TWI351982B - - Google Patents
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- Publication number
- TWI351982B TWI351982B TW093127010A TW93127010A TWI351982B TW I351982 B TWI351982 B TW I351982B TW 093127010 A TW093127010 A TW 093127010A TW 93127010 A TW93127010 A TW 93127010A TW I351982 B TWI351982 B TW I351982B
- Authority
- TW
- Taiwan
- Prior art keywords
- metal
- acid
- metal nanoparticle
- dispersion
- nanoparticle
- Prior art date
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- 239000002082 metal nanoparticle Substances 0.000 claims description 69
- 229910052751 metal Inorganic materials 0.000 claims description 57
- 239000002184 metal Substances 0.000 claims description 57
- 239000006185 dispersion Substances 0.000 claims description 42
- -1 amine metal complex compound Chemical class 0.000 claims description 26
- 238000004519 manufacturing process Methods 0.000 claims description 23
- 150000001412 amines Chemical class 0.000 claims description 21
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 21
- 229930195729 fatty acid Natural products 0.000 claims description 21
- 239000000194 fatty acid Substances 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 17
- 150000004665 fatty acids Chemical class 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 238000010304 firing Methods 0.000 claims description 14
- 150000002902 organometallic compounds Chemical class 0.000 claims description 13
- 239000000758 substrate Substances 0.000 claims description 11
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 10
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 10
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 10
- 239000005642 Oleic acid Substances 0.000 claims description 10
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 10
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 10
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 10
- 235000021313 oleic acid Nutrition 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 9
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002105 nanoparticle Substances 0.000 claims description 9
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 8
- 239000012454 non-polar solvent Substances 0.000 claims description 8
- WJYIASZWHGOTOU-UHFFFAOYSA-N Heptylamine Chemical compound CCCCCCCN WJYIASZWHGOTOU-UHFFFAOYSA-N 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 150000002739 metals Chemical class 0.000 claims description 6
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 6
- 239000002798 polar solvent Substances 0.000 claims description 6
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims description 5
- 235000020661 alpha-linolenic acid Nutrition 0.000 claims description 5
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 5
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 claims description 5
- 229960004488 linolenic acid Drugs 0.000 claims description 5
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims description 4
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 claims description 4
- 239000005639 Lauric acid Substances 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 229910000510 noble metal Inorganic materials 0.000 claims description 4
- 229960002446 octanoic acid Drugs 0.000 claims description 4
- ZDPHROOEEOARMN-UHFFFAOYSA-N undecanoic acid Chemical compound CCCCCCCCCCC(O)=O ZDPHROOEEOARMN-UHFFFAOYSA-N 0.000 claims description 4
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 claims description 3
- LTHNHFOGQMKPOV-UHFFFAOYSA-N 2-ethylhexan-1-amine Chemical compound CCCCC(CC)CN LTHNHFOGQMKPOV-UHFFFAOYSA-N 0.000 claims description 3
- 235000003441 saturated fatty acids Nutrition 0.000 claims description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims description 3
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims description 3
- UNBMPKNTYKDYCG-UHFFFAOYSA-N 4-methylpentan-2-amine Chemical compound CC(C)CC(C)N UNBMPKNTYKDYCG-UHFFFAOYSA-N 0.000 claims 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 claims description 2
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims description 2
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052723 transition metal Inorganic materials 0.000 claims description 2
- 150000003624 transition metals Chemical class 0.000 claims description 2
- ABVVEAHYODGCLZ-UHFFFAOYSA-N tridecan-1-amine Chemical compound CCCCCCCCCCCCCN ABVVEAHYODGCLZ-UHFFFAOYSA-N 0.000 claims description 2
- QFKMMXYLAPZKIB-UHFFFAOYSA-N undecan-1-amine Chemical compound CCCCCCCCCCCN QFKMMXYLAPZKIB-UHFFFAOYSA-N 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims 2
- 150000002736 metal compounds Chemical class 0.000 claims 1
- 239000010408 film Substances 0.000 description 23
- 239000010931 gold Substances 0.000 description 20
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 11
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 150000003973 alkyl amines Chemical class 0.000 description 9
- 238000005755 formation reaction Methods 0.000 description 9
- 229960002969 oleic acid Drugs 0.000 description 9
- 229910052709 silver Inorganic materials 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- PVYPHUYXKVVURH-UHFFFAOYSA-N boron;2-methylpropan-2-amine Chemical compound [B].CC(C)(C)N PVYPHUYXKVVURH-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 229910052737 gold Inorganic materials 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical compound [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- MNWFXJYAOYHMED-UHFFFAOYSA-N heptanoic acid Chemical compound CCCCCCC(O)=O MNWFXJYAOYHMED-UHFFFAOYSA-N 0.000 description 4
- 239000002923 metal particle Substances 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- YRSQDSCQMOUOKO-KVVVOXFISA-M silver;(z)-octadec-9-enoate Chemical compound [Ag+].CCCCCCCC\C=C/CCCCCCCC([O-])=O YRSQDSCQMOUOKO-KVVVOXFISA-M 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 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 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 3
- 235000020778 linoleic acid Nutrition 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- DIOQZVSQGTUSAI-UHFFFAOYSA-N n-butylhexane Natural products CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 2
- VZXTWGWHSMCWGA-UHFFFAOYSA-N 1,3,5-triazine-2,4-diamine Chemical compound NC1=NC=NC(N)=N1 VZXTWGWHSMCWGA-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- DMEGYFMYUHOHGS-UHFFFAOYSA-N cycloheptane Chemical compound C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 description 2
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 150000004671 saturated fatty acids Chemical class 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000003760 tallow Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- IIYFAKIEWZDVMP-UHFFFAOYSA-N tridecane Chemical compound CCCCCCCCCCCCC IIYFAKIEWZDVMP-UHFFFAOYSA-N 0.000 description 2
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
- XKZKQTCECFWKBN-VOTSOKGWSA-N (e)-dec-4-enoic acid Chemical compound CCCCC\C=C\CCC(O)=O XKZKQTCECFWKBN-VOTSOKGWSA-N 0.000 description 1
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- GYSCBCSGKXNZRH-UHFFFAOYSA-N 1-benzothiophene-2-carboxamide Chemical compound C1=CC=C2SC(C(=O)N)=CC2=C1 GYSCBCSGKXNZRH-UHFFFAOYSA-N 0.000 description 1
- WXBXVVIUZANZAU-UHFFFAOYSA-N 2E-decenoic acid Natural products CCCCCCCC=CC(O)=O WXBXVVIUZANZAU-UHFFFAOYSA-N 0.000 description 1
- QBVCURPNLGSYTD-UHFFFAOYSA-N C(C)C(CN)CCCC.C(CCCCCCCCCCC)N Chemical compound C(C)C(CN)CCCC.C(CCCCCCCCCCC)N QBVCURPNLGSYTD-UHFFFAOYSA-N 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 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
- 125000002029 aromatic hydrocarbon group Chemical group 0.000 description 1
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 1
- 229910010277 boron hydride Inorganic materials 0.000 description 1
- QFLVHLKRNQNMGT-UHFFFAOYSA-N boron;methanamine Chemical compound [B].NC QFLVHLKRNQNMGT-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- WJTCGQSWYFHTAC-UHFFFAOYSA-N cyclooctane Chemical compound C1CCCCCCC1 WJTCGQSWYFHTAC-UHFFFAOYSA-N 0.000 description 1
- 239000004914 cyclooctane Substances 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
- KWKXNDCHNDYVRT-UHFFFAOYSA-N dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1 KWKXNDCHNDYVRT-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- SEPFQHJECFKHGD-UHFFFAOYSA-N henicos-2-ene Chemical group CCCCCCCCCCCCCCCCCCC=CC SEPFQHJECFKHGD-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229940049918 linoleate Drugs 0.000 description 1
- 229960004232 linoleic acid Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 description 1
- DBIJGSRXWPQTLH-UHFFFAOYSA-N n-butyloctan-1-amine Chemical compound CCCCCCCCNCCCC DBIJGSRXWPQTLH-UHFFFAOYSA-N 0.000 description 1
- HKUFIYBZNQSHQS-UHFFFAOYSA-N n-octadecyloctadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCCCNCCCCCCCCCCCCCCCCCC HKUFIYBZNQSHQS-UHFFFAOYSA-N 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- NTNWKDHZTDQSST-UHFFFAOYSA-N naphthalene-1,2-diamine Chemical compound C1=CC=CC2=C(N)C(N)=CC=C21 NTNWKDHZTDQSST-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- QTLNZGHUUPEBIK-UHFFFAOYSA-N octan-1-amine silver Chemical compound [Ag].C(CCCCCCC)N QTLNZGHUUPEBIK-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000412 polyarylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- WXBXVVIUZANZAU-CMDGGOBGSA-N trans-2-decenoic acid Chemical compound CCCCCCC\C=C\C(O)=O WXBXVVIUZANZAU-CMDGGOBGSA-N 0.000 description 1
- XKZKQTCECFWKBN-UHFFFAOYSA-N trans-4-decenoic acid Natural products CCCCCC=CCCC(O)=O XKZKQTCECFWKBN-UHFFFAOYSA-N 0.000 description 1
- FLTJDUOFAQWHDF-UHFFFAOYSA-N trimethyl pentane Natural products CCCCC(C)(C)C FLTJDUOFAQWHDF-UHFFFAOYSA-N 0.000 description 1
- VSRBKQFNFZQRBM-UHFFFAOYSA-N tuaminoheptane Chemical compound CCCCCC(C)N VSRBKQFNFZQRBM-UHFFFAOYSA-N 0.000 description 1
- 229960003986 tuaminoheptane Drugs 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
- B01J13/0043—Preparation of sols containing elemental metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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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
- 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
- B22F1/102—Metallic powder coated with organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
-
- 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
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/288—Deposition of conductive or insulating materials for electrodes conducting electric current from a liquid, e.g. electrolytic deposition
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
- H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
- H01L23/498—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers
- H01L23/49866—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials
- H01L23/49883—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials the conductive materials containing organic materials or pastes, e.g. for thick films
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
- H05K1/097—Inks comprising nanoparticles and specially adapted for being sintered at low temperature
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
- C09K23/16—Amines or polyamines
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12181—Composite powder [e.g., coated, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Computer Hardware Design (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Electrodes Of Semiconductors (AREA)
Description
1351982 (1) 九、發明說明 【發明所屬之技術領域】 本發明係有關金屬奈米粒子及 粒子分散液及其製造方法、以及金 成方法者。 【先前技術】 先前技術,做爲lOOnm以下 導電性金屬奈米粒子之製造方法者 金屬或銅離子後,取得貴金屬或銅 文獻1)。又,公知之至少含有1 金屬膠質液者(如:專利文獻2 ) 安定之金屬膠質者均爲不易者。 〔專利文獻1〕特開平1 1 ~ 3 利範圍) 〔專利文獻2〕特開平2002-專利範圍) 用於電氣電子工業領域之配線 低溫化者。又,做爲金屬奈米粒子 材者爲使用玻璃、聚亞醯等多種類 最近針對搭載TFT (薄膜電晶體) 金屬奈米粒子者,成膜溫度被要求 基材之性質而異,一般低者被要求: 此狀況中,被強烈要求於低溫 其製造方法’金屬奈米 屬細線及金屬膜及其形 之金屬奈米粒子所成之 如公知者之藉由還原貴 膠質之方法(如:專利 個胺基與羧基之化合物 。惟,欲以高濃度製作 ]9 5 3 8號公報(申請專 -245854號公報(申請 形成法近年來積極進行 之塗佈、乾燥、燒成基 者,此等基材以外,於 於玻璃上之基板亦適用 低溫化。燒成溫度依其 5令200°C之燒成者。 燒成下,且,儘可能減 -5- (2) (2)1351982 少塗佈次數或成膜次數形成具有所期待厚度之配線者。因 此,即使低溫燒成仍可取得電阻率低之配線,同時被期待 取得金屬濃度高的分散金屬奈米粒子。先行技術,形成用 於此用途金屬奈米粒子所成之膜時,雖可實現低電阻,惟 ,務必爲溫燒成者,造成雖可低溫處理,卻塗佈次數變多 等問題。又,爲減少塗佈次數,即使以任意方法使塗佈液 之固形份濃度變濃,所取得液體仍呈不安定者,出現2次 凝聚,金屬粒子沈澱之問題。 【發明內容】 本發明課題係解決先行技術之問題點後,提供一種可 實現減少塗佈次數或成膜次數之金屬固形份高濃度化,同 時藉由低溫燒成處理亦可達成充份之導電率之安定的金屬 奈米粒子及其製造方法、金屬奈米粒子分散液及其製造方 法、以及利用此分散液取得金屬細線及金屬膜及其形成方 法者。 本發明金屬奈米粒子之特徵係於各金屬周圍附著做爲 分散劑之有機金屬化合物者。 此有機金屬化合物之特徵爲含有至少1種選自貴金屬 及過渡金屬之金屬、或至少2種此等金屬之合金者。 該有機金屬化合物之特徵係爲脂肪酸之有機金屬化合 物、胺基金屬配位化合物、脂肪酸之有機金屬化合物與胺 基之金屬配位化合物相互之混合物者。 該脂肪酸之特徵係至少]種選自具有直鏈或支鏈結構 -6- (3) (3)1351982 之C0〜C22之飽和脂肪酸及不飽和脂肪酸之脂肪酸者,如 :至少1種選自己酸 '庚酸、辛酸、壬酸 '癸酸、--酸 、月桂酸、十四酸、廿酸、廿二酸、2-乙基己酸、油酸 、亞油酸、亞麻酸之脂肪酸者。 該胺基之特徵爲具有直鏈或支鏈結構之C6-C, 3之脂 肪放胺者,如:至少1種選自己胺、庚胺、辛胺、癸胺、 月桂胺' 2_乙基己胺、1,3 —二甲基一η — 丁胺、I —胺 基十一烷、1一胺基十三烷之胺者。 本發明金屬奈米粒子之製造方法其特徵爲將該脂肪酸 之有機金屬化合物,該胺基金屬配位化合物、或此有機金 屬化合物與金屬配位化合物相互之混合物溶於非極性溶媒 ,此液中添加還原劑進行還原處理後,取得金屬奈米粒子 〇 該還原處理之特徵係藉由導入氫氣、一氧化碳氣體、 含氫氣體、或含一氧化碳氣體後進行者。 該製造方法中係進行還原處理後,更添加脫離子水, 攪拌後靜置之後,使雜質移行至極性溶媒,降低非極性溶 媒中雜質濃度者爲特徵者。 本發明金屬奈米粒子分散液之特徵係藉由該製造方法 後濃縮含取得金屬奈米粒子之分散液後,使金屬奈米粒子 藉由再分散後,使金屬奈米粒子之濃度範圍做成5wt%以 上' 90wt%以下者。 本發明金屬奈米粒子分散液之製造方法之特徵係藉由 該製造方法進行所取得含金屬奈米粒子之分散液後,使金 -7- (4) (4)1351982 屬奈米粒子進行再分散後’取得金屬奈米粒子爲5 wt %以 上90wt%以下之金屬奈米粒子分散液者* 該金屬奈米粒子之大小爲1nm以上’ ]〇〇nm以下者 〇 本發明金屬細線或金屬膜之形成方法其特徵係該含金 屬奈米粒子之分散液’藉由該製造方法取得含金屬奈米粒 子之分散液,將該分散液 '或藉由該製造方法取得之金屬 奈米粒子分散液塗佈於基材,乾燥燒成後形成具有導電性 之金屬細線或金屬膜者。 本發明金屬細線或金屬膜係藉由該形成方法取得之。 該燒成溫度以〗40〜300 °C爲其特徵,較佳者爲140〜 22 0〇C ° 本發明提供一種高濃度安定之金屬奈米粒子分散液者 ,因此,可減少其塗佈次數、成膜次數,同時,220 °C之 低溫下燒成處理仍可達成充份實用之導電率。 【實施方式】 〔發明實施之最佳形態〕 本發明金屬奈米粒子之構成金屬係由]種或2種以上 選自 Ag ' Au、Cu、Pt ' Pd ' W、Ni、Ta、In、Sn、Zn、 Cr ' Fe、Co、及Si等所成群之金屬、或至少2種金屬所 成之含金者,可依其目的、用途進行做適當選取之,此等 金屬中又以至少1種選自Ag'Au等貴金屬、及Cu之金 屬 '或由至少2種此等金屬所成之合金爲較佳者。亦可混 (5) (5)1351982 在源於還原劑之B、N、P等者。該金屬所構成之金屬奈 米粒子係於此金屬周圍具有附著做爲分散液之有機金屬化 合物結構者。此所謂「附著」係指有機酸金屬鹽、金屬胺 配位化合物介著金屬離子吸附於金屬粒子表面之意,金屬 粒子係有助於安定分散於大機分散體之狀態者。 做爲該有機金屬化合物之脂肪酸的構成有機金屬化合 物之脂肪酸爲至少1種選自C6〜C 2 2之飽和脂肪酸及不飽 和脂肪酸之脂肪酸者,較佳者爲至少1種選自己酸、庚酸 、辛酸、壬酸、癸酸、十一酸、十二酸、十四酸、廿酸、 廿二酸' 2-乙基己酸 '油酸、亞油酸、亞麻酸之脂肪酸 〇 又,做爲有機金屬化合物之胺的構成金屬絡合物之胺 者只要至少1種選自烷胺者即可。 做爲本發明可使用之烷胺例者未特別限定,一般可爲 第1〜3級胺者,亦可爲單胺 '雙胺、三胺等多價胺均可。 特別是具有碳數4〜20之主骨架烷胺者爲佳,具有碳數 8〜18之主骨架烷胺之安定性,掌控性面爲更佳者。又, 所有級數之烷胺均做爲分散劑有效者,惟,第1級之烷胺 其安定性、掌控性爲較理想者。當烷基之主鏈碳數短於4 時,則胺之鹽基性太強有金屬奈米粒子腐蝕之傾向,最後 恐出現溶解此奈米粒子之問題產生。又,烷胺之主鏈碳數 長過20則金屬奈米分散液濃度太高時,其分散液黏度上 昇,掌控性將變差’且,燒成後之金屬細線、金屬膜中易 殘留碳,造成比電阻値上昇之問題。 -9- (6) 1351982 做爲本發明可使用之烷胺具體例者如:丁 辛胺、壬胺、十二胺、己十二胺、辛癸胺、椰 胺、氫化牛脂胺、油胺、月桂胺、及硬脂烯胺 、二椰子胺、二氫化牛脂胺、及二硬脂烯胺等 及十二烷二甲胺、二十二烷單甲胺、十四烷二 二甲胺、椰子二甲胺、十二烷四癸二甲胺、及 3級胺、其他,有萘二胺、硬脂烯丙烯二胺、 胺、及壬二胺等二胺。此等胺中又以己胺、庚 癸胺、十二胺' 2 —乙基己胺、1,3 —二甲基-1 一胺基十一烷、I -胺基十二烷爲佳者。 本發明含金屬奈米粒子之分散液中烷胺之 奈米粒子金屬重量基準爲0.1重量%以上,10 者宜,較佳者爲1重量%以上,5重量%以下。 重量%時,則出現相互脂肪酸金屬化合物互相 黏作用,還原後分散性變差,反之,超出10 與金屬強固結合後剛出現效果時,即使於燒成 中仍無法取出氮,呈妨礙低溫燒成特性者。 本發明該有機金屬化合物亦可爲任意比例 機金屬化合物與胺金屬配位化合物之混合物者 本發明金屬奈米粒子之製造方法係使脂肪 屬化合物及/或胺基之金屬配位化合物溶於非: 於此液中添加還原劑後進行還原處理之後取得 子。 做爲該還原劑者以如:氫化硼鈉' 二甲胺 胺、己胺' 子胺、牛脂 等第1級胺 第2級胺、 甲胺、辛癸 三辛胺等第 辛亞烷基二 胺、辛胺、 -η — 丁胺' 金屬以金屬 重量%以下 當不足0.1 結合產生增 重量%則氮 熱分解過程 脂肪酸之有 〇 酸之有機金 區性溶媒, 金屬奈米粒 ΛτΑ» , '弟二— -10- (7) (7)1351982 丁胺硼等使用者宜。做爲還原劑者並未受限於此,只要具 有相同還原作用者即可,亦可使用其他公知之還原劑者。 此還原反應更於反應系中導入氫氣、一氧化碳氣體、含氫 之氣體、含一氧化碳之氣體後進行者爲較佳者。 該還原處理係於攪拌處理中進行沸騰,於室溫或加熱 迴流之條件下進行者。 如上述,於非極性溶媒中進行還原處理後形成金屬膠 質,惟,反應液中存在雜質(如:還原劑中之硼等)者。 因此,於反應液中添加脫離子水,進行攪拌後,靜置所定 時間後回收上澄液。此時,存在於反應液中之雜質中親水 性雜質往水層方向移動,因此,可降低雜質。以短碳數之 極性溶媒取代脫離子水使用者亦可。更進行去除過剩脂肪 酸、脂肪酸酯、胺等後,提昇純度及金屬濃度,因此,可 藉由超速過濾等之過濾後進行濃縮,其結果,可取得含有 5 wt %以上,90 wt %以下之金屬奈米粒子之分散液者。 本發明如上所製造之金屬奈米粒子分散液即使爲90 重量%之高濃度仍不致造成奈米粒子相互凝聚,且,不致 失去分散液之流動性。若使90重量%之金屬奈米粒子分 散液用於IC基板等多層配線,IC內部配線時,亦不致失 去此分散液之流動性,且,不致引起金屬奈米粒子之凝聚 ,可形成導電性無缺陷之均一微細之配線圖案者。 本發明所使用之非極性溶媒以使用如:弱極性之溶媒 者,主鏈碳數爲6〜18之有機溶媒者爲宜。當碳數不足6 時,則將出現溶媒極性強、未能分散之、或 '乾燥太快, -11 - (8) (8)1351982 不易掌控分散液製品之問題產生。反之,碳數超出1 8則 黏度上昇、燒成時易殘留碳數之問題產生。做爲此等溶媒 者,可使用如:己烷、庚烷、辛烷、癸烷、十一烷、十二 烷、十三烷、三甲基戊烷等長鏈鏈烷、環己烷、環庚烷、 環辛烷等環狀鏈烷 '苯、甲苯、二甲苯 '三甲基苯、十二 烷苯等芳香族烴基 '己醇 '庚醇、辛醇、癸醇、環己醇、 萜品醇等醇者。此等溶媒可單獨使用,亦可以混合溶媒之 形態使用之。如··長鏈鏈烷混合物之礦油精者亦可。 又,極性溶媒以碳數短之溶媒,如:甲醇、乙醇、丙 醇等爲宜。 本發明可提供金屬奈米粒子尺寸爲lOOnm以下者。 1(=基板等多層配線、半導體內部崩線等時,近年來更求 精密化,被要求爲]#m以下之配線,因此,金屬奈米粒 子之尺寸所要求線幅之〗门〇以下,亦即,lnm以上 I〇〇nm以下,較佳者爲Inm以上,l〇nm以下者,而,本 發明金屬奈米粒子充份滿足此期待。又,當大於I〇〇nm 之粒子時,由於自體太重出現沈澱現象,未能取得良好之 分散特性。 本發明之具導電性金屬細線或金屬膜之形成方法,將 該金屬奈米粒子分散液利用如:旋轉塗佈法等塗佈法塗佈 於各種基材後,進行乾燥之後燒成之。此時乾燥溫度只要 未流動塗佈液者即可,如:50〜]00 °C即可。又,燒成溫度 以]40〜3 00 °C者宜,較佳者爲]40〜22 0 °C即可充份達成實 用之導電率。 -12 - 1351982
〔實施例1〕 以油酸銀做爲有機酸鹽,以辛胺之銀配位化合物做爲 肢配位化合物者。首先,除非極性溶媒中加入28g油酸銀 ,:1 2g辛胺之銀配位化合物後,做成均勻液體。隨後,將 0. I g做成1 0%之二甲胺硼溶於甲醇之還原劑溶液加入該油 酸銀與辛胺銀配位化合物相互之溶液後,進行反應之。還 原溶液添加後該液之顏色由透明變成茶色,確定金屬膠質 之形成。此存在硼等雜質,因此,添加脫離子水於此反應 液後,劇烈攪拌後放置一晚,僅回收上澄液。更爲去除影 響熱分解之過剩油酸、辛胺,以超速過濾進行濃縮後,以 甲苯做爲非極性溶媒使用後進行濃度調整,調製3 5wt%濃 度之Ag分散液。此Ag奈米粒子之粒徑爲5nm者》 將此分散液藉由旋轉塗佈法塗佈於基板(玻璃), H)〇°C乾燥’ 2 50 °C燒成後製成銀的薄膜。進行測定此薄膜 之表面電阻後,取得膜厚爲〇.3Aim,比電阻爲3.6x]0-6 Ω · cm。 〔實施例2〕 以亞油酸銀做爲有機酸,且,以辛胺之銀配位化合物 做爲胺配位化合物使用之外,與實施例1同法進行銀奈米 粒子之合成、成膜、評定。此時電阻値爲膜厚〇.3#m, 比電阻 3 · 6 X 1 0 - δ Ω · c m 者。 使用以下表]所示原料,與實施例]同法進行金屬奈 -13- 1351982 (10) 米粒子之合成、成膜、評定 (11)1351982 實施例 有機酸鹽 胺 還原劑 金屬濃度 膜厚 電阻値 (%) {β m) (Ω · cm) 3 癸酸Ag 己胺Ag t-丁胺硼 35 0.30 3·2χ ]0·6 4 癸烯酸Ag 辛胺Ag 氣化硼Na 35 0.35 4.8χ ΙΟ'6 5 油酸Ag 月桂胺Ag 二甲胺硼 35 0.35 4·2χ ΙΟ·6 6 庚酸Ag 庚胺Ag 二甲胺硼 35 0.35 3.5χ ΙΟ'6 7 辛酸Ag 己胺Ag t-丁胺硼 35 0.25 4.0χ ΙΟ'6 8 壬酸Ag 癸胺Ag 氫化硼Na 35 0.30 3.3χ ΙΟ'6 9 油酸Ag 2-乙基己胺Ag CO氣體 35 0.25 3.6χ ΙΟ·6 ]0 癸酸Ag ]-胺基Η*—烷Ag H2氣體 35 0.30 4.0χ ΙΟ·6 Π 癸稀酸Ag 己胺Ag CO+N2氣體 35 0.25 3.8χ ΙΟ'6 12 亞油酸Ag 辛胺Ag H2+N2氣體 35 0.25 3.5χ 10-6 13 亞麻酸Ag 庚胺Ag t-丁胺硼 35 0.30 3.2χ ΙΟ'6 14 己酸Ag 己胺Ag 氫化硼Na 35 0.30 3_8χ ]0·6 15 月桂酸Ag 癸胺Ag 二甲胺硼 35 0.25 3.5χ ΙΟ'6 16 油酸Ag 庚胺Ag t-丁胺硼 35 0.25 3·9χ ]0·6 17 癸酸Au 己胺Au CO+N2氣體 35 0.30 4·0χ 】0·6 18 癸烯酸Au 1-胺基Η烷Au H2氣體 35 0.25 3·4χ ]0·6 19 亞油酸Au 庚胺Au 二甲胺硼 35 0.25 3.6χ ΙΟ'6 20 亞麻酸Au 辛胺Au t-丁胺硼 35 0.30 3.9χ ΙΟ'6 21 己酸Au 癸胺Au t-丁胺硼 35 0.30 3.5χ ΙΟ'6 22 月桂酸Au 己胺Au H2+N2氣體 35 0.25 3.8χ ΙΟ'6 23 油酸Au 庚胺Au 氫化硼Na 35 0.25 3.2χ ]〇'6 -15- (12) (12)1351982 使用實施例5所示之油酸Ag、月桂胺Ag配位化合物 所製成之銀奈米粒子之TOF- SIMS分析之結果如圖]所 示。由此結果,確定金屬表面附著油酸銀(Oleicacid + Ag )、或月桂胺銀(Dodecylamine + Ag)者。 〔比較例I〕 針對10%硝酸銀水溶液,使用高分子系之Soluspas 24〇00 (商品名:Zeneka公司製)做爲分散劑,使用二乙 醇胺做爲還原劑,與實施例1同法進行調製銀奈米粒子分 散液。反應後調整最終濃度呈35%。 將此分散液藉由旋轉塗佈法塗佈於基板後,]〇〇 °C乾 燥,2 5 (TC燒成後製成銀薄膜。進行測定此薄膜之表面電 阻後,呈膜厚0.3//、比電阻爲7χ]0—2Ω · cm。 〔比較例2〕 將〇.44g之合成甘胺酸與3.2g之硫酸亞鐵七水合物 溶於90 之離子交換水後,以氫氧化鈉水溶液(以離子 交換水使和光純藥工業(股份)製,試藥特級調整呈適當 濃度者)進行調整呈pH爲7之後,添加離子交換水做成 全量爲1 2 8 4。再於室溫下,以磁力攪拌器進行攪拌同時 ,於此滴入2 m£之含]g硝酸銀之水溶液後,製成金屬含 量約爲5 g/L之銀膠質液。此時,針對]g銀其甘胺的量爲 0 · 6 9 g 〇 該銀膠質液之濃度低,因此,藉由超速過濾進行高濃 -16- (13) (13)1351982 度化,惟,途中出現凝聚。且,爲取得充份導電性,務必 有一定膜厚,而,此濃度務必塗佈]〇次以上。 [產業上可利用性〕 本發明含金屬奈米粒子之分散液其金屬濃度極高,因 此,可減少成膜次數,同時,可藉由低溫燒成處理達成充 份實用之導電率。此金屬奈米粒子分散液於電氣電子工業 等領域下做爲無光儀表顯示器等顯示機器之用,於印刷配 線做爲金屬配線等製作之用。 【圖式簡單說明】 圖1代表實施例5所製成之本發明銀奈米粒子之TOF 一 SIM S分析結果之曲線圖。
Claims (1)
1351982 i?#忿月/7[日修正本 第093127010號專利申請案中文申請專利範圍修正本 民國100年8月17曰修正 十、申請專利範圍 1. 一種金屬奈米粒子,其係於各金屬周圍附著做爲 分散劑之有機金屬化合物之金屬奈米粒子,其特徵爲,該 有機金屬化合物爲脂肪酸之有機金屬化合物與胺之金屬配 位化合物之混合物的金屬奈米粒子,該胺爲具有直鏈或支 鏈結構之脂肪族胺者。 2-如申請專利範圍第1項之金屬奈米粒子,其中該有 機金屬化合物爲含有由至少1種選自貴金屬及過渡金屬之 金屬或至少2種之此等金屬所成之合金者。 3.如申請專利範圍第1項之金屬奈米粒子,其中該脂 肪酸爲至少1種選自具有直鏈或支鏈結構之C6~C22飽和脂 肪酸及不飽和脂肪酸之脂肪酸者。 4 ·如申請專利範圍第3項之金屬奈米粒子,其中該脂 肪酸爲至少1種選自:己酸、庚酸、辛酸、壬酸、癸酸、 十一酸、月桂酸、十四酸、廿酸、廿二酸、2—乙基己酸 、油酸、亞油酸、亞麻酸之脂肪酸者。 5 ·如申請專利範圍第1項之金屬奈米粒子,其中該胺 爲至少1種選自:己胺、庚胺、辛胺、癸胺、十二胺、2-乙基己胺、1,3 —二甲基一 η - 丁胺、1 一胺基十一烷、1 -胺基十三烷之胺者。 6-如申請專利範圍第1項至第5項中任一項之金屬奈 米粒子,其中該金屬奈米粒子之尺寸爲lnin以上,100nm 1351982 以下者。 7· —種金屬奈米粒子之製造方法,其特徵係於非極 性溶媒中溶解申請專利範圍第3項或第4項之脂肪酸有機金 屬化合物,與申請專利範圍第1項或第5項之胺金屬配位化 合物之混合物後,於此液中添加還原劑後,再於此液中導 入氫氣、一氧化碳氣體、含氫氣體,或含一氧化碳之氣體 後進行還原處理,隨後,添加脫離子水,攪拌、靜置後, •使雜質轉移至極性溶媒,而降低非極性溶媒中之雜質濃度 者。 8·如申請專利範圍第7項之金屬奈米粒子之製造方法 ’其中該還原處理係更導入氫氣、一氧化碳氣體、含氫氣 體’或含一氧化碳之氣體後進行者》 9·如申請專利範圍第7項或第8項之金屬奈米粒子之 製造方法,其中於該還原處理後,再添加脫離子水,攪拌 、靜置後,使雜質轉移至極性溶媒,而降低非極性溶媒中 ®之雜質濃度。 10·如申請專利範圍第7項至第9項中任一項之金屬奈 米粒子之製造方法,其中該金屬奈米粒子之尺寸爲lnm以 上,1 OOnm以下者。 11. —種金屬奈米粒子分散液,其特徵係濃縮藉由申 請專利範圍第7項至第10項中任一項之方法所得之含金屬 奈米粒子之分散液,使金屬奈米粒子進行再分散後,而得 金屬奈米粒子之濃度範圍爲5wt%以上,90wt%以下者。 12. 如申請專利範圍第11項之金屬奈米粒子分散液, -2- 1351982 其中該金屬奈米粒子之尺寸爲lnm以上,10〇nm以下者β 13. —種金屬奈米粒子分散液之製造方法,其特徵係 藉由濃縮含有依申請專利範圍第7項至第10項中任一項之 方法所得金屬奈米粒子混合物後,其次對於該金屬奈米粒 子進行再分散後,製得金屬奈米粒子之濃度範圍爲5wt% 以上,90wt%以下之金屬奈米粒子。 14. 如申請專利範圍第13項之金屬奈米粒子分散液之 製造方法,其中該金屬奈米粒子之尺寸爲lnm以上, 1 0 Onm以下者。 15. —種金屬細線或金屬膜之形成方法,其特徵係將 含有申請專利範圍第1項至第6項中任一項之金屬奈米粒子 之分散液,含有申請專利範圍第7項至第10項中任一項之 製造方法所得之含金屬奈米粒子之分散液,申請專利範圍 第1 1項或第1 2項之分散液,或申請專利範圍第1 3項或第1 4 項之製造方法所得之金屬奈米粒子分散液塗佈於基材後, 經乾燥後燒成之後形成具有導電性之金屬細線或金屬膜者 〇 16. 如申請專利範圍第15項之金屬細線或金屬膜之形 成方法,其中該燒成溫度爲1 40-3 00 °C者。 17. —種金屬細線,其特徵係藉由如申請專利範圍第 15項或第16項之形成方法所取得者。 18. 一種金屬膜,其特徵係藉由如申請專利範圍第15 項或第1 6項之形成方法所取得者。
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EP1666408A1 (en) | 2006-06-07 |
US20070134491A1 (en) | 2007-06-14 |
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CN1849260B (zh) | 2011-12-14 |
TW200510060A (en) | 2005-03-16 |
KR20060069491A (ko) | 2006-06-21 |
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