよび材料と同じものを用いた。実施例1の液体組成物を複数のスライドガラス上にスピンコーティングし、ホットプレート上で約100℃または約110℃にて約10分間アニールした。アニール中、本発明の組成物薬剤として酢酸を用い、アニールされている膜サンプルの上に空気中で噴霧した。その結果、110℃でアニールした膜サンプルの導電率は約2.37×104S/cmであり、実施例1の対照サンプルよりも107倍を超えて高かった。この方法を用いると、アニール時に例示的酢酸を付与することで、アニール温度が30℃低くなった。
実施例2と比較すると、第2の例示的な酸性組成物である塩酸(HCl)(36.5wt%)を、アニール工程中にホットプレートの側で空中に数滴滴下することで付与(例えば噴霧)した以外は、実施例2と同様にして膜サンプルを得た。得られた膜サンプルは、アニール温度が100℃の場合に約3,970S/cmの導電率を示し、110℃の場合には約5.68×104S/cmの導電率を示した。これは、プロセス温度を約100℃にまで低下させることが可能であることを示している。
実施例3と同様に、HCl蒸気を用いた。実施例3と異なり、堆積させた液体組成物をアニールする前に約1〜2分間HCl蒸気を付与し、その後、アニールプロセスをホットプレート上で約110℃にて約10分間行った。次いで、導電率を測定したところ、約3.5×104S/cmであった。このことは、低いアニール温度を用いて所望の高導電率を得ることができる場合、アニールを実施する前に酸に暴露してもよいことを示している。
本実施例では、実施例1〜4の液体組成物のそれぞれを噴射可能なインクへと配合し、スライドガラス上に印刷して、幅約60μmの線状構造体を含む導電性の微細構造体を形成した。印刷した組成物構造体の上に酢酸を噴霧した。次いで、酸処理された構造体を約110℃で約10分間アニールした。その結果、印刷された線は高導電性になり、酸を塗布しても、印刷された構造体に損傷はなかった。
104 付与工程
106 加熱工程
10 基板
20 液体組成物
24 組成物構造体
30 組成物薬剤
40 導電性構造体
Claims (5)
- 複数の銀含有ナノ粒子を含む液体組成物を堆積させて基板上に組成物構造体を形成する工程;
前記組成物構造体を加熱して高導電性構造体を形成する工程;ならびに
加熱工程の温度を低下させるために前記組成物構造体に組成物薬剤を付与する工程であって、前記組成物薬剤が、前記堆積工程、前記堆積工程の後であって前記加熱工程より前の工程、および前記加熱工程から選択される工程において付与される、組成物薬剤を付与する工程
を含み、前記組成物薬剤が、HClを含む、高導電性構造体を形成する方法。 - 有機アミンで安定化された複数の銀含有ナノ粒子を含む液体組成物を堆積させてフレキシブル基板上に組成物構造体を形成する工程;
前記組成物構造体を140℃以下の温度で加熱する工程;ならびに
前記組成物構造体に酸性組成物を付与して高導電性構造体を形成する工程であって、前記酸性組成物が、前記堆積工程、前記堆積工程の後であって前記加熱工程より前の工程、および前記加熱工程からなる群から選択される工程において付与される、酸性組成物を付与する工程
を含む、請求項1に記載の方法。 - 有機アミンで安定化された複数の銀含有ナノ粒子を含む液体組成物を堆積させて、ポリエチレンテレフタラートを含む基板上に1つまたは複数の組成物構造体を形成する工程;
前記1つまたは複数の組成物構造体を120℃以下の温度でアニールする工程;ならびに
前記1つまたは複数の組成物構造体に酸性組成物を付与して1つまたは複数の高導電性構造体を形成する工程であって、前記酸性組成物が、前記堆積工程、前記堆積工程の後であって前記加熱工程より前の工程、および前記加熱工程からなる群から選択される工程において塗布される、酸性組成物を付与する工程、
を含む、請求項1または請求項2に記載の方法。 - 前記組成物構造体への前記酸性組成物の付与により、前記有機アミンで安定化された複数の銀含有ナノ粒子の有機アミンとのネットワーク、複合体、または塩が形成され、
前記有機アミンが、ブチルアミン、ペンチルアミン、ヘキシルアミン、ヘプチルアミン、オクチルアミン、ノニルアミン、デシルアミン、ヘキサデシルアミン、ウンデシルアミン、ドデシルアミン、トリデシルアミン、テトラデシルアミン、ジアミノペンタン、ジアミノヘキサン、ジアミノヘプタン、ジアミノオクタン、ジアミノノナン、ジアミノデカン、ジアミノオクタン、ジプロピルアミン、ジブチルアミン、ジペンチルアミン、ジヘキシルアミン、ジヘプチルアミン、ジオクチルアミン、ジノニルアミン、ジデシルアミン、ヘキシルデカンアミン、メチルプロピルアミン、エチルプロピルアミン、プロピルブチルアミン、エチルブチルアミン、エチルペンチルアミン、プロピルペンチルアミン、ブチルペンチルアミン、トリブチルアミン、トリヘキシルアミン、およびこれらの混合物からなる群から選択される、請求項3に記載の方法。 - 請求項1〜4のいずれか1項に記載の方法によって形成される高導電性構造体であって、
前記高導電性構造体の厚さが50nm〜10μmであり、電気伝導率が1,000S/cm超である、高導電性構造体。
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WO2013036519A1 (en) | 2011-09-06 | 2013-03-14 | Henkel Corporation | Conductive material and process |
CN103975030A (zh) * | 2011-09-06 | 2014-08-06 | 汉高知识产权控股有限责任公司 | 导电金属和方法 |
JP6099472B2 (ja) * | 2013-04-26 | 2017-03-22 | Dowaエレクトロニクス株式会社 | 金属ナノ粒子分散体、金属ナノ粒子分散体の製造方法および接合方法 |
CN105340370B (zh) * | 2013-07-04 | 2020-03-24 | 爱克发-格法特公司 | 制备导电金属层或图案的方法 |
CN105579533B (zh) | 2013-08-16 | 2020-04-14 | 汉高知识产权控股有限责任公司 | 亚微米银颗粒油墨组合物、方法和用途 |
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CN103928617A (zh) * | 2014-05-06 | 2014-07-16 | 电子科技大学 | 一种高电导率有机薄膜太阳能光伏电池的制备方法 |
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JP2018109232A (ja) * | 2016-12-28 | 2018-07-12 | Dowaエレクトロニクス株式会社 | 接合材及びそれを用いた接合方法 |
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