JP5944668B2 - 金属銅焼結膜の製造方法 - Google Patents
金属銅焼結膜の製造方法 Download PDFInfo
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- JP5944668B2 JP5944668B2 JP2012006955A JP2012006955A JP5944668B2 JP 5944668 B2 JP5944668 B2 JP 5944668B2 JP 2012006955 A JP2012006955 A JP 2012006955A JP 2012006955 A JP2012006955 A JP 2012006955A JP 5944668 B2 JP5944668 B2 JP 5944668B2
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- JP
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- Prior art keywords
- copper
- acid
- film
- metal copper
- gelatin
- 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.)
- Expired - Fee Related
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- 239000010949 copper Substances 0.000 title claims description 140
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims description 139
- 229910052802 copper Inorganic materials 0.000 title claims description 139
- 229910052751 metal Inorganic materials 0.000 title claims description 89
- 239000002184 metal Substances 0.000 title claims description 89
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000002245 particle Substances 0.000 claims description 81
- 108010010803 Gelatin Proteins 0.000 claims description 62
- 239000008273 gelatin Substances 0.000 claims description 62
- 229920000159 gelatin Polymers 0.000 claims description 62
- 235000019322 gelatine Nutrition 0.000 claims description 62
- 235000011852 gelatine desserts Nutrition 0.000 claims description 62
- 239000002253 acid Substances 0.000 claims description 60
- 229920000642 polymer Polymers 0.000 claims description 47
- -1 glycol ethers Chemical class 0.000 claims description 46
- 239000002270 dispersing agent Substances 0.000 claims description 41
- 150000001412 amines Chemical class 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 34
- 239000006185 dispersion Substances 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 26
- 239000003960 organic solvent Substances 0.000 claims description 22
- 239000007788 liquid Substances 0.000 claims description 11
- 239000012298 atmosphere Substances 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- 150000002334 glycols Chemical class 0.000 claims description 3
- 150000002170 ethers Chemical class 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 description 66
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 32
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 27
- 229960004643 cupric oxide Drugs 0.000 description 25
- 239000005751 Copper oxide Substances 0.000 description 23
- 239000008139 complexing agent Substances 0.000 description 23
- 229910000431 copper oxide Inorganic materials 0.000 description 23
- 239000000463 material Substances 0.000 description 19
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 18
- 229910052717 sulfur Inorganic materials 0.000 description 18
- 239000011593 sulfur Substances 0.000 description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 17
- 239000002585 base Substances 0.000 description 17
- 229910052760 oxygen Inorganic materials 0.000 description 17
- 239000001301 oxygen Substances 0.000 description 17
- 239000003638 chemical reducing agent Substances 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 16
- 239000007789 gas Substances 0.000 description 15
- 125000004429 atom Chemical group 0.000 description 14
- 238000000576 coating method Methods 0.000 description 14
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- 239000003125 aqueous solvent Substances 0.000 description 11
- 239000002904 solvent Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 235000001014 amino acid Nutrition 0.000 description 10
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- 239000011347 resin Substances 0.000 description 10
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 7
- 230000002378 acidificating effect Effects 0.000 description 7
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 150000001735 carboxylic acids 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
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- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- HDFRDWFLWVCOGP-UHFFFAOYSA-N carbonothioic O,S-acid Chemical compound OC(S)=O HDFRDWFLWVCOGP-UHFFFAOYSA-N 0.000 description 5
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- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 4
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 4
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- 229910001882 dioxygen Inorganic materials 0.000 description 4
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 235000011007 phosphoric acid Nutrition 0.000 description 4
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 4
- 239000011112 polyethylene naphthalate Substances 0.000 description 4
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- 238000010298 pulverizing process Methods 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 4
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 102000008186 Collagen Human genes 0.000 description 3
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- 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 3
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
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- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- TTZLKXKJIMOHHG-UHFFFAOYSA-M benzyl-decyl-dimethylazanium;chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 TTZLKXKJIMOHHG-UHFFFAOYSA-M 0.000 description 1
- OCBHHZMJRVXXQK-UHFFFAOYSA-M benzyl-dimethyl-tetradecylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 OCBHHZMJRVXXQK-UHFFFAOYSA-M 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
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- 229910052794 bromium Inorganic materials 0.000 description 1
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- 229910052732 germanium Inorganic materials 0.000 description 1
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- 150000002429 hydrazines Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
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- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
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- 238000000691 measurement method Methods 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
- 229920003145 methacrylic acid copolymer Polymers 0.000 description 1
- 229940117841 methacrylic acid copolymer Drugs 0.000 description 1
- CYEBJEDOHLIWNP-UHFFFAOYSA-N methanethioamide Chemical compound NC=S CYEBJEDOHLIWNP-UHFFFAOYSA-N 0.000 description 1
- 229930182817 methionine Natural products 0.000 description 1
- RMIODHQZRUFFFF-UHFFFAOYSA-M methoxyacetate Chemical compound COCC([O-])=O RMIODHQZRUFFFF-UHFFFAOYSA-M 0.000 description 1
- 229940057867 methyl lactate Drugs 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- XKBGEWXEAPTVCK-UHFFFAOYSA-M methyltrioctylammonium chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC XKBGEWXEAPTVCK-UHFFFAOYSA-M 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
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- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- MJCJUDJQDGGKOX-UHFFFAOYSA-N n-dodecyldodecan-1-amine Chemical compound CCCCCCCCCCCCNCCCCCCCCCCCC MJCJUDJQDGGKOX-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000002832 nitroso derivatives Chemical class 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 229910052755 nonmetal Chemical class 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-O octylazanium Chemical compound CCCCCCCC[NH3+] IOQPZZOEVPZRBK-UHFFFAOYSA-O 0.000 description 1
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- 239000013034 phenoxy resin Substances 0.000 description 1
- 229920006287 phenoxy resin Polymers 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 239000010665 pine oil Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- KYKNRZGSIGMXFH-ZVGUSBNCSA-M potassium bitartrate Chemical compound [K+].OC(=O)[C@H](O)[C@@H](O)C([O-])=O KYKNRZGSIGMXFH-ZVGUSBNCSA-M 0.000 description 1
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 1
- 239000001472 potassium tartrate Substances 0.000 description 1
- 229940111695 potassium tartrate Drugs 0.000 description 1
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- 238000001556 precipitation Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 150000004053 quinones Chemical class 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
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- 239000010980 sapphire Substances 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 229940079827 sodium hydrogen sulfite Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- HLJWMCUZPYEUDI-UHFFFAOYSA-L sodium hyponitrite Chemical compound [Na+].[Na+].[O-]N=N[O-] HLJWMCUZPYEUDI-UHFFFAOYSA-L 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000001433 sodium tartrate Substances 0.000 description 1
- 229960002167 sodium tartrate Drugs 0.000 description 1
- 235000011004 sodium tartrates Nutrition 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
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- HDFRDWFLWVCOGP-UHFFFAOYSA-M sulfanylformate Chemical compound [O-]C(S)=O HDFRDWFLWVCOGP-UHFFFAOYSA-M 0.000 description 1
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- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 125000001302 tertiary amino group Chemical group 0.000 description 1
- NQRYJNQNLNOLGT-UHFFFAOYSA-N tetrahydropyridine hydrochloride Natural products C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229950006389 thiodiglycol Drugs 0.000 description 1
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- 229930192474 thiophene Natural products 0.000 description 1
- IBBLKSWSCDAPIF-UHFFFAOYSA-N thiopyran Chemical compound S1C=CC=C=C1 IBBLKSWSCDAPIF-UHFFFAOYSA-N 0.000 description 1
- SWZDQOUHBYYPJD-UHFFFAOYSA-N tridodecylamine Chemical compound CCCCCCCCCCCCN(CCCCCCCCCCCC)CCCCCCCCCCCC SWZDQOUHBYYPJD-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical class [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 description 1
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Images
Landscapes
- Non-Insulated Conductors (AREA)
- Manufacturing Of Electric Cables (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
- Powder Metallurgy (AREA)
- Manufacturing Of Printed Wiring (AREA)
Description
本発明で製造した金属銅焼結膜は、電極、配線パターン又は塗膜等に用いることができる。具体的には、金属銅焼結膜の体積抵抗値は20μΩ・cm以下のものが得られ、また、膜厚の薄い焼結膜とすることができることから、プリンタブルエレクトロニクス分野でのプリント配線基板等の微細電極及び回路配線パターンに特に有用である。
(アミン価の測定方法)
ゼラチン又は高分子分散剤5g、ブロモクレゾールグリーンエタノール溶液数滴を300mLのエタノールと純水の混合溶媒に溶解させ、ファクター(補正係数)を算出した0.1M HClエタノール溶液を添加し、ブロモクレゾールグリーン指示薬の黄色が30秒続いた時の0.1M HClエタノール溶液の滴定量からアミン価を算出する。
(酸価の測定方法)
ゼラチン又は高分子分散剤5g、フェノールフタレイン液数滴を300mLの純水に溶解させ、ファクター(補正係数)を算出した0.1M KOHエタノール溶液を添加する。フェノールフタレイン指示薬の薄紅色が30秒続いた時の0.1M KOHエタノール溶液の滴定量から酸価を算出する。
(1)窒素がドナー原子である錯化剤としては、(a)アミン類(例えば、ブチルアミン、エチルアミン、プロピルアミン、エチレンジアミン等の1級アミン類、ジブチルアミン、ジエチルアミン、ジプロピルアミン、及び、ピペリジン、ピロリジン等のイミン類等の2級アミン類、トリブチルアミン、トリエチルアミン、トリプロピルアミン等の3級アミン類、ジエチレントリアミン、トリエチレンテトラミンの1分子内に1〜3級アミンを2種以上有するもの等)、(b)窒素含有複素環式化合物(例えば、イミダゾール、ピリジン、ビピリジン等)、(c)ニトリル類(例えば、アセトニトリル、ベンゾニトリル等)及びシアン化合物、(d)アンモニア及びアンモニウム化合物(例えば、塩化アンモニウム、硫酸アンモニウム等)、(e)オキシム類等が挙げられる。
(2)酸素がドナー原子である錯化剤としては、(a)カルボン酸類(例えば、クエン酸、リンゴ酸、酒石酸、乳酸等のオキシカルボン酸類、酢酸、ギ酸等のモノカルボン酸類、シュウ酸、マロン酸等のジカルボン酸類、安息香酸等の芳香族カルボン酸類等)、(b)ケトン類(例えば、アセトン等のモノケトン類、アセチルアセトン、ベンゾイルアセトン等のジケトン類等)、(c)アルデヒド類、(d)アルコール類(1価アルコール類、グリコール類、グリセリン類等)、(e)キノン類、(f)エーテル類、(g)リン酸(正リン酸)及びリン酸系化合物(例えば、ヘキサメタリン酸、ピロリン酸、亜リン酸、次亜リン酸等)、(h)スルホン酸又はスルホン酸系化合物等が挙げられる。
(3)硫黄がドナー原子である錯化剤としては、(a)脂肪族チオール類(例えば、メチルメルカプタン、エチルメルカプタン、プロピルメルカプタン、イソプロピルメルカプタン、n−ブチルメルカプタン、アリルメルカプタン、ジメチルメルカプタン等)、(b)脂環式チオール類(シクロヘキシルチオール等)、(c)芳香族チオール類(チオフェノール等)、(d)チオケトン類、(e)チオエーテル類、(f)ポリチオール類、(g)チオ炭酸類(トリチオ炭酸類)、(h)硫黄含有複素環式化合物(例えば、ジチオール、チオフェン、チオピラン等)、(i)チオシアナート類及びイソチオシアナート類、(j)無機硫黄化合物(例えば、硫化ナトリウム、硫化カリウム、硫化水素等)等が挙げられる。
(4)2種以上のドナー原子を有する錯化剤としては、(a)アミノ酸類(ドナー原子が窒素及び酸素:例えば、グリシン、アラニン等の中性アミノ酸類、ヒスチジン、アルギニン等の塩基性アミノ酸類、アスパラギン酸、グルタミン酸等の酸性アミノ酸類)、(b)アミノポリカルボン酸類(ドナー原子が窒素及び酸素:例えば、エチレンジアミンテトラ酢酸(EDTA)、ニトリロトリ酢酸(NTA)、イミノジ酢酸(IDA)、エチレンジアミンジ酢酸(EDDA)、エチレングリコールジエチルエーテルジアミンテトラ酢酸(GEDA)等)、(c)アルカノールアミン類(ドナー原子が窒素及び酸素:例えば、エタノールアミン、ジエタノールアミン、トリエタノールアミン等)、(d)ニトロソ化合物及びニトロシル化合物(ドナー原子が窒素及び酸素)、(e)メルカプトカルボン酸類(ドナーが硫黄及び酸素:例えば、メルカプトプロピオン酸、メルカプト酢酸、チオジプロピオン酸、メルカプトコハク酸、ジメルカプトコハク酸、チオ酢酸、チオジグリコール酸等)、(f)チオグリコール類(ドナーが硫黄及び酸素:例えば、メルカプトエタノール、チオジエチレングリコール等)、(g)チオン酸類(ドナーが硫黄及び酸素)、(h)チオ炭酸類(ドナー原子が硫黄及び酸素:例えば、モノチオ炭酸、ジチオ炭酸、チオン炭酸)、(i)アミノチオール類(ドナーが硫黄及び窒素:アミノエチルメルカプタン、チオジエチルアミン等)、(j)チオアミド類(ドナー原子が硫黄及び窒素:例えば、チオホルムアミド等)、(k)チオ尿素類(ドナー原子が硫黄及び窒素)、(l)チアゾール類(ドナー原子が硫黄及び窒素:例えばチアゾール、ベンゾチアゾール等)、(m)含硫黄アミノ酸類(ドナーが硫黄、窒素及び酸素:システイン、メチオニン等)等が挙げられる。
(5)上記の化合物の塩や誘導体としては、例えば、クエン酸トリナトリウム、酒石酸ナトリウム・カリウム、次亜リン酸ナトリウム、エチレンジアミンテトラ酢酸ジナトリウム等のそれらのアルカリ金属塩や、カルボン酸、リン酸、スルホン酸等のエステル等が挙げられる。
このような錯化剤のうち、少なくとも1種を用いることができる。錯化剤の使用量は錯化剤の種類により最適量が異なるため、その種類に応じて適宜設定する。錯化剤の使用量を少なくすると、金属銅微粒子の一次粒子を小さくすることができ、使用量を多くすると、一次粒子を大きくすることができる。
工業用酸化第二銅(エヌシーテック社製N−120)24g、保護コロイドとしてゼラチン(アミン価23、酸価29、アミン価−酸価=−6)2.8gを150ミリリットルの純水に添加、混合し、15%のアンモニア水を用いて混合液のpHを11に調整した後、20分かけて室温から90℃まで昇温した。昇温後、撹拌しながら、錯化剤として1%の3−メルカプトプロピオン酸溶液0.24gと、80%のヒドラジン一水和物10gを150ミリリットルの純水に混合した液を添加し、1時間かけて酸化銅と反応させ、ゼラチンで被覆した銅微粒子を生成させた。その後、濾液比導電率が100μS/cm以下になるまで濾過洗浄し、窒素ガスの雰囲気で60℃の温度で10時間かけて乾燥し、ゼラチンで被覆した金属銅粒子を得た。
上記方法にて合成したゼラチンで被覆した平均粒子径50nmの金属銅粒子20gと高分子分散剤を溶解した有機溶媒(用いた高分子分散剤の種類、その酸価、アミン価、(アミン価−酸価)、添加量と有機溶媒の種類を表1に示す。)20gを混合・懸濁し、ペイントシェーカーにて1時間分散させ、金属銅分散液(試料A、B)を得た。
なお、ゼラチン、高分子分散剤の酸価、アミン価は前記のJIS K 7700あるいはASTM D2074に準拠した方法で測定した。
前記の金属銅分散液(試料A、B)をポリイミドフィルム(東レデュポン株式会社製 カプトン(登録商標)フィルム 300Vタイプ 75μm厚)にバーコーター#3で塗布し、金属銅含有膜を作製した。その後、(株)ニッシン製 MicroLabo-PSを用いて、プラズマ処理を次のように行い、金属銅焼結膜を得た。
まず、金属銅含有膜をプラズマ装置内の100℃又は150℃の所定温度に加熱したステージに置き、180秒又は30秒の所定時間加熱した。その後、装置内を60秒減圧し、3%H2−Heガスを装置内に30秒充填し、プラズマ照射を表2に記載の所定時間行った。プラズマ処理後、90秒、N2ガスをパージすることで冷却し、金属銅焼結膜を得た。
前記の試料Aを100ppm−O2−N2混合ガス気流中、200℃で予備加熱を行い、3%水素含有窒素ガス気流中250℃で行った。加熱には光洋サーモシステム社 電気管状炉(KTF085N)を使用し、昇温および降温は10℃/分とし、加熱時間は各工程とも1時間とした。
得られた金属銅焼結膜の表面と断面に白金を蒸着した後、走査型電子顕微鏡を用いて観察し、膜厚を測定した。また、金属銅焼結膜の体積抵抗値の測定には、ロレスタ−GP型低抵抗率計(三菱化学社製)を用いた。結果を表2、3に示す。本金属銅含有膜をプラズマ処理することで、加熱焼成法と同等に抵抗値の低い良好な金属銅焼結膜が得られた。
Claims (5)
- 少なくとも、アミン価と酸価の差(アミン価−酸価)が−50〜0であるゼラチンを粒子表面に有する金属銅粒子と、高分子分散剤と有機溶媒とを含む分散液であって、前記の金属銅粒子100重量部に対してゼラチンが0.1〜15重量部含まれ、高分子分散剤が0.1〜20重量部含まれている分散液を用いて基材の表面に金属銅含有膜を形成する工程(a)、
次いで、その金属銅含有膜をプラズマ発生装置に入れ、大気中で180℃以下に加熱し、次いで、低圧又は真空条件下で180℃以下に加熱し、引き続き、ガスを充填しプラズマ照射して金属銅含有膜の全領域又は一部領域にプラズマ処理する工程(b)を含む金属銅焼結膜の製造方法。 - 前記の高分子分散剤は、アミン価と酸価の差(アミン価−酸価)が0〜50である、請求項1に記載の金属銅焼結膜の製造方法。
- 有機溶媒が、炭化水素、アルコール、ケトン、エステル、エーテル、グリコール、グリコールエーテル、グリコールエステルから選ばれる少なくとも1種である請求項1又は2に記載の金属銅焼結膜の製造方法。
- メジアン径が1〜200nmである金属銅粒子を用いる請求項1〜3のいずれか一項に記載の金属銅焼結膜の製造方法。
- 製造された金属銅焼結膜の体積抵抗値が20μΩ・cm以下である、請求項1〜4のいずれか一項に記載の金属銅焼結膜の製造方法。
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