JP6737381B1 - 銀ペースト及びその製造方法並びに接合体の製造方法 - Google Patents
銀ペースト及びその製造方法並びに接合体の製造方法 Download PDFInfo
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- JP6737381B1 JP6737381B1 JP2019114214A JP2019114214A JP6737381B1 JP 6737381 B1 JP6737381 B1 JP 6737381B1 JP 2019114214 A JP2019114214 A JP 2019114214A JP 2019114214 A JP2019114214 A JP 2019114214A JP 6737381 B1 JP6737381 B1 JP 6737381B1
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- silver
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 462
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 373
- 239000004332 silver Substances 0.000 title claims abstract description 373
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 212
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 54
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229930195729 fatty acid Natural products 0.000 claims abstract description 54
- 239000000194 fatty acid Substances 0.000 claims abstract description 54
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 53
- 239000011259 mixed solution Substances 0.000 claims description 43
- 239000002904 solvent Substances 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 38
- 238000010438 heat treatment Methods 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 28
- 229920005989 resin Polymers 0.000 claims description 21
- 239000011347 resin Substances 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 4
- 238000004898 kneading Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010586 diagram Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 40
- 238000009826 distribution Methods 0.000 description 20
- 239000010419 fine particle Substances 0.000 description 18
- 238000012360 testing method Methods 0.000 description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 14
- 239000002002 slurry Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000011164 primary particle Substances 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 239000005416 organic matter Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 229910001961 silver nitrate Inorganic materials 0.000 description 7
- -1 aliphatic amines Chemical class 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 6
- 229940071536 silver acetate Drugs 0.000 description 6
- 229920001187 thermosetting polymer Polymers 0.000 description 6
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000011342 resin composition Substances 0.000 description 5
- 239000011163 secondary particle Substances 0.000 description 5
- 150000003378 silver Chemical class 0.000 description 5
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229920002050 silicone resin Polymers 0.000 description 4
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000002296 dynamic light scattering Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 239000011268 mixed slurry Substances 0.000 description 3
- FJDUDHYHRVPMJZ-UHFFFAOYSA-N nonan-1-amine Chemical compound CCCCCCCCCN FJDUDHYHRVPMJZ-UHFFFAOYSA-N 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000000790 scattering method Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 description 3
- OHGHHPYRRURLHR-UHFFFAOYSA-M silver;tetradecanoate Chemical compound [Ag+].CCCCCCCCCCCCCC([O-])=O OHGHHPYRRURLHR-UHFFFAOYSA-M 0.000 description 3
- 239000001509 sodium citrate Substances 0.000 description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000004280 Sodium formate Substances 0.000 description 2
- YFHNDHXQDJQEEE-UHFFFAOYSA-N acetic acid;hydrazine Chemical compound NN.CC(O)=O YFHNDHXQDJQEEE-UHFFFAOYSA-N 0.000 description 2
- 239000005456 alcohol based solvent Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003141 primary amines Chemical class 0.000 description 2
- 150000003335 secondary amines Chemical class 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000010944 silver (metal) Substances 0.000 description 2
- 229940071575 silver citrate Drugs 0.000 description 2
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 2
- 235000019254 sodium formate Nutrition 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 150000003512 tertiary amines Chemical class 0.000 description 2
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- QUTYHQJYVDNJJA-UHFFFAOYSA-K trisilver;2-hydroxypropane-1,2,3-tricarboxylate Chemical compound [Ag+].[Ag+].[Ag+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QUTYHQJYVDNJJA-UHFFFAOYSA-K 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- 229940088601 alpha-terpineol Drugs 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- AVIYEYCFMVPYST-UHFFFAOYSA-N hexane-1,3-diol Chemical group CCCC(O)CCO AVIYEYCFMVPYST-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- WSTNFGAKGUERTC-UHFFFAOYSA-N n-ethylhexan-1-amine Chemical compound CCCCCCNCC WSTNFGAKGUERTC-UHFFFAOYSA-N 0.000 description 1
- 239000004843 novolac epoxy resin Substances 0.000 description 1
- AZJXQVRPBZSNFN-UHFFFAOYSA-N octane-3,3-diol Chemical compound CCCCCC(O)(O)CC AZJXQVRPBZSNFN-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007665 sagging Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- JKOCEVIXVMBKJA-UHFFFAOYSA-M silver;butanoate Chemical compound [Ag+].CCCC([O-])=O JKOCEVIXVMBKJA-UHFFFAOYSA-M 0.000 description 1
- CYLMOXYXYHNGHZ-UHFFFAOYSA-M silver;propanoate Chemical compound [Ag+].CCC([O-])=O CYLMOXYXYHNGHZ-UHFFFAOYSA-M 0.000 description 1
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 1
- 235000010378 sodium ascorbate Nutrition 0.000 description 1
- 229960005055 sodium ascorbate Drugs 0.000 description 1
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
Classifications
-
- 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
- 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
-
- 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
-
- 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
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
-
- 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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
- B23K35/025—Pastes, creams, slurries
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0466—Alloys based on noble metals
-
- 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
-
- 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
- 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
- B22F2007/042—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 characterised by the layer forming method
- B22F2007/047—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 characterised by the layer forming method non-pressurised baking of the paste or slurry containing metal powder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/02—Bonding areas; Manufacturing methods related thereto
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Abstract
Description
先ず、酢酸銀(脂肪酸銀)、アミノデカン(脂肪族アミン)及びブチルカルビトールアセテート(溶媒)を用意し、脂肪酸銀、脂肪族アミン及び溶媒の合計量を100質量%としたとき、酢酸銀(脂肪酸銀)22質量%、アミノデカン(脂肪族アミン)41.3質量%、ブチルカルビトールアセテート(溶媒)36.7質量%の割合で取り分け、これらをスターラーの撹拌子とともにガラス製の容器に入れた。そして、50℃に加熱したホットプレートに前記容器を載せ、スターラーの撹拌子を300rpmで回転させながら、1時間撹拌して混合液を調製した。次いで、この混合液が貯留された容器をホットプレートから降ろしてこの混合液の温度を室温まで下げた。これにより脂肪酸銀・脂肪族アミン混合溶液(以下、単に混合溶液と呼ぶ)を調製した。この混合溶液を実施例1とした。
実施例2〜14及び比較例1〜2の混合溶液は、脂肪酸銀、脂肪族アミン及び溶媒として、表1に示す種類のものを用いるとともに、脂肪酸銀、脂肪族アミン及び溶媒を、表1に示すような割合でそれぞれ配合した。なお、比較例1では脂肪酸銀を含まず、比較例2では脂肪族アミンを含まないため、混合溶液ではないけれども、本明細書では、便宜上、比較例1〜2も混合溶液と呼ぶ。また、表1中の脂肪酸銀の種類の欄において、『A1』は酢酸銀であり、『A2』はシュウ酸銀であり、『A3』はミリスチン酸銀である。また、表1中の脂肪族アミンの種類の欄において、『B1』はアミノデカンを示し、『B2』はヘキシルアミンを示し、『B3』はノニルアミンであり、『B4』はドデシルアミンである。更に、表1中の溶媒の種類の欄において、『C1』はブチルカルビトールアセテートであり、『C2』はエチレングリコールであり、『C3』はテルピネオールであり、『C4』は2−エチル1,3−ヘキサンジオールである。
実施例1〜14及び比較例1〜2の混合溶液を撹拌しながら130℃に10分間加熱した後、この混合溶液1gをシリコンウェーハ上に滴下し、25℃の温度で減圧乾燥することにより、乾燥物が表面に付着したウェーハを作製した。そして、このウェーハの表面をSEM(走査電子顕微鏡)観察し、表面に付着した粒子を1000個計数し、画像処理ソフト(Image−J(アメリカ国立衛生研究所:開発))を用いて、抽出した粒子(一次粒子)の投影面積を測定し、得られた投影面積から円相当径を算出し、これを一次粒子径とした。輪郭が視認できない箇所がある粒子については、円相当径を測定しなかった。得られた一次粒子径を、体積基準の粒径に変換し、その体積基準の粒径の平均値を乾燥物の平均粒径とした。また、前記乾燥物から銀粉が生じたものを『可』とし、乾燥物から銀粉が生じなかったもの或いは銀粉を測定できなかったものを『不可』と判定した。前記乾燥物の平均粒径と、判定結果を表2に示す。なお、表2には、脂肪酸銀の種類と、脂肪族アミンの種類と溶媒の種類も示した。
銀ペーストを100質量%とするために、実施例1の混合溶液25質量%と銀粉(第1〜第3銀粒子の凝集体)75質量%を混練した後、プラネタリー遊星撹拌機にて撹拌し、更に3本ロールミルにて混練した。これにより銀ペーストを得た。この銀ペーストを実施例15とした。
先ず、銀微粒子0.1gをイオン交換水20g中に投入し、25kHzの超音波を5分間照射して、イオン交換水に銀微粒子を分散させた。次に、得られた銀微粒子の分散液を、動的光散乱式粒度分布測定装置(堀場製作所:LB−550)用の観察セルに注ぎ、この装置の手順に従い粒度分布を測定した。
SEMを用いて、第1〜第3銀粒子が凝集した凝集体(二次粒子)500個の画像を取得し、各銀粒子凝集体に含まれている銀粒子(一次粒子)の粒径を測定した。このときSEMの装置倍率は100000倍とした。500個の銀粒子凝集体のSEM画像から、銀粒子(一次粒子)の全体の輪郭が視認できる銀粒子を抽出した。次いで、画像処理ソフト(Image−J)を用いて、抽出した銀粒子の投影面積を測定し、得られた投影面積から円相当径を算出し、これを銀粒子の粒径とした。輪郭が視認できない箇所がある銀粒子については、円相当径を測定しなかった。得られた銀粒子の粒径を、体積基準の粒径に変換し、その体積基準の粒径の粒度分布を求めた。その結果を表5に示す。
混合溶液と混合する前の銀粉を量り取り、大気中にて150℃の温度で30分間加熱した。加熱後、室温まで放冷し、銀粉の質量を測定した。次の式(1)より、有機物の含有量を算出した。この結果、有機物の含有量は0.2質量%であった。
有機物の含有量(質量%)={(A−B)/A}×100 ……(1)
但し、式(1)中のAは加熱前の銀粉の質量であり、Bは加熱後の銀粉の質量である。得られた結果を表5に示す。
実施例16〜33及び比較例3〜8の銀ペーストは、混合溶液として、表1に示す脂肪酸銀、脂肪族アミン及び溶媒種類のものを用いるとともに、銀粉、混合溶液を、表3及び表4に示すような割合でそれぞれ配合し、表3及び表4に示した配合以外は、実施例15と同様にして、銀ペーストを調製した。なお、実施例15〜33及び比較例3〜8で用いた混合溶液を表3及び表4中の混合溶液の種類の欄に実施例1〜14のいずれかで示した。また、実施例15〜33及び比較例3〜8では、表5に示す粒度分布の異なる10種類(No.1〜No.10)の銀粉のいずれかを配合しており、実施例15〜33及び比較例3〜8で用いた銀粉を表3及び表4中の銀粉の種類の欄にNo.1〜No.10のいずれかで示した。
(1) 実施例15〜33及び比較例3〜8の銀ペーストを用いて接合体をそれぞれ作製した。具体的には、先ず、第1部材として、最表面に金メッキを施した2.5mm角のSiウェーハ(厚さ:200μm)を用意し、第2部材として、最表面に銀メッキを施した20mm角のCu板(厚さ:1mm)を用意した。次いで、第2部材の表面に、前記銀ペーストを、メタルマスク法により塗布して銀ペースト層を形成した。次に、銀ペースト層上に第1部材を載せて、積層体を作製した。更に、この積層体を焼成することにより、即ち積層体を150℃の温度(加熱温度)に60分間(加熱時間)保持することにより、第1部材と第2部材とを接合層を介して接合した。これらの接合体を実施例15〜33及び比較例3〜8の接合体とした。なお、前記積層体は、加圧しなかった。これらの接合体の接合強度を次のように測定した。
実施例15〜33及び比較例3〜8の接合体の接合強度は、せん断強度評価試験機を用いて測定した。具体的には、接合強度の測定は、接合体の第1部材(Cu板)を水平に固定し、接合層の表面(上面)から50μm上方の位置でシェアツールにより、第2部材(Siウェーハ)を横から水平方向に押して、第2部材が破断されたときの強度を測定することによって行った。なお、シェアツールの移動速度は0.1mm/秒とした。1条件に付き3回強度試験を行い、それらの算術平均値を接合強度の測定値とした。
実施例15〜33及び比較例3〜8の銀焼成膜についてレーザフラッシュ法により熱拡散率を測定した。具体的には、先ず、銀焼成膜の表面にパルスレーザを均一に照射して瞬間的に加熱したときの銀焼成膜の裏面の温度変化T(t)を測定した。次に、銀焼成膜の裏面の温度変化T(t)は1次元の熱伝導方程式で表されるので、銀焼成膜の裏面の温度変化T(t)を縦軸にとりかつ経過時間tを横軸にとることにより(T(t)−t)曲線が得られ、この曲線から最大上昇温度TMAXの半分の温度に達するのに要した時間t0.5を求めた。そして、銀焼成膜の熱拡散率αを次の式(2)により求めた。
α = 1.370×L2/(π2×t0.5) ……(2)
前記式(2)中のLは銀焼成膜の厚さである。これらの接合体の接合強度及び銀焼成膜の熱拡散率を表3及び表4に示す。
実施例15〜17及び比較例3の接合体について、接合層の断面をFE−SEMにより観察した。その結果を図1〜図4に示す。
実施例34及び35の銀ペーストは、混合溶液及び樹脂として、表1及び表6に示す種類のものを用いるとともに、銀粉、混合溶液及び樹脂を、表6に示すような割合でそれぞれ配合した。樹脂は、混合溶液と銀粉を混合する際に添加し、これらとともに混錬した。なお、表6に示した配合以外は、実施例15と同様にして、銀ペーストを調製した。
実施例17、実施例34及び実施例35の銀ペーストを用いて、比較試験2と同様に接合体をそれぞれ作製し、これらの接合体の接合強度を比較試験2と同様に測定した。また、実施例17、実施例34及び実施例35の銀ペーストを用いて、比較試験2と同様に銀焼成膜をそれぞれ作製し、これらの銀焼成膜の熱拡散率を比較試験2と同様に測定した。更に、実施例17、実施例34及び実施例35の接合体について冷熱サイクル試験を行った後に、これらの接合体の接合強度を比較試験2と同様に測定した。前記冷熱サイクル試験は、気相法を用いて、−40℃に20分保持した後に、+150℃に20分保持する操作を1000サイクル繰返すことにより行った。その結果を表6及び表7に示す。
Claims (5)
- 銀粉と、脂肪酸銀と、脂肪族アミンと、溶媒とを含む銀ペーストであって、
前記銀粉は、粒径が100nm以上500nm未満である第1銀粒子と、粒径が50nm以上100nm未満である第2銀粒子と、粒径が50nm未満である第3銀粒子とからなり、かつ前記第1〜第3銀粒子の合計量100体積%に対して、前記第1銀粒子を55体積%以上95体積%以下、前記第2銀粒子を5体積%以上40体積%以下、前記第3銀粒子を5体積%以下の範囲で含み、
前記脂肪酸銀と前記脂肪族アミンと前記溶媒との合計量を100質量%としたときに、前記脂肪酸銀を13.2質量%〜33.0質量%、前記脂肪族アミンを0.1質量%〜60質量%、前記溶媒を80質量%以下の割合で含み、
前記銀ペーストを100質量%としたときに、前記銀粉の含有量が50質量%〜95質量%である
ことを特徴とする銀ペースト。 - 樹脂を更に含む請求項1記載の銀ペースト。
- 前記脂肪酸銀の少なくとも一部と前記脂肪族アミンの少なくとも一部とが反応して形成される錯体を含む請求項1記載の銀ペースト。
- 脂肪酸銀、脂肪族アミン及び溶媒を、前記脂肪酸銀と前記脂肪族アミンと前記溶媒との合計量を100質量%としたときに、前記脂肪酸銀が13.2質量%〜33.0質量%、前記脂肪族アミンが0.1質量%〜60質量%、前記溶媒が80質量%以下の割合で混合して混合物を得る工程と、
前記混合物を30℃〜100℃に加熱して撹拌した後に冷却して混合溶液を得る工程と、
前記混合溶液と銀粉とを混練して銀ペーストを得る工程と
を含む銀ペーストの製造方法であって、
前記銀粉は、粒径が100nm以上500nm未満である第1銀粒子と、粒径が50nm以上100nm未満である第2銀粒子と、粒径が50nm未満である第3銀粒子とからなり、かつ前記第1〜第3銀粒子の合計量100体積%に対して、前記第1銀粒子を55体積%以上95体積%以下、前記第2銀粒子を5体積%以上40体積%以下、前記第3銀粒子を5体積%以下の範囲で含み、
前記銀ペーストを100質量%としたときに、前記銀粉の含有量が50質量%〜95質量%である
ことを特徴とする銀ペーストの製造方法。 - 第1部材と第2部材とを用意する工程と、
前記第1部材及び/又は前記第2部材の表面に、請求項1ないし3いずれか1項に記載の銀ペースト又は請求項4に記載の方法で製造された銀ペーストを塗布して銀ペースト層を形成する工程と、
前記第1部材と前記第2部材とを前記銀ペースト層を介して積層して積層体を作製する工程と、
前記積層体を加熱することにより前記銀ペースト層中の第1銀粒子と第2銀粒子と第3銀粒子を焼結させて接合層を形成させ、前記第1部材と前記第2部材とが接合層を介して接合された接合体を作製する工程と
を含む接合体の製造方法。
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