JP2016050360A - 銀被覆銅粉およびその製造方法 - Google Patents
銀被覆銅粉およびその製造方法 Download PDFInfo
- Publication number
- JP2016050360A JP2016050360A JP2015161498A JP2015161498A JP2016050360A JP 2016050360 A JP2016050360 A JP 2016050360A JP 2015161498 A JP2015161498 A JP 2015161498A JP 2015161498 A JP2015161498 A JP 2015161498A JP 2016050360 A JP2016050360 A JP 2016050360A
- Authority
- JP
- Japan
- Prior art keywords
- silver
- copper powder
- gold
- coated
- coated copper
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 199
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 239000004332 silver Substances 0.000 title claims abstract description 182
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 175
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000010931 gold Substances 0.000 claims abstract description 112
- 229910052737 gold Inorganic materials 0.000 claims abstract description 109
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 92
- 238000007747 plating Methods 0.000 claims abstract description 35
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011248 coating agent Substances 0.000 claims abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 15
- 229940100890 silver compound Drugs 0.000 claims abstract description 12
- 150000003379 silver compounds Chemical class 0.000 claims abstract description 12
- PJAHUDTUZRZBKM-UHFFFAOYSA-K potassium citrate monohydrate Chemical compound O.[K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O PJAHUDTUZRZBKM-UHFFFAOYSA-K 0.000 claims abstract description 9
- 229960004543 anhydrous citric acid Drugs 0.000 claims abstract description 8
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims abstract description 7
- 229960005261 aspartic acid Drugs 0.000 claims abstract description 7
- CKLJMWTZIZZHCS-UHFFFAOYSA-N D-OH-Asp Natural products OC(=O)C(N)CC(O)=O CKLJMWTZIZZHCS-UHFFFAOYSA-N 0.000 claims abstract description 6
- CKLJMWTZIZZHCS-UWTATZPHSA-N L-Aspartic acid Natural products OC(=O)[C@H](N)CC(O)=O CKLJMWTZIZZHCS-UWTATZPHSA-N 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 28
- 230000001186 cumulative effect Effects 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 14
- PPVNYSRNJQOELF-UHFFFAOYSA-N [K].[Au].N#CC#N Chemical compound [K].[Au].N#CC#N PPVNYSRNJQOELF-UHFFFAOYSA-N 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- 239000004020 conductor Substances 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 48
- 238000003860 storage Methods 0.000 abstract description 10
- 239000007788 liquid Substances 0.000 abstract description 4
- 238000000889 atomisation Methods 0.000 abstract 1
- XTFKWYDMKGAZKK-UHFFFAOYSA-N potassium;gold(1+);dicyanide Chemical compound [K+].[Au+].N#[C-].N#[C-] XTFKWYDMKGAZKK-UHFFFAOYSA-N 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 33
- 239000000706 filtrate Substances 0.000 description 21
- 239000010949 copper Substances 0.000 description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 18
- 229910052802 copper Inorganic materials 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 239000000126 substance Substances 0.000 description 11
- 239000010944 silver (metal) Substances 0.000 description 9
- 229910001961 silver nitrate Inorganic materials 0.000 description 9
- 239000003960 organic solvent Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 6
- 239000001099 ammonium carbonate Substances 0.000 description 6
- 239000002738 chelating agent Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 235000012501 ammonium carbonate Nutrition 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- -1 citric acid is added Chemical class 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 4
- 235000012431 wafers Nutrition 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229960004106 citric acid Drugs 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 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
- 230000001376 precipitating effect Effects 0.000 description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 2
- 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 2
- 239000008117 stearic acid Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000009692 water atomization Methods 0.000 description 2
- DAFHKNAQFPVRKR-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylpropanoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)C DAFHKNAQFPVRKR-UHFFFAOYSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 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
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- PPJLYRZMZCJFAA-UHFFFAOYSA-N [K].[K].N#CC#N Chemical compound [K].[K].N#CC#N PPJLYRZMZCJFAA-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 1
- 235000003704 aspartic acid Nutrition 0.000 description 1
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
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- 239000012046 mixed solvent Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/26—Processes for applying liquids or other fluent materials performed by applying the liquid or other fluent material from an outlet device in contact with, or almost in contact with, the surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
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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
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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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
- B22F1/17—Metallic particles coated with metal
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- C—CHEMISTRY; METALLURGY
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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- C—CHEMISTRY; METALLURGY
- 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
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
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- C23C18/1637—Composition of the substrate metallic substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1646—Characteristics of the product obtained
- C23C18/165—Multilayered product
- C23C18/1653—Two or more layers with at least one layer obtained by electroless plating and one layer obtained by electroplating
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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Abstract
Description
アトマイズ法により製造された市販の銅粉(日本アトマイズ加工株式会社製のアトマイズ銅粉SF−Cu 5μm)を用意し、この(銀被覆前の)銅粉の粒度分布を求めたところ、銅粉の累積10%粒子径(D10)は2.26μm、累積50%粒子径(D50)は5.20μm、累積90%粒子径(D90)は9.32μmであった。なお、銅粉の粒度分布は、レーザー回折式粒度分布装置(日機装株式会社製のマイクロトラック粒度分布測定装置MT−3300)により測定して、累積10%粒子径(D10)、累積50%粒子径(D50)、累積90%粒子径(D90)を求めた。
実施例1で得られた銀被覆銅粉3gを純水15gに添加し、金めっき液の量を0.55mLとした以外は、実施例1と同様の方法により、表面に金を担持させた銀被覆銅粉を得た。なお、ろ液の量は123.65gであり、ろ液中のAu、Ag、Cuの濃度を実施例1と同様の方法により測定したところ、それぞれ1mg/L未満、1mg/L未満、66mg/Lであった。
実施例1で得られた銀被覆銅粉3gを純水15gに添加し、金めっき液の量を0.25mLとした以外は、実施例1と同様の方法により、表面に金を担持させた銀被覆銅粉を得た。なお、ろ液の量は74.74gであり、ろ液中のAu、Ag、Cuの濃度を実施例1と同様の方法により測定したところ、それぞれ1mg/L未満、1mg/L未満、99mg/Lであった。
実施例1で得られた銀被覆銅粉5gを純水15gに添加し、金めっき液の量を0.25mLとした以外は、実施例1と同様の方法により、表面に金を担持させた銀被覆銅粉を得た。なお、ろ液の量は110.5gであり、ろ液中のAu、Ag、Cuの濃度を実施例1と同様の方法により測定したところ、それぞれ1mg/L未満、1mg/L未満、110mg/Lであった。
実施例1で得られた銀被覆銅粉7gを純水15gに添加し、これを金濃度49g/Lのシアン金カリウム溶液からなる金めっき液0.25mLに添加した以外は、実施例1と同様の方法により、表面に金を担持させた銀被覆銅粉を得た。なお、ろ液の量は84.82gであり、ろ液中のAu、Ag、Cuの濃度を実施例1と同様の方法により測定したところ、それぞれ5mg/L、1mg/L未満、4mg/Lであった。本実施例では、クエン酸などを添加していないため、金めっき液が酸性でないので、反応が進み難く、ろ液にAuが残存していた。
金めっき液として、金濃度10g/Lのシアン金カリウム溶液0.91gと、1.87gのクエン酸三カリウム1水和物と、0.07gの無水クエン酸とを含む溶液から分取した金めっき液1mLを使用し、実施例1で得られた銀被覆銅粉3gを純水15gに添加した以外は、実施例1と同様の方法により、表面に金を担持させた銀被覆銅粉を得た。なお、ろ液の量は100.57gであり、ろ液中のAu、Ag、Cuの濃度を実施例1と同様の方法により測定したところ、それぞれ1mg/L未満、1mg/L未満、83mg/Lであった。
金めっき液として、金濃度10g/Lのシアン金カリウム溶液5mLに、0.05gのクエン酸三カリウム1水和物と、0.041gの無水クエン酸とを添加した溶液から分取した金めっき液1mLを使用し、実施例1で得られた銀被覆銅粉10gを純水15gに添加した以外は、実施例1と同様の方法により、表面に金を担持させた銀被覆銅粉を得た。なお、ろ液の量は123.9gであり、ろ液中のAu、Ag、Cuの濃度を実施例1と同様の方法により測定したところ、それぞれ1mg/L未満、1mg/L未満、120mg/Lであった。
金めっき液として、金濃度10g/Lのシアン金カリウム溶液5mLに、0.05gのクエン酸三カリウム1水和物と、0.041gの無水クエン酸と、0.0085gのL−アスパラギン酸とを添加した溶液から分取した金めっき液1mLを使用し、実施例1で得られた銀被覆銅粉10gを純水15gに添加した以外は、実施例1と同様の方法により、表面に金を担持させた銀被覆銅粉を得た。なお、ろ液の量は88gであり、ろ液中のAu、Ag、Cuの濃度を実施例1と同様の方法により測定したところ、それぞれ1mg/L未満、1mg/L未満、140mg/Lであった。
実施例1で得られた銀被覆銅粉(金めっき液に添加しないで、表面に金を担持させていない銀被覆銅粉)中のAgの含有量を実施例1と同様の方法により測定したところ、10.9質量%であった。また、銀被覆銅粉の200℃、250℃、300℃および350℃における重量増加率を実施例1と同様の方法により求めたところ、それぞれ0.16%、0.46%、1.27%、3.80%であった。
アトマイズ法により製造された市販の銅粉(日本アトマイズ加工株式会社製のアトマイズ銅粉SFR−5μm)を用意し、この銅粉の粒度分布を実施例1と同様の方法により求めたところ、銅粉の累積10%粒子径(D10)は2.12μm、累積50%粒子径(D50)は4.93μm、累積90%粒子径(D90)は10.19μmであった。
シアン金カリウム(小島薬品化学株式会社製)1.4633gと、無水クエン酸(和光純薬工業株式会社製)0.8211gと、L−アスパラギン酸(和光純薬工業株式会社製)0.1708gと、クエン酸三カリウム1水和物(和光純薬工業株式会社製)0.9998gとを純水100gに加えて30℃で11分間撹拌して金めっき液を作製した。
Claims (15)
- 表面が銀含有層で被覆された銅粉を金めっき液に添加して、銀含有層で被覆された銅粉の表面に金を担持させることを特徴とする、銀被覆銅粉の製造方法。
- 前記銀含有層が銀または銀化合物からなる層であることを特徴とする、請求項1に記載の銀被覆銅粉の製造方法。
- 前記銀被覆銅粉に対する前記銀含有層の量が5質量%以上であることを特徴とする、請求項1または2に記載の銀被覆銅粉の製造方法。
- 前記銀被覆銅粉に対する前記金の量が0.01質量%以上であることを特徴とする、請求項1乃至3のいずれかに記載の銀被覆銅粉の製造方法。
- 前記金めっき液が、シアン金カリウム溶液からなることを特徴とする、請求項1乃至4のいずれかに記載の銀被覆銅粉の製造方法。
- 前記金めっき液が、クエン酸三カリウム1水和物、無水クエン酸およびL−アスパラギン酸からなる群から選ばれる少なくとも一種以上を添加したシアン金カリウム溶液からな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被覆銅粉の製造方法。
- 前記銅粉のレーザー回折式粒度分布装置により測定した累積50%粒子径(D50径)が0.1〜15μm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被覆銅粉の製造方法。
- 銀含有層で被覆された銅粉の表面に金が担持されていることを特徴とする、銀被覆銅粉。
- 前記銀含有層が銀または銀化合物からなる層であることを特徴とする、請求項8に記載の銀被覆銅粉。
- 前記銀被覆銅粉に対する前記銀含有層の量が5質量%以上であることを特徴とする、請求項8または9に記載の銀被覆銅粉。
- 前記銀被覆銅粉に対する前記金の量が0.01質量%以上であることを特徴とする、請求項8乃至10のいずれかに記載の銀被覆銅粉。
- 前記銅粉のレーザー回折式粒度分布装置により測定した累積50%粒子径(D50径)が0.1〜15μmであることを特徴とする、請求項8乃至11のいずれかに記載の銀被覆銅粉。
- 請求項8乃至12のいずれかに記載の銀粉を導体として用いたことを特徴とする、導電性ペースト。
- 溶剤および樹脂を含み、導電性紛体として請求項8乃至12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。
- 請求項13または14の導電性ペーストを基板に塗布した後に硬化させることにより基板の表面に電極を形成することを特徴とする、太陽電池用電極の製造方法。
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015161498A JP6567921B2 (ja) | 2014-08-29 | 2015-08-19 | 銀被覆銅粉およびその製造方法 |
PCT/JP2015/004197 WO2016031210A1 (ja) | 2014-08-29 | 2015-08-21 | 銀被覆銅粉およびその製造方法 |
CN201580046175.9A CN106794516B (zh) | 2014-08-29 | 2015-08-21 | 银被覆铜粉及其制造方法 |
KR1020177007296A KR20170052595A (ko) | 2014-08-29 | 2015-08-21 | 은 피복 구리분 및 그 제조 방법 |
US15/501,880 US20170232510A1 (en) | 2014-08-29 | 2015-08-21 | Silver-coated copper powder and method for producing same |
TW104127922A TWI668707B (zh) | 2014-08-29 | 2015-08-26 | 覆銀銅粉及其製造方法 |
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Cited By (2)
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JP2017201052A (ja) * | 2016-05-06 | 2017-11-09 | 株式会社村田製作所 | 金属粉末の製造方法 |
CN108213415A (zh) * | 2018-01-11 | 2018-06-29 | 宁波广新纳米材料有限公司 | 耐腐蚀耐高温银铜包覆粉的生产方法 |
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JP6151742B2 (ja) * | 2015-06-09 | 2017-06-21 | タツタ電線株式会社 | 導電性ペースト |
JP6811080B2 (ja) * | 2016-02-03 | 2021-01-13 | Dowaエレクトロニクス株式会社 | 銀被覆銅粉およびその製造方法 |
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EP1327491B1 (en) * | 2000-10-02 | 2010-05-12 | Asahi Kasei EMD Corporation | Functional metal alloy particles |
US20050227074A1 (en) * | 2004-04-08 | 2005-10-13 | Masaaki Oyamada | Conductive electrolessly plated powder and method for making same |
JP4261973B2 (ja) * | 2003-04-28 | 2009-05-13 | 日本化学工業株式会社 | 導電性無電解めっき粉体の製造方法 |
JP4235227B2 (ja) * | 2004-09-02 | 2009-03-11 | 積水化学工業株式会社 | 導電性微粒子及び異方性導電材料 |
JP4962706B2 (ja) * | 2006-09-29 | 2012-06-27 | 日本化学工業株式会社 | 導電性粒子およびその製造方法 |
JP5430093B2 (ja) * | 2008-07-24 | 2014-02-26 | デクセリアルズ株式会社 | 導電性粒子、異方性導電フィルム、及び接合体、並びに、接続方法 |
JP5402350B2 (ja) * | 2009-07-24 | 2014-01-29 | 藤倉化成株式会社 | 導電性ペーストの製造方法および導電性ペースト |
JP5512306B2 (ja) * | 2010-01-29 | 2014-06-04 | 日本化学工業株式会社 | 導電性粒子の製造方法 |
CN102211185B (zh) * | 2011-05-17 | 2014-01-22 | 陈钢强 | 银包铜合金粉 |
KR101151366B1 (ko) * | 2011-11-24 | 2012-06-08 | 한화케미칼 주식회사 | 도전성 입자 및 이의 제조방법 |
JP2014005531A (ja) * | 2012-01-17 | 2014-01-16 | Dowa Electronics Materials Co Ltd | 銀被覆銅合金粉末およびその製造方法 |
JP5973257B2 (ja) * | 2012-07-03 | 2016-08-23 | 日本化学工業株式会社 | 導電性粒子及びそれを含む導電性材料 |
CN102873324A (zh) * | 2012-10-17 | 2013-01-16 | 厦门大学 | 一种包裹型铜镍银复合粉体及其制备方法 |
JP5785532B2 (ja) * | 2012-11-30 | 2015-09-30 | 三井金属鉱業株式会社 | 銀コート銅粉及びその製造方法 |
CN103464742B (zh) * | 2013-09-18 | 2016-01-20 | 武汉理工大学 | 一种铜包覆银包覆钨的复合包覆粉体的制备方法 |
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- 2015-08-21 US US15/501,880 patent/US20170232510A1/en not_active Abandoned
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Cited By (2)
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JP2017201052A (ja) * | 2016-05-06 | 2017-11-09 | 株式会社村田製作所 | 金属粉末の製造方法 |
CN108213415A (zh) * | 2018-01-11 | 2018-06-29 | 宁波广新纳米材料有限公司 | 耐腐蚀耐高温银铜包覆粉的生产方法 |
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CN106794516B (zh) | 2020-05-26 |
WO2016031210A1 (ja) | 2016-03-03 |
JP6567921B2 (ja) | 2019-08-28 |
TWI668707B (zh) | 2019-08-11 |
CN106794516A (zh) | 2017-05-31 |
US20170232510A1 (en) | 2017-08-17 |
KR20170052595A (ko) | 2017-05-12 |
TW201614678A (en) | 2016-04-16 |
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