JP6949755B2 - 銀ナノ粒子複合体の製造方法及び銀ナノ粒子複合体、並びに、導電性インク及び導電膜の形成方法 - Google Patents
銀ナノ粒子複合体の製造方法及び銀ナノ粒子複合体、並びに、導電性インク及び導電膜の形成方法 Download PDFInfo
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- JP6949755B2 JP6949755B2 JP2018029066A JP2018029066A JP6949755B2 JP 6949755 B2 JP6949755 B2 JP 6949755B2 JP 2018029066 A JP2018029066 A JP 2018029066A JP 2018029066 A JP2018029066 A JP 2018029066A JP 6949755 B2 JP6949755 B2 JP 6949755B2
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- nanoparticle composite
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- carbon nanotubes
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims description 41
- 239000004332 silver Substances 0.000 title claims description 41
- 239000002105 nanoparticle Substances 0.000 title claims description 39
- 239000002131 composite material Substances 0.000 title claims description 37
- 238000000034 method Methods 0.000 title claims description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 59
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 57
- 239000002041 carbon nanotube Substances 0.000 claims description 55
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 55
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 44
- 239000003638 chemical reducing agent Substances 0.000 claims description 43
- 125000000524 functional group Chemical group 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 29
- -1 gallic acid ester Chemical class 0.000 claims description 23
- 239000006185 dispersion Substances 0.000 claims description 22
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 22
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- WXTMDXOMEHJXQO-UHFFFAOYSA-N 2,5-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC(O)=CC=C1O WXTMDXOMEHJXQO-UHFFFAOYSA-N 0.000 claims description 15
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
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- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 8
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- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
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- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims description 4
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
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- SZNYYWIUQFZLLT-UHFFFAOYSA-N 2-methyl-1-(2-methylpropoxy)propane Chemical compound CC(C)COCC(C)C SZNYYWIUQFZLLT-UHFFFAOYSA-N 0.000 description 2
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- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
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- 150000001298 alcohols Chemical class 0.000 description 2
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
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- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 description 1
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- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- RRQYJINTUHWNHW-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxyethoxy)ethane Chemical compound CCOCCOCCOCC RRQYJINTUHWNHW-UHFFFAOYSA-N 0.000 description 1
- KIAMPLQEZAMORJ-UHFFFAOYSA-N 1-ethoxy-2-[2-(2-ethoxyethoxy)ethoxy]ethane Chemical compound CCOCCOCCOCCOCC KIAMPLQEZAMORJ-UHFFFAOYSA-N 0.000 description 1
- HFZLSTDPRQSZCQ-UHFFFAOYSA-N 1-pyrrolidin-3-ylpyrrolidine Chemical compound C1CCCN1C1CNCC1 HFZLSTDPRQSZCQ-UHFFFAOYSA-N 0.000 description 1
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- YQUVCSBJEUQKSH-UHFFFAOYSA-M 3,4-dihydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1O YQUVCSBJEUQKSH-UHFFFAOYSA-M 0.000 description 1
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- LEVWYRKDKASIDU-QWWZWVQMSA-N D-cystine Chemical compound OC(=O)[C@H](N)CSSC[C@@H](N)C(O)=O LEVWYRKDKASIDU-QWWZWVQMSA-N 0.000 description 1
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- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 description 1
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 1
- ZDXPYRJPNDTMRX-VKHMYHEASA-N L-glutamine Chemical compound OC(=O)[C@@H](N)CCC(N)=O ZDXPYRJPNDTMRX-VKHMYHEASA-N 0.000 description 1
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- GHDIHPNJQVDFBL-UHFFFAOYSA-N methoxycyclohexane Chemical compound COC1CCCCC1 GHDIHPNJQVDFBL-UHFFFAOYSA-N 0.000 description 1
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- Non-Insulated Conductors (AREA)
- Carbon And Carbon Compounds (AREA)
- Conductive Materials (AREA)
Description
(A)表面に官能基が導入されたカーボンナノチューブを含む水溶液を用意する工程と、
(B)上記水溶液に、硝酸銀と、該硝酸銀を還元する還元剤とを混合する工程と
を含む。
カーボンナノチューブを、硝酸水溶液中で熱還流処理して、官能基化されたカーボンナノチューブを作製した。作製したカーボンナノチューブ0.02gを、蒸留水20mlに入れ、室温で10分間攪拌した。この溶液に、硝酸銀0.5gを添加、攪拌した後、ジメチルアミノエタノール0.262gをさらに添加した。この溶液に、没食子酸一水和物0.276gを蒸留水30mlに溶解した溶液を、室温で30分間滴下した。その後、さらに、1時間攪拌した。
カーボンナノチューブとリシンとを水溶液中で混合することによって、官能基化されたカーボンナノチューブを作製した。作製したカーボンナノチューブ0.04gを、蒸留水20mlに入れ、室温で10分間攪拌した。この溶液に、硝酸銀0.5gを添加、攪拌した後、ジメチルアミノエタノール0.262gをさらに添加した。この溶液に、没食子酸一水和物0.276gを蒸留水30mlに溶解した溶液を、室温で30分間滴下した。その後、さらに、1時間攪拌した。
Claims (8)
- (A)表面に官能基が導入されたカーボンナノチューブを含む水溶液を用意する工程と、
(B)前記水溶液に、硝酸銀と、該硝酸銀を還元する還元剤とを混合する工程と
を含み、
前記官能基は、少なくともカルボキシル基、アミノ基の何れか一つを含み、
前記還元剤は、没食子酸、没食子酸塩、没食子酸エステル、ジヒドロキシ安息香酸、ジヒドロキシ安息香酸塩、及びジヒドロキシ安息香酸エステルからなる群から選択された化合物からなり、
前記工程(B)において、前記硝酸銀が前記還元剤で還元されると同時に、還元生成された銀ナノ粒子が、前記カーボンナノチューブの表面に導入された官能基と結合することにより、前記還元剤で還元された銀ナノ粒子が、前記カーボンナノチューブの表面に分散された構造を有する銀ナノ粒子複合体が形成される、銀ナノ粒子複合体の製造方法。 - 前記工程(B)において、前記銀ナノ粒子は、前記還元剤からなる膜で被覆された状態で、前記カーボンナノチューブの表面に導入された官能基と結合している、請求項1に記載の銀ナノ粒子複合体の製造方法。
- 前記工程(A)は、前記カーボンナノチューブと、親水性アミノ酸とを水溶液中で混合することにより、表面に官能基が導入されたカーボンナノチューブの水溶液が用意される、請求項1に記載の銀ナノ粒子複合体の製造方法。
- 前記工程(B)において、前記水溶液に、アミン化合物がさらに含まれている、請求項1に記載の銀ナノ粒子複合体の製造方法。
- 銀ナノ粒子が、カーボンナノチューブの表面に分散された構造を有する銀ナノ粒子複合体であって、
前記カーボンナノチューブの表面に、少なくともカルボキシル基、アミノ基の何れか一つを含む官能基が導入されており、
前記銀ナノ粒子は、没食子酸、没食子酸塩、没食子酸エステル、ジヒドロキシ安息香酸、ジヒドロキシ安息香酸塩、及びジヒドロキシ安息香酸エステルからなる群から選択された化合物からなる膜で被覆された状態で、前記カーボンナノチューブの表面に導入された官能基と結合している、銀ナノ粒子複合体。 - 請求項5に記載の銀ナノ粒子複合体が、分散溶液に分散された導電性インク。
- 前記分散溶液は、イソプロピルアルコール、エタノール、1−プロパノール、2−プロパノール、ブタノール、PMA(プロピレングリコールモノメチルエーテルアセテート)、NMP(N-メチルピロリドン)、γブチロラクトン、PGME(プロピレングリコールモノメチルエーテル)、トリエチレングリコールモノブチルーエーテル、ポリエチレングリコールモノブチルエーテル、及びその異性体からなる群から選択される、請求項6に記載の導電性インク。
- 請求項6または7に記載の導電性インクを、基材上に塗布する工程と、
前記基材上に塗布された前記導電性インクの分散溶液を蒸発させる工程と
を含む、導電膜の形成方法。
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