JP2008069374A - 金属ナノ粒子分散体および金属被膜 - Google Patents
金属ナノ粒子分散体および金属被膜 Download PDFInfo
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- JP2008069374A JP2008069374A JP2006246379A JP2006246379A JP2008069374A JP 2008069374 A JP2008069374 A JP 2008069374A JP 2006246379 A JP2006246379 A JP 2006246379A JP 2006246379 A JP2006246379 A JP 2006246379A JP 2008069374 A JP2008069374 A JP 2008069374A
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- Prior art keywords
- metal
- acid
- nanoparticle dispersion
- substrate
- metal nanoparticle
- Prior art date
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- 239000006185 dispersion Substances 0.000 title claims abstract description 70
- 239000002105 nanoparticle Substances 0.000 title abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 58
- 239000002184 metal Substances 0.000 claims abstract description 58
- 239000000758 substrate Substances 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 23
- -1 organic acid salt Chemical class 0.000 claims abstract description 18
- 229910052738 indium Inorganic materials 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 12
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- 229910052718 tin Inorganic materials 0.000 claims abstract description 12
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 12
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 12
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 10
- 239000002082 metal nanoparticle Substances 0.000 claims description 73
- 239000010949 copper Substances 0.000 claims description 39
- 229910052802 copper Inorganic materials 0.000 claims description 35
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 34
- 238000010304 firing Methods 0.000 claims description 32
- 150000007524 organic acids Chemical class 0.000 claims description 12
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 2
- 150000001735 carboxylic acids Chemical group 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 239000012298 atmosphere Substances 0.000 description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 239000011248 coating agent Substances 0.000 description 19
- 238000000576 coating method Methods 0.000 description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 16
- 230000001590 oxidative effect Effects 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 238000000034 method Methods 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- 239000010419 fine particle Substances 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 9
- 239000011572 manganese Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 239000011701 zinc Substances 0.000 description 9
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 238000011282 treatment Methods 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 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
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 6
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 6
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 description 6
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 6
- ZDPHROOEEOARMN-UHFFFAOYSA-N undecanoic acid Chemical compound CCCCCCCCCCC(O)=O ZDPHROOEEOARMN-UHFFFAOYSA-N 0.000 description 6
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 5
- NUMHJBONQMZPBW-UHFFFAOYSA-K bis(2-ethylhexanoyloxy)bismuthanyl 2-ethylhexanoate Chemical compound [Bi+3].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O NUMHJBONQMZPBW-UHFFFAOYSA-K 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 5
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 4
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 4
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 4
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 4
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- IIYFAKIEWZDVMP-UHFFFAOYSA-N tridecane Chemical compound CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 description 4
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- FJDUDHYHRVPMJZ-UHFFFAOYSA-N nonan-1-amine Chemical compound CCCCCCCCCN FJDUDHYHRVPMJZ-UHFFFAOYSA-N 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- QFKMMXYLAPZKIB-UHFFFAOYSA-N undecan-1-amine Chemical compound CCCCCCCCCCCN QFKMMXYLAPZKIB-UHFFFAOYSA-N 0.000 description 3
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 2
- JPZYXGPCHFZBHO-UHFFFAOYSA-N 1-aminopentadecane Chemical compound CCCCCCCCCCCCCCCN JPZYXGPCHFZBHO-UHFFFAOYSA-N 0.000 description 2
- GYSCBCSGKXNZRH-UHFFFAOYSA-N 1-benzothiophene-2-carboxamide Chemical compound C1=CC=C2SC(C(=O)N)=CC2=C1 GYSCBCSGKXNZRH-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- FHRAKXJVEOBCBQ-UHFFFAOYSA-L 2-ethylhexanoate;manganese(2+) Chemical compound [Mn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O FHRAKXJVEOBCBQ-UHFFFAOYSA-L 0.000 description 2
- KMZHTRWVLZTASP-UHFFFAOYSA-N 2-ethylhexanoic acid oxygen(2-) zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4].C(C)C(C(=O)O)CCCC KMZHTRWVLZTASP-UHFFFAOYSA-N 0.000 description 2
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 description 2
- 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
- AWQSAIIDOMEEOD-UHFFFAOYSA-N 5,5-Dimethyl-4-(3-oxobutyl)dihydro-2(3H)-furanone Chemical compound CC(=O)CCC1CC(=O)OC1(C)C AWQSAIIDOMEEOD-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 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
- 239000005711 Benzoic acid Substances 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- GHVNFZFCNZKVNT-UHFFFAOYSA-N Decanoic acid Natural products CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- 229910001111 Fine metal Inorganic materials 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
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- 239000002253 acid Substances 0.000 description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- 235000010233 benzoic acid Nutrition 0.000 description 2
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 description 2
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
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- 150000002736 metal compounds Chemical class 0.000 description 2
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- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
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- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
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- 238000003756 stirring Methods 0.000 description 2
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- 229940116411 terpineol Drugs 0.000 description 2
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 2
- ABVVEAHYODGCLZ-UHFFFAOYSA-N tridecan-1-amine Chemical compound CCCCCCCCCCCCCN ABVVEAHYODGCLZ-UHFFFAOYSA-N 0.000 description 2
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- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 description 1
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 1
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- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- GMOGUOKCSWHKPY-UHFFFAOYSA-M 2-ethylhexanoate iron(3+) Chemical compound [Fe+3].CCCCC(CC)C([O-])=O GMOGUOKCSWHKPY-UHFFFAOYSA-M 0.000 description 1
- YKJSOAKPHMIDLP-UHFFFAOYSA-J 2-ethylhexanoate;molybdenum(4+) Chemical compound [Mo+4].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O YKJSOAKPHMIDLP-UHFFFAOYSA-J 0.000 description 1
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- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 1
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- 229910001656 zinc mineral Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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Abstract
【解決手段】 平均粒子径が1〜100nmである金属ナノ粒子と、Bi、Mo、Mn、Fe、Zn、In、Sn、Zr、LaおよびCeから選ばれる少なくとも1種の金属とを、好ましくは有機酸塩の形態で含有する金属ナノ粒子分散体。
【選択図】 なし
Description
上記のようにして得られた金属ナノ粒子分散体を、冷却、例えば、5℃以下にまで冷却した後、再度メンブランフィルターなどによりろ過することにより、あるいは、さらに、このろ過により得られるろ過液中の溶媒を減圧除去した後、再度上記溶媒に分散させることにより、分散体中の不純物を除去できるとともに、金属ナノ粒子の含有量を10〜80質量%の範囲に、また、分散体中の金属の質量(M)と窒素の質量(N)との比(M/N)を5/1〜40/1の範囲に調整することができる。つまり、分散体中の金属ナノ粒子含有量および比(M/N)を測定しながら、上記操作を適宜選択し、あるいは繰り返すことにより、金属ナノ粒子分散体中の金属ナノ粒子含有量を10〜80質量%の範囲に、また比(M/N)を5/1〜40/1の範囲に調整することができる。比(M/N)が5/1未満では、この金属ナノ粒子分散体を焼成して得られる金属被膜の導電性が低下し、一方、40/1を超えると、金属ナノ粒子が分散体中で安定した分散状態を維持できなくなるか、あるいは分散体の粘性が高まり、配線などの微細な金属被膜を形成するのが困難となる傾向にある。この傾向は、銅ナノ粒子分散体の場合に特に顕著である。
<条件>
加速電圧:15kV
ビームサイズ:100μmΦ
試料電流:0.1μA
また、金属ナノ粒子の含有量については、熱重量・示差熱同時分析装置(TG−DTA)(マックサイエンス社製、TG−DTA2000S)を用い、下記条件下に、分散体を室温から800℃まで昇温した際の質量変化から算出した。
<条件>
空気供給量:50mL/min
サンプリング間隔:1.0秒
昇温速度:10.0deg/min
本発明の金属ナノ粒子分散体を基板に塗布した後、焼成することにより、基板への密着性、あるいは、さらに導電性に優れた金属被膜を形成することができる。
(実施例1)
酢酸銅一水和物(和光純薬工業株式会社製)31.4gとオクチルアミン(和光純薬工業株式会社製)203.4gを40℃にて20分攪拌混合した後、20%水素化ホウ素ナトリウム水溶液29.8gを徐々に添加することにより還元処理を実施した。還元処理後の溶液を攪拌しながらアセトンを1000g添加し、しばらく放置後、ろ過により銅および有機物からなる沈殿物を分離した。
(実施例2〜10)
実施例1における2−エチルヘキサン酸ビスマス(III)2−エチルヘキサン酸溶液(Bi:25%)の代わりに、2−エチルヘキサン酸モリブデン、2−エチルヘキサン酸マンガン(II)ミネラルスピリット溶液(Mn:8%)、2−エチルヘキサン酸鉄(III)ミネラルスピリット溶液(Fe:6%)、2−エチルヘキサン酸亜鉛ミネラルスピリット溶液(Zn:15%)、2−エチルヘキサン酸インジウム(III)トルエン溶液(In:5%)、2−エチルヘキサン酸すず(II)、2−エチルヘキサン酸酸化ジルコニウム(IV)ミネラルスピリット溶液(Zr:12%)、2−エチルヘキサン酸ランタントルエン溶液(La:7%)、2−エチルヘキサン酸セリウム(III)2−エチルヘキサン酸溶液(Ce:12%)を銅微粒子ペーストに加えた以外は実施例1と同様にして、表1に示す金属含有量の分散体(2)〜(10)を得た。なお、いずれの分散体も銅の含有量は30%であった。
(実施例11〜13)
銅微粒子ペーストに2−エチルヘキサン酸ビスマス(III)2−エチルヘキサン酸溶液を実施例1より多く加えた以外は実施例1と同様にして、銅を30%含有し、100部の銅に対して21.7部、11.2部および8.5部のビスマスを含有する銅ナノ粒子分散体(11)、(12)および(13)を得た。
(実施例14)
銅微粒子ペーストに2−エチルヘキサン酸ビスマス(III)2−エチルヘキサン酸溶液を実施例1より少なく加えた以外は実施例1と同様にして、銅を30%含有し、100部の銅に対して0.23部のビスマスを含有する銅ナノ粒子分散体(14)を得た。
(比較例1)
銅微粒子ペーストに2−エチルヘキサン酸ビスマス(III)2−エチルヘキサン酸溶液をくわえなかった以外は実施例1と同様にして、銅を30%含有する銅ナノ粒子分散体(比較1)を得た。
(実施例15)
実施例1〜14および比較例1で得られた銅ナノ粒子分散体(1)〜(14)および(比較1)を、それぞれ1cm×3cmの面積で、ガラス基板上に塗布した後、ガラス基板を焼成炉に入れた。焼成炉内に5体積%の水素(残りの95体積%は窒素)を流通させながら室温から300℃まで1時間で昇温した。温度が300℃に到達してから0.5時間保持し還元性雰囲気中での焼成を行った。続いて、温度を300℃に維持した状態で、流通させるガスを空気に切り替えて0.5時間保持し酸化性雰囲気中での焼成を行った。その後、温度を300℃に維持した状態で、流通させるガスを5体積%の水素(残りの95体積%は窒素)に切り替えて0.5時間保持し還元性雰囲気中での焼成を行い、銅被膜を得た。銅被膜の膜厚は、いずれも0.5μmであった。
Claims (6)
- 平均粒子径が1〜100nmである金属ナノ粒子と、Bi、Mo、Mn、Fe、Zn、In、Sn、Zr、LaおよびCeから選ばれる少なくとも1種の金属とを含有することを特徴とする金属ナノ粒子分散体。
- Bi、Mo、Mn、Fe、Zn、In、Sn、Zr、LaおよびCeから選ばれる少なくとも1種の金属が有機酸塩の形態で存在する請求項1に記載の金属ナノ粒子分散体。
- 有機酸塩を構成する有機酸が一般式:RCOOH(R=炭素数7〜11の炭化水素)で表されるカルボン酸である請求項2に記載の金属ナノ粒子分散体。
- 金属ナノ粒子の含有量(分散体の質量基準)が10〜80質量%であり、Bi、Mo、Mn、Fe、Zn、In、Sn、Zr、LaおよびCeから選ばれる少なくとも1種の金属の含有量は、金属ナノ粒子の金属100質量部に対して0.1〜20質量部である請求項1ないし3のいずれかに記載の金属ナノ粒子分散体。
- 金属ナノ粒子の金属が銀および/または銅である請求項1ないし4のいずれかに記載の金属ナノ粒子分散体。
- 請求項1ないし5のいずれかの金属ナノ粒子分散体を基板に塗布した後、100〜600℃の温度で焼成して得られる金属被膜。
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PCT/JP2007/067719 WO2008032733A1 (fr) | 2006-09-12 | 2007-09-12 | Dispersion de nanoparticules métalliques, film de revêtement métallique et procédé pour la production de nanoparticules métalliques |
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JP2010013721A (ja) * | 2008-07-07 | 2010-01-21 | Nippon Shokubai Co Ltd | 成膜性に優れた金属ナノ粒子分散体の製造方法および金属被膜 |
JP2010269290A (ja) * | 2009-05-25 | 2010-12-02 | Tanaka Kikinzoku Kogyo Kk | 金属ナノ粒子を含有するコロイド溶液 |
JP2012094510A (ja) * | 2010-10-01 | 2012-05-17 | Furukawa Electric Co Ltd:The | 金属構造体の製造方法、および金属構造体、ならびに金属部品 |
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WO2013018777A1 (ja) * | 2011-08-03 | 2013-02-07 | 日立化成工業株式会社 | 組成物セット、導電性基板及びその製造方法並びに導電性接着材組成物 |
JP2013216931A (ja) * | 2012-04-05 | 2013-10-24 | Ulvac Japan Ltd | 金属微粒子分散液 |
JP2015056238A (ja) * | 2013-09-10 | 2015-03-23 | 株式会社東芝 | 金属粒子ペースト、これを用いた硬化物、および半導体装置 |
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JP2016167379A (ja) * | 2015-03-09 | 2016-09-15 | 株式会社東芝 | 導電ペースト、その乾燥物、及び複合体 |
JP2017162824A (ja) * | 2017-04-17 | 2017-09-14 | 株式会社東芝 | 金属粒子ペースト、これを用いた硬化物、および半導体装置 |
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CN103733277A (zh) * | 2011-08-03 | 2014-04-16 | 日立化成株式会社 | 组合物套剂、导电性基板及其制造方法以及导电性粘接材料组合物 |
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WO2013018777A1 (ja) * | 2011-08-03 | 2013-02-07 | 日立化成工業株式会社 | 組成物セット、導電性基板及びその製造方法並びに導電性接着材組成物 |
JP2013216931A (ja) * | 2012-04-05 | 2013-10-24 | Ulvac Japan Ltd | 金属微粒子分散液 |
JP2015056238A (ja) * | 2013-09-10 | 2015-03-23 | 株式会社東芝 | 金属粒子ペースト、これを用いた硬化物、および半導体装置 |
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JP2016167379A (ja) * | 2015-03-09 | 2016-09-15 | 株式会社東芝 | 導電ペースト、その乾燥物、及び複合体 |
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