JP2017082327A - 銀粉およびその製造方法 - Google Patents
銀粉およびその製造方法 Download PDFInfo
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- JP2017082327A JP2017082327A JP2016204799A JP2016204799A JP2017082327A JP 2017082327 A JP2017082327 A JP 2017082327A JP 2016204799 A JP2016204799 A JP 2016204799A JP 2016204799 A JP2016204799 A JP 2016204799A JP 2017082327 A JP2017082327 A JP 2017082327A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 61
- 229910052709 silver Inorganic materials 0.000 claims abstract description 27
- 239000004332 silver Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 230000001186 cumulative effect Effects 0.000 description 29
- 238000000034 method Methods 0.000 description 12
- 238000009826 distribution Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000011362 coarse particle Substances 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000009692 water atomization Methods 0.000 description 2
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 241000892865 Heros Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- -1 dried and crushed Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
- B22F2009/0828—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid with water
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- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
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- B22F2304/00—Physical aspects of the powder
- B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
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Abstract
【解決手段】銀の融点(962℃)より330〜730℃高い温度(1292〜1692℃)に加熱した銀溶湯を落下させながら(好ましくは水圧90〜160MPaで)高圧水を吹き付けて急冷凝固させることによって銀を粉末化することにより、平均粒径が1〜6μm、500℃における収縮率が8%以下(好ましくは7%以下)であり、平均粒径と500℃における収縮率の積が1〜11μm・%(好ましくは1.5〜10.5μm・%)である銀粉を製造する。
【選択図】図1
Description
銀12kgを1600℃(銀の融点(962℃)より638℃高い温度)に加熱して溶解した溶湯をタンディッシュ下部から落下させながら、水圧150MPa、水量160L/分で高圧水を吹き付けて急冷凝固させ、得られた粉末をろ過し、水洗し、乾燥し、解砕し、風力分級機(株式会社セイシン企業製のクラッシールN−01型)により粗大粒子を除去して、銀粉を得た。
風力分級機により粗大粒子を除去する際に10μmより大きい銀の凝集体を除去することにより粒度を調整した以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。
加熱温度を1400℃とし、水圧を100MPaとした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。
加熱温度を1400℃とし、水圧を70MPaとした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。
加熱温度を1500℃とした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。
加熱温度を1250℃とし、水圧を150MPaとした以外は、実施例1と同様の方法により、得られた銀粉について、粒度分布、収縮率、結晶子径、BET比表面積、タップ密度、炭素含有量を求めた。
銀54kgを含む硝酸銀水溶液4500kgに、25質量%のアンモニア水203kgを添加して、銀アンミン錯塩水溶液を得た。この銀アンミン錯塩水溶液の液温を40℃とし、37質量%のホルマリン水溶液240kgを添加して銀粒子を析出させて銀含有スラリーを得た。この銀含有スラリー中に、銀に対して0.2質量%のステアリン酸を含むステアリン酸エマルジョンを添加した後、濾過し、水洗し、ケーキ15.0kgを得た。このケーキを乾燥機に投入し、乾燥粉13.6kgを得た。この乾燥粉を解砕した後、分級して10μmより大きい銀の凝集体を除去した。
Claims (6)
- 銀の融点より330〜730℃高い温度に加熱した銀溶湯を落下させながら高圧水を吹き付けて急冷凝固させることによって銀を粉末化することを特徴とする、銀粉の製造方法。
- 前記高圧水が水圧90〜160MPaで吹き付けられることを特徴とする、請求項1に記載の銀粉の製造方法。
- 平均粒径が1〜6μm、500℃における収縮率が8%以下であり、平均粒径と500℃における収縮率の積が1〜11μm・%であることを特徴とする、銀粉。
- BET比表面積(m2/g)×タップ密度(g/m3)/結晶子径(m)の値が1×1013〜6×1013(m−2)であることを特徴とする、請求項3に記載の銀粉。
- 炭素含有量が0.1質量%以下であることを特徴とする、請求項3または4に記載の銀粉。
- 溶剤および樹脂を含み、導電性粉体として請求項3乃至5のいずれかに記載の銀粉を含むことを特徴とする、導電性ペースト。
Priority Applications (8)
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TW105134429A TWI734710B (zh) | 2015-10-30 | 2016-10-25 | 銀粉及其製造方法 |
SG11201802822PA SG11201802822PA (en) | 2015-10-30 | 2016-10-26 | Silver powder and method for producing same |
PCT/JP2016/004706 WO2017073057A1 (ja) | 2015-10-30 | 2016-10-26 | 銀粉およびその製造方法 |
CN201680063241.8A CN108349009A (zh) | 2015-10-30 | 2016-10-26 | 银粉及其制造方法 |
US15/768,065 US10828702B2 (en) | 2015-10-30 | 2016-10-26 | Silver powder and method for producing same |
KR1020187014652A KR102446788B1 (ko) | 2015-10-30 | 2016-10-26 | 은 분말 및 그 제조 방법 |
EP16859295.4A EP3357608B1 (en) | 2015-10-30 | 2016-10-26 | Method for producing a silver powder |
US17/086,552 US11407030B2 (en) | 2015-10-30 | 2020-11-02 | Silver powder and method for producing same |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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KR20200062263A (ko) * | 2017-09-29 | 2020-06-03 | 도와 일렉트로닉스 가부시키가이샤 | 은 분말 및 그의 제조 방법 |
JP2021004410A (ja) * | 2019-06-27 | 2021-01-14 | Dowaエレクトロニクス株式会社 | 銀粉およびその製造方法 |
JPWO2020137330A1 (ja) * | 2018-12-26 | 2021-11-11 | 昭栄化学工業株式会社 | 銀ペースト |
JPWO2020137329A1 (ja) * | 2018-12-26 | 2021-11-18 | 昭栄化学工業株式会社 | 銀ペースト |
JPWO2020137331A1 (ja) * | 2018-12-26 | 2021-11-18 | 昭栄化学工業株式会社 | 銀ペースト |
Families Citing this family (1)
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KR102263618B1 (ko) * | 2019-03-29 | 2021-06-10 | 대주전자재료 주식회사 | 혼합 은 분말 및 이를 포함하는 도전성 페이스트 |
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US20210078081A1 (en) | 2021-03-18 |
JP7110421B2 (ja) | 2022-08-01 |
EP3357608A1 (en) | 2018-08-08 |
CN108349009A (zh) | 2018-07-31 |
SG11201802822PA (en) | 2018-05-30 |
KR102446788B1 (ko) | 2022-09-22 |
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US11407030B2 (en) | 2022-08-09 |
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