JP6068406B2 - ナノサイズ銀微粒子インク及び銀微粒子焼結体 - Google Patents
ナノサイズ銀微粒子インク及び銀微粒子焼結体 Download PDFInfo
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- JP6068406B2 JP6068406B2 JP2014179615A JP2014179615A JP6068406B2 JP 6068406 B2 JP6068406 B2 JP 6068406B2 JP 2014179615 A JP2014179615 A JP 2014179615A JP 2014179615 A JP2014179615 A JP 2014179615A JP 6068406 B2 JP6068406 B2 JP 6068406B2
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- 229910052709 silver Inorganic materials 0.000 title claims description 151
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims description 149
- 239000004332 silver Substances 0.000 title claims description 149
- 239000010419 fine particle Substances 0.000 title claims description 89
- 239000002105 nanoparticle Substances 0.000 title claims description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 22
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 22
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 22
- 239000005642 Oleic acid Substances 0.000 claims description 22
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 22
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 22
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 22
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 claims description 22
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 18
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 17
- 239000003960 organic solvent Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 13
- 239000000758 substrate Substances 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 11
- 238000004528 spin coating Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 238000004817 gas chromatography Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 2
- 238000002360 preparation method Methods 0.000 claims 1
- 239000000976 ink Substances 0.000 description 62
- 239000010408 film Substances 0.000 description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 30
- 150000003973 alkyl amines Chemical class 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 15
- IUNMPGNGSSIWFP-UHFFFAOYSA-N dimethylaminopropylamine Chemical compound CN(C)CCCN IUNMPGNGSSIWFP-UHFFFAOYSA-N 0.000 description 11
- 239000003223 protective agent Substances 0.000 description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 10
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 10
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 10
- 238000004898 kneading Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 239000010944 silver (metal) Substances 0.000 description 6
- 239000011882 ultra-fine particle Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229920002799 BoPET Polymers 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 229940100890 silver compound Drugs 0.000 description 4
- 150000003379 silver compounds Chemical class 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- -1 oxalate ions Chemical class 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 150000003378 silver Chemical group 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 125000003438 dodecyl group Chemical group [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])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical compound O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Conductive Materials (AREA)
- Manufacturing Of Electric Cables (AREA)
Description
以下、本発明の実施例を具体的に説明する。
表1に実験例1〜15を示す。また比較例1〜8を表2に示す。
昇温条件:80℃(保持5min)〜200℃(保持20min)、昇温20℃/min注入口温度:200℃、スプリット方式(20:1)
検出器温度:210℃、FID(水素炎イオン検出器)
キャリアガス:ヘリウム 160kPa
注入量:1μL
カラム温度:250℃
注入口温度:250℃、スプリット方式(20:1)
検出器温度:230℃、FID(水素炎イオン検出器)
キャリアガス:ヘリウム 160kPa
注入量:1μL
Claims (7)
- 銀微粒子を溶媒により分散してなるナノサイズ銀微粒子インクであって、30〜200wt%の有機溶剤により湿潤されたシュウ酸銀を銀材料とした銀微粒子を前記溶媒に1wt%以上、50wt%以下になるように溶解し、ナノサイズ銀微粒子インクをFIDのキャピラリーカラムを持つガスクロマトグラフィーで分析し、少なくともヘキシルアミン、ドデシルアミン及びオレイン酸を含み、ヘキシルアミン対ドデシルアミンのモル比は、3:1〜60:1であり、オレイン酸量が銀質量に対して0.02mmol/g以上0.30mmol/g以下であり、スピンコートで基板に塗布して形成した銀膜を、室温で5分間乾燥後、100℃で焼結させた焼結体の体積抵抗率が8μΩ・cm以上25μΩ・cm以下であることを特徴とするナノサイズ銀微粒子インク。
- 請求項1において、
前記溶媒は、アルカン類とアルコール類の少なくとも2種類以上を含んでなり、アルカン類とアルコール類の混合比率が2:1から4:1であることを特徴とするナノサイズ銀微粒子インク。 - 請求項1において、
前記銀粒子が平均粒径10nm以上15nm以下であることを特徴とするナノサイズ銀微粒子インク。 - 請求項1乃至3のいずれかにおいて、
常温常圧で保管した際、作製から1ヶ月経過したとき、銀沈殿が目視により、確認されないナノサイズ銀微粒子インク。 - 請求項1乃至4のいずれかにおいて、
基板に塗布して形成した銀膜を、室温で5分間乾燥後、100℃で焼結させた際、12μΩ・cm以下の体積抵抗になるナノサイズ銀微粒子インク。 - 請求項1乃至5のいずれかにおいて、
基板に塗布して形成した銀膜を、室温で5分間乾燥後、100℃で焼結させた際、焼結して形成された銀微粒子焼結体の表面が鏡面となるナノサイズ銀微粒子インク。 - 請求項1乃至6のいずれかのナノサイズ銀微粒子インクを塗布し、その後100℃で焼結してなり、表面が鏡面である銀微粒子焼結体。
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JP2014179615A JP6068406B2 (ja) | 2014-09-03 | 2014-09-03 | ナノサイズ銀微粒子インク及び銀微粒子焼結体 |
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JP2014179615A JP6068406B2 (ja) | 2014-09-03 | 2014-09-03 | ナノサイズ銀微粒子インク及び銀微粒子焼結体 |
Related Parent Applications (1)
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JP2012175456A Division JP5647650B2 (ja) | 2012-08-07 | 2012-08-07 | 銀微粒子インクの製造方法 |
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JP2015017264A JP2015017264A (ja) | 2015-01-29 |
JP6068406B2 true JP6068406B2 (ja) | 2017-01-25 |
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Cited By (2)
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KR20210028030A (ko) * | 2019-09-03 | 2021-03-11 | 김승용 | 능동형 환풍기 제어 장치 및 방법 |
KR20210029239A (ko) | 2018-08-30 | 2021-03-15 | 다나카 기킨조쿠 고교 가부시키가이샤 | 저온 소성용의 은 잉크 |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
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GB2535214A (en) | 2015-02-13 | 2016-08-17 | Dst Innovation Ltd | Printable conductive ink and method of forming transparent printed electrodes |
JP6528270B2 (ja) * | 2015-03-31 | 2019-06-12 | トッパン・フォームズ株式会社 | 金属インク組成物及び配線板 |
Family Cites Families (2)
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JP5574761B2 (ja) * | 2009-04-17 | 2014-08-20 | 国立大学法人山形大学 | 被覆銀超微粒子とその製造方法 |
JP5791146B2 (ja) * | 2010-08-03 | 2015-10-07 | バンドー化学株式会社 | コロイド分散液 |
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Cited By (3)
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KR20210029239A (ko) | 2018-08-30 | 2021-03-15 | 다나카 기킨조쿠 고교 가부시키가이샤 | 저온 소성용의 은 잉크 |
KR20210028030A (ko) * | 2019-09-03 | 2021-03-11 | 김승용 | 능동형 환풍기 제어 장치 및 방법 |
KR102279567B1 (ko) * | 2019-09-03 | 2021-07-20 | 김승덕 | 능동형 환풍기 제어 장치 및 방법 |
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