JP2010255037A - 銀ナノワイヤーの連続的製造方法 - Google Patents
銀ナノワイヤーの連続的製造方法 Download PDFInfo
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- JP2010255037A JP2010255037A JP2009105477A JP2009105477A JP2010255037A JP 2010255037 A JP2010255037 A JP 2010255037A JP 2009105477 A JP2009105477 A JP 2009105477A JP 2009105477 A JP2009105477 A JP 2009105477A JP 2010255037 A JP2010255037 A JP 2010255037A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 55
- 239000000243 solution Substances 0.000 claims abstract description 101
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 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 claims abstract description 36
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003223 protective agent Substances 0.000 claims abstract description 27
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 26
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 26
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 26
- 230000032683 aging Effects 0.000 claims abstract description 24
- 239000012266 salt solution Substances 0.000 claims description 28
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 14
- 239000002070 nanowire Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005342 ion exchange Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 150000002334 glycols Chemical class 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 abstract description 16
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 abstract description 13
- 230000000717 retained effect Effects 0.000 abstract 2
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- -1 silver ions Chemical class 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000011437 continuous method Methods 0.000 description 2
- 239000011258 core-shell material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000523 polyvinylpolypyrrolidone Polymers 0.000 description 1
- 235000013809 polyvinylpolypyrrolidone Nutrition 0.000 description 1
- 239000001253 polyvinylpolypyrrolidone Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
【解決手段】グリコール溶液を反応タンクおよび時効処理タンクに供給して加熱する。この反応タンク内に銀塩のグリコール溶液、保護剤ポリビニルピロリドンのグリコール溶液を連続的に供給し、その混合溶液を、所定の温度、時間反応させ銀ナノ粒子を得る。銀ナノ粒子を含む反応溶液を時効処理タンクに送り所定時間滞留させ、銀ナノ粒子の一次元成長を安定に維持し、銀ナノワイヤーを形成する。
【選択図】なし
Description
Claims (20)
- 下記工程を含む、銀ナノワイヤーの連続的製造方法。
第一の溶液を反応タンク内及び時効処理タンク内に供給し、前記反応タンク及び前記時効処理タンク内で、前記第一の溶液を第一の温度範囲まで加熱する工程;
銀−塩溶液及び保護剤溶液を、ある比率に従って前記反応タンク内へ連続的に供給し
第二の温度範囲で前記銀−塩溶液及び前記保護剤溶液をお互いに混合し、第一の滞留時間、反応タンク内に滞留させ、第二の溶液を形成する工程:
前記第二の溶液を前記時効処理タンク内に供給し、前記第二の溶液を、第二の滞留時間、前記時効処理タンク内に滞留させ、第三の溶液を形成する工程;及び
前記第三の溶液を精製し、少なくとも1本の銀ナノワイヤーを得る工程。 - 前記第一の溶液がグリコール溶液である、請求項1記載の方法。
- 前記銀−塩溶液が、水溶性銀塩を第一の溶媒に溶解することにより生成される、請求項1記載の方法。
- 前記銀−塩溶液が、硝酸銀を第一の溶媒に溶解することにより生成される、請求項3記載の方法。
- 前記銀−塩溶液が、酢酸銀又は硝酸銀を前記第一の溶媒に溶解することにより生成される、請求項3記載の方法。
- 銀−塩溶液の水溶性銀塩の濃度が0.5重量%より高い、請求項3記載の方法。
- 前記保護剤溶液が、ポリビニルピロリドンを第二の溶媒に溶解することにより生成される、請求項4記載の方法。
- 前記第一の溶媒及び第二の溶媒がグリコールである、請求項7記載の方法。
- 前記第三の溶液を精製する工程が下記工程を含む、請求項8記載の方法。
過剰のアセトンを前記第三の溶液に供給し、前記第三の溶液を前記グリコールと混合し、透明な液状部分及び沈殿部分を形成する工程;
前記透明な液状部分を除去し、前記沈殿部分を熱水に溶解し、第四の溶液を形成する工程;
前記第四の溶液をイオン交換処理により処理し、第五の溶液を形成する工程;
前記第五の溶液を、複数回繰り返して加熱、撹拌及び固液分離して第六の溶液を得る工程;及び
前記第六の溶液を噴霧乾燥して前記第六の溶液の水を除去し、少なくとも1本のナノワイヤーの粉末を得る工程。 - 前記第三の溶液に対する前記アセトンの容量比が2〜6を含む、請求項9記載の方法。
- 前記銀−塩溶液及び前記保護剤溶液が前記反応タンク内に供給される場合、前記硝酸銀に対する前記ポリビニルピロリドンの重量比が0.5〜6を含む、請求項7記載の方法。
- 前記保護剤溶液のポリビニルピロリドンの分子量が5000〜360000を含む、請求項7記載の方法。
- 前記銀−塩溶液及び前記保護剤溶液が、連続供給により前記反応タンク内に供給される、請求項1記載の方法
- 前記第一の温度範囲が170℃〜180℃を含む、請求項1記載の方法。
- 前記第二の温度範囲が140℃〜180℃を含む、請求項1記載の方法。
- 前記第二の温度範囲が150℃〜170℃を含む、請求項15記載の方法。
- 前記第一の滞留時間が10分〜30分を含む、請求項1記載の方法。
- 前記第二の滞留時間が30分を含む、請求項1記載の方法。
- 前記第一の温度範囲が、マイクロ波加熱により供給される、請求項1記載の方法。
- 前記第二の温度範囲が、マイクロ波加熱により供給される、請求項1記載の方法。
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Cited By (14)
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CN102211205A (zh) * | 2011-05-18 | 2011-10-12 | 山东大学 | 一种制备系列高纯度银纳米材料的方法 |
WO2012094072A1 (en) * | 2011-01-04 | 2012-07-12 | Carestream Health, Inc. | Nanowire recovery methods, compositions, and articles |
WO2012112239A1 (en) | 2011-02-15 | 2012-08-23 | Carestream Health, Inc. | Nanowire preparation methods, compositions, and articles |
JP2013007082A (ja) * | 2011-06-23 | 2013-01-10 | Nippon Steel & Sumikin Chemical Co Ltd | 金属ナノ粒子の連続製造装置及び連続製造方法 |
CN103084584A (zh) * | 2013-01-29 | 2013-05-08 | 中国科学院理化技术研究所 | 一种利用水热法制备银纳米线的方法 |
CN103357889A (zh) * | 2013-07-15 | 2013-10-23 | 中南大学 | 一种高长宽比银纳米线的制备方法及应用 |
KR101327074B1 (ko) | 2011-07-29 | 2013-11-07 | 주식회사 나노픽시스 | 나노 와이어 및 이의 제조 방법 |
KR101326952B1 (ko) | 2011-07-29 | 2013-11-13 | 주식회사 나노픽시스 | 나노 와이어 및 이의 제조방법 |
WO2013191337A1 (ko) * | 2012-06-20 | 2013-12-27 | 한국과학기술원 | 은 나노와이어의 제조방법 |
CN105537622A (zh) * | 2016-01-07 | 2016-05-04 | 嘉兴禾浦光电科技有限公司 | 一种制备银纳米线的方法 |
CN106541146A (zh) * | 2016-10-28 | 2017-03-29 | 中国科学院宁波材料技术与工程研究所 | 一种超长银纳米线的制备方法 |
US9956616B2 (en) | 2011-07-29 | 2018-05-01 | Lg Innotek Co., Ltd. | Nano-wire and method for manufacturing the same |
CN113510239A (zh) * | 2021-07-07 | 2021-10-19 | 黄河科技学院 | 一种基于银包覆的金纳米棒、其制备方法及应用 |
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KR101465467B1 (ko) * | 2013-09-13 | 2014-11-27 | 영남대학교 산학협력단 | 마이크로웨이브를 이용한 금속 나노와이어의 제조방법 및 그로부터 제조된 금속 나노와이어 |
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WO2012094072A1 (en) * | 2011-01-04 | 2012-07-12 | Carestream Health, Inc. | Nanowire recovery methods, compositions, and articles |
US8696947B2 (en) | 2011-01-04 | 2014-04-15 | Carestream Health, Inc. | Nanowire recovery methods, compositions, and articles |
JP2014511435A (ja) * | 2011-02-15 | 2014-05-15 | ケアストリーム ヘルス インク | ナノワイヤ調製方法、組成物、および物品 |
WO2012112239A1 (en) | 2011-02-15 | 2012-08-23 | Carestream Health, Inc. | Nanowire preparation methods, compositions, and articles |
CN102211205A (zh) * | 2011-05-18 | 2011-10-12 | 山东大学 | 一种制备系列高纯度银纳米材料的方法 |
JP2013007082A (ja) * | 2011-06-23 | 2013-01-10 | Nippon Steel & Sumikin Chemical Co Ltd | 金属ナノ粒子の連続製造装置及び連続製造方法 |
US9956616B2 (en) | 2011-07-29 | 2018-05-01 | Lg Innotek Co., Ltd. | Nano-wire and method for manufacturing the same |
KR101327074B1 (ko) | 2011-07-29 | 2013-11-07 | 주식회사 나노픽시스 | 나노 와이어 및 이의 제조 방법 |
KR101326952B1 (ko) | 2011-07-29 | 2013-11-13 | 주식회사 나노픽시스 | 나노 와이어 및 이의 제조방법 |
WO2013191337A1 (ko) * | 2012-06-20 | 2013-12-27 | 한국과학기술원 | 은 나노와이어의 제조방법 |
CN103084584A (zh) * | 2013-01-29 | 2013-05-08 | 中国科学院理化技术研究所 | 一种利用水热法制备银纳米线的方法 |
CN103357889A (zh) * | 2013-07-15 | 2013-10-23 | 中南大学 | 一种高长宽比银纳米线的制备方法及应用 |
CN105537622A (zh) * | 2016-01-07 | 2016-05-04 | 嘉兴禾浦光电科技有限公司 | 一种制备银纳米线的方法 |
CN106541146A (zh) * | 2016-10-28 | 2017-03-29 | 中国科学院宁波材料技术与工程研究所 | 一种超长银纳米线的制备方法 |
CN113510239A (zh) * | 2021-07-07 | 2021-10-19 | 黄河科技学院 | 一种基于银包覆的金纳米棒、其制备方法及应用 |
CN113510239B (zh) * | 2021-07-07 | 2022-12-09 | 黄河科技学院 | 一种基于银包覆的金纳米棒、其制备方法及应用 |
CN113649558A (zh) * | 2021-07-08 | 2021-11-16 | 山东建邦胶体材料有限公司 | 一种纳米银线及其制备方法 |
CN113649558B (zh) * | 2021-07-08 | 2023-03-10 | 山东建邦胶体材料有限公司 | 一种纳米银线及其制备方法 |
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