JP4149364B2 - デンドライト状微粒銀粉及びその製造方法 - Google Patents
デンドライト状微粒銀粉及びその製造方法 Download PDFInfo
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- JP4149364B2 JP4149364B2 JP2003388584A JP2003388584A JP4149364B2 JP 4149364 B2 JP4149364 B2 JP 4149364B2 JP 2003388584 A JP2003388584 A JP 2003388584A JP 2003388584 A JP2003388584 A JP 2003388584A JP 4149364 B2 JP4149364 B2 JP 4149364B2
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- silver powder
- dendritic
- silver
- powder
- fine
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims description 86
- 239000010946 fine silver Substances 0.000 title claims description 41
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 66
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 33
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 33
- 239000003638 chemical reducing agent Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 229960005070 ascorbic acid Drugs 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229910052709 silver Inorganic materials 0.000 claims description 9
- 239000004332 silver Substances 0.000 claims description 9
- 239000002211 L-ascorbic acid Substances 0.000 claims description 8
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 8
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 claims description 5
- 235000010350 erythorbic acid Nutrition 0.000 claims description 5
- 229940026239 isoascorbic acid Drugs 0.000 claims description 5
- 238000000691 measurement method Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 26
- 239000000843 powder Substances 0.000 description 20
- 239000007864 aqueous solution Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 238000000034 method Methods 0.000 description 14
- 238000001000 micrograph Methods 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 235000010323 ascorbic acid Nutrition 0.000 description 6
- 239000011668 ascorbic acid Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 5
- 238000005868 electrolysis reaction Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 210000001787 dendrite Anatomy 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- OGFYIDCVDSATDC-UHFFFAOYSA-N silver silver Chemical compound [Ag].[Ag] OGFYIDCVDSATDC-UHFFFAOYSA-N 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Non-Insulated Conductors (AREA)
Description
本件発明にかかる微粒銀粉は、実質的に粉粒がデンドライト状である。
上述したデンドライト状微粒銀粉は、硝酸銀溶液と還元剤とを反応させ製造するものであるが、この反応時の還元剤を反応に必要な理論量以上に過剰に添加するという点に特徴を有しているのである。
[比較例1]
[比較例2]
[比較例3]
そして、上記硝酸銀溶液を撹拌しつつ、そこにアスコルビン酸水溶液を一括で添加して3分間撹拌を行い、撹拌を止めると静置して、生成した微粒銀粉を沈殿させた。
以上に述べてきた実施例と比較例とを対比すると、以下のようなことが分かるのである。
Claims (2)
- デンドライト状の銀粉であり、
当該粉粒の持つレーザー回折散乱式粒度分布測定法によるD10が3.0μm以下、D50が12.0μm以下、D90が18.0μm以下、Dmaxが44.0μm以下であることを特徴とするデンドライト状微粒銀粉。 - 硝酸銀溶液と還元剤とを反応させ請求項1に記載のデンドライト状微粒銀粉を製造する方法であって、
硝酸銀溶液と還元剤とを反応させる際の反応溶液の硝酸銀濃度が10g/l〜90g/lであり、
還元剤は、L−アスコルビン酸、イソアスコルビン酸のいずれか一種若しくは二種であり、
前記硝酸銀溶液に含まれる1当量の銀あたり、還元剤が3当量以上となるように添加して攪拌しつつ反応させ、濾過し、洗浄し、乾燥することによりデンドライト状微粒銀粉を得ることを特徴としたデンドライト状微粒銀粉の製造方法。
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JP2003388584A JP4149364B2 (ja) | 2003-11-18 | 2003-11-18 | デンドライト状微粒銀粉及びその製造方法 |
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JP2003388584A JP4149364B2 (ja) | 2003-11-18 | 2003-11-18 | デンドライト状微粒銀粉及びその製造方法 |
Publications (2)
Publication Number | Publication Date |
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JP2005146387A JP2005146387A (ja) | 2005-06-09 |
JP4149364B2 true JP4149364B2 (ja) | 2008-09-10 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103260795A (zh) * | 2010-11-08 | 2013-08-21 | 纳美仕有限公司 | 金属粒子及其制造方法 |
Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
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KR101846474B1 (ko) * | 2011-05-31 | 2018-04-06 | 토요잉크Sc홀딩스주식회사 | 도전성 시트 및 그 제조 방법, 및 전자 부품 |
JP5320442B2 (ja) * | 2011-07-13 | 2013-10-23 | 三井金属鉱業株式会社 | デンドライト状銅粉 |
JP5631910B2 (ja) * | 2011-10-21 | 2014-11-26 | 三井金属鉱業株式会社 | 銀被覆銅粉 |
CN104819975A (zh) * | 2015-05-21 | 2015-08-05 | 中北大学 | 滤纸基树枝状银表面增强拉曼散射活性基底及其制备方法 |
US10357824B2 (en) | 2015-12-03 | 2019-07-23 | Mitsui Mining & Smelting Co., Ltd. | Dendritic silver powder |
CN109773210A (zh) * | 2019-03-01 | 2019-05-21 | 天津工业大学 | 一种具有细长大花瓣的花朵状微米银粉的制备方法 |
CN110935888B (zh) * | 2019-11-01 | 2022-07-01 | 武汉船用电力推进装置研究所(中国船舶重工集团公司第七一二研究所) | 一种树枝状银粉的制备方法 |
EP4227026A4 (en) * | 2020-10-05 | 2024-03-06 | Mitsui Mining & Smelting Co., Ltd. | SILVER POWDER, PRODUCTION METHOD THEREFOR, AND CONDUCTIVE RESIN COMPOSITION |
CN112536445A (zh) * | 2020-12-10 | 2021-03-23 | 长沙新材料产业研究院有限公司 | 一种微纳米树枝状银粉及其制备方法和应用 |
CN115055692B (zh) * | 2022-07-06 | 2023-09-26 | 江西理工大学南昌校区 | 气溶胶喷涂工艺用电子级微纳米树枝状银颗粒的合成方法 |
CN116721795A (zh) * | 2023-03-02 | 2023-09-08 | 苏州星翰新材料科技有限公司 | 使用高导电片状微米级银粉制备光伏电池用银浆的方法 |
CN117600482B (zh) * | 2024-01-23 | 2024-05-28 | 长春黄金研究院有限公司 | 高振实密度片状银粉的制备方法 |
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- 2003-11-18 JP JP2003388584A patent/JP4149364B2/ja not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103260795A (zh) * | 2010-11-08 | 2013-08-21 | 纳美仕有限公司 | 金属粒子及其制造方法 |
CN103260795B (zh) * | 2010-11-08 | 2015-10-07 | 纳美仕有限公司 | 金属粒子及其制造方法 |
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