JP2019065386A - 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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- JP2019065386A JP2019065386A JP2018162411A JP2018162411A JP2019065386A JP 2019065386 A JP2019065386 A JP 2019065386A JP 2018162411 A JP2018162411 A JP 2018162411A JP 2018162411 A JP2018162411 A JP 2018162411A JP 2019065386 A JP2019065386 A JP 2019065386A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 267
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 112
- 239000010949 copper Substances 0.000 claims abstract description 75
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052802 copper Inorganic materials 0.000 claims abstract description 74
- 230000001186 cumulative effect Effects 0.000 claims abstract description 57
- 229910052751 metal Inorganic materials 0.000 claims abstract description 52
- 239000002184 metal Substances 0.000 claims abstract description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 42
- 229910052709 silver Inorganic materials 0.000 claims abstract description 39
- 239000004332 silver Substances 0.000 claims abstract description 39
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000001301 oxygen Substances 0.000 claims abstract description 32
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000009826 distribution Methods 0.000 claims abstract description 7
- 239000000758 substrate Substances 0.000 claims description 11
- 238000005507 spraying Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 239000011164 primary particle Substances 0.000 description 65
- 239000011163 secondary particle Substances 0.000 description 53
- 238000000034 method Methods 0.000 description 34
- 239000000203 mixture Substances 0.000 description 15
- 229910045601 alloy Inorganic materials 0.000 description 14
- 239000000956 alloy Substances 0.000 description 14
- 229910017944 Ag—Cu Inorganic materials 0.000 description 13
- 238000009825 accumulation Methods 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 12
- 239000000919 ceramic Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000011230 binding agent Substances 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 238000009692 water atomization Methods 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- -1 silver ions Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 241000557876 Centaurea cineraria Species 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052809 inorganic oxide Inorganic materials 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000007639 printing Methods 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
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-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
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000003130 blood coagulation factor inhibitor Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005336 cracking Methods 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
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
- H01B1/026—Alloys based on copper
-
- 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
- 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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- B22—CASTING; POWDER METALLURGY
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
- B22F7/04—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers with one or more layers not made from powder, e.g. made from solid metal
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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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
- C22C5/08—Alloys based on silver with copper as the next major constituent
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- H—ELECTRICITY
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- 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
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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
- B22F2009/0804—Dispersion in or on liquid, other than with sieves
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- 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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- B22F2301/10—Copper
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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
Description
純度99.99質量%のショット銀23.96kgと(228ppmの銅を含む)Ag−Cu合金6.04kgとを大気雰囲気中において1600℃に加熱して溶解した溶湯(46ppmの銅を含む銀の溶湯)をタンディッシュ下部から落下させながら、水アトマイズ装置により大気雰囲気中において水圧150MPa、水量160L/分でアルカリ水(純水21.6m3に対して苛性ソーダ157.55gを添加したアルカリ水溶液(pH10.7))を吹き付けて急冷凝固させ、得られたスラリーを固液分離し、固形物を水洗し、乾燥し、(微量の銅を含む)銀粉を得た。
ショット銀25kgと(581ppmの銅を含む)Ag−Cu合金15kgとを溶解した溶湯(218ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(微量の銅を含む)銀粉を得た。
ショット銀24kgと(595ppmの銅を含む)Ag−Cu合金16kgとを溶解した溶湯(238ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(微量の銅を含む)銀粉を得た。
ショット銀25kgと(675ppmの銅を含む)Ag−Cu合金15kgとを溶解した溶湯(253ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(微量の銅を含む)銀粉を得た。
ショット銀18.62kgと(975ppmの銅を含む)Ag−Cu合金11.38kgとを溶解した溶湯(370ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(微量の銅を含む)銀粉を得た。
ショット銀6.27kgと(1343ppmの銅を含む)Ag−Cu合金2.43kgとを溶解した溶湯(375ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(微量の銅を含む)銀粉を得た。
ショット銀29.79kgと(1508ppmの銅を含む)Ag−Cu合金10.21kgとを溶解した溶湯(385ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(微量の銅を含む)銀粉を得た。
ショット銀39.97kgと(28質量%の銅を含む)Ag−Cu合金0.031kgとを溶解した溶湯(218ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(220ppmの銅を含む)銀粉を得た。
ショット銀31.79kgと(1252ppmの銅を含む)Ag−Cu合金8.21kgとを溶解した溶湯(257ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(270ppmの銅を含む)銀粉を得た。
ショット銀48.00kgと(757ppmの銅を含む)Ag−Cu合金32.00kgとを溶解した溶湯(303ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(310ppmの銅を含む)銀粉を得た。
ショット銀20.69kgと(723ppmの銅を含む)Ag−Cu合金19.31kgとを溶解した溶湯(349ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(360ppmの銅を含む)銀粉を得た。
ショット銀6.00kgと(800ppmの銅を含む)Ag−Cu合金14.00kgとを溶解した溶湯(560ppmの銅を含む銀の溶湯)を使用した以外は、実施例1と同様の方法により、(620ppmの銅を含む)銀粉を得た。
ショット銀5kgを溶解した溶湯を使用した以外は、実施例1と同様の方法により、銀粉を得た。
Claims (12)
- 40ppm以上の銅を含み且つ炭素含有量が0.1質量%以下であることを特徴とする、銀粉。
- 前記銀粉中の銅の含有量が40〜10000ppmであることを特徴とする、請求項1に記載の銀粉。
- レーザー回折式粒度分布測定装置により測定した体積基準の累積50%粒子径が1〜15μmであることを特徴とする、請求項1または2に記載の銀粉。
- 前記銀粉の累積50%粒子径(D50径)に対する、電界放出型走査電子顕微鏡によって観測した単体粒子の平均粒子径(SEM径)の比(SEM径/D50径)が0.3〜1.0であることを特徴とする、請求項3に記載の銀粉。
- 前記銀粉の累積50%粒子径(D50径)に対するタップ密度の比(タップ密度/D50径)が0.45〜3.0g/(cm3・μm)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。
- 前記銀粉中の酸素含有量が0.1質量%以下であることを特徴とする、請求項1乃至5のいずれかに記載の銀粉。
- 前記銀粉のBET比表面積が0.1〜1.0m2/gであることを特徴とする、請求項1乃至6のいずれかに記載の銀粉。
- 前記銀粉のタップ密度が2〜6g/cm3であることを特徴とする、請求項1乃至7のいずれかに記載の銀粉。
- 40ppm以上の銅を含む銀を溶解した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を特徴とする、銀粉の製造方法。
- 前記溶湯中の銅の含有量が40〜10000ppmであることを特徴とする、請求項9に記載の銀粉の製造方法。
- 請求項1乃至8のいずれかに記載の銀粉が有機成分中に分散していることを特徴とする、導電性ペースト。
- 請求項11の導電性ペーストを基板上に塗布した後に焼成して導電膜を製造することを特徴とする、導電膜の製造方法。
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CN201880061178.3A CN111132777B (zh) | 2017-09-29 | 2018-09-18 | 银粉及其制造方法 |
PCT/JP2018/034336 WO2019065341A1 (ja) | 2017-09-29 | 2018-09-18 | 銀粉およびその製造方法 |
US16/648,423 US11420256B2 (en) | 2017-09-29 | 2018-09-18 | Silver powder and method for producing same |
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