CN110335700B - High-temperature sintering type yellow light conductive paste, conductive circuit and preparation method - Google Patents
High-temperature sintering type yellow light conductive paste, conductive circuit and preparation method Download PDFInfo
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- CN110335700B CN110335700B CN201910574418.6A CN201910574418A CN110335700B CN 110335700 B CN110335700 B CN 110335700B CN 201910574418 A CN201910574418 A CN 201910574418A CN 110335700 B CN110335700 B CN 110335700B
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- Prior art keywords
- methacrylate
- acrylate
- percent
- photosensitive organic
- temperature
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- 238000005245 sintering Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 80
- 239000011521 glass Substances 0.000 claims abstract description 59
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 40
- 239000000178 monomer Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 8
- 230000008018 melting Effects 0.000 claims abstract description 8
- 230000007704 transition Effects 0.000 claims abstract description 7
- 239000002002 slurry Substances 0.000 claims description 41
- 239000002245 particle Substances 0.000 claims description 40
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 19
- 238000009835 boiling Methods 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229910052709 silver Inorganic materials 0.000 claims description 12
- 239000004332 silver Substances 0.000 claims description 12
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 9
- 239000000194 fatty acid Substances 0.000 claims description 9
- 229930195729 fatty acid Natural products 0.000 claims description 9
- 150000004665 fatty acids Chemical class 0.000 claims description 9
- 230000002209 hydrophobic effect Effects 0.000 claims description 9
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000003292 glue Substances 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000002518 antifoaming agent Substances 0.000 claims description 6
- 239000007810 chemical reaction solvent Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000004014 plasticizer Substances 0.000 claims description 6
- 239000013008 thixotropic agent Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 5
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 5
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 claims description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000008240 homogeneous mixture Substances 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 claims description 4
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 2
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- VEPKQEUBKLEPRA-UHFFFAOYSA-N VX-745 Chemical compound FC1=CC(F)=CC=C1SC1=NN2C=NC(=O)C(C=3C(=CC=CC=3Cl)Cl)=C2C=C1 VEPKQEUBKLEPRA-UHFFFAOYSA-N 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims description 2
- OCDWICPYKQMQSQ-UHFFFAOYSA-N docosyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCCCCCOC(=O)C(C)=C OCDWICPYKQMQSQ-UHFFFAOYSA-N 0.000 claims description 2
- KHAYCTOSKLIHEP-UHFFFAOYSA-N docosyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCCCCCOC(=O)C=C KHAYCTOSKLIHEP-UHFFFAOYSA-N 0.000 claims description 2
- HYUPPKVFCGIMDB-UHFFFAOYSA-N ethyl 2-(4-hydroxyphenyl)acetate Chemical compound CCOC(=O)CC1=CC=C(O)C=C1 HYUPPKVFCGIMDB-UHFFFAOYSA-N 0.000 claims description 2
- ZWEDFBKLJILTMC-UHFFFAOYSA-N ethyl 4,4,4-trifluoro-3-hydroxybutanoate Chemical compound CCOC(=O)CC(O)C(F)(F)F ZWEDFBKLJILTMC-UHFFFAOYSA-N 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- ZNAOFAIBVOMLPV-UHFFFAOYSA-N hexadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C(C)=C ZNAOFAIBVOMLPV-UHFFFAOYSA-N 0.000 claims description 2
- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 claims description 2
- LNMQRPPRQDGUDR-UHFFFAOYSA-N hexyl prop-2-enoate Chemical compound CCCCCCOC(=O)C=C LNMQRPPRQDGUDR-UHFFFAOYSA-N 0.000 claims description 2
- CFBXDFZIDLWOSO-UHFFFAOYSA-N icosyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCCCOC(=O)C(C)=C CFBXDFZIDLWOSO-UHFFFAOYSA-N 0.000 claims description 2
- NGYRYRBDIPYKTL-UHFFFAOYSA-N icosyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCCCOC(=O)C=C NGYRYRBDIPYKTL-UHFFFAOYSA-N 0.000 claims description 2
- DOULWWSSZVEPIN-UHFFFAOYSA-N isoproturon-monodemethyl Chemical compound CNC(=O)NC1=CC=C(C(C)C)C=C1 DOULWWSSZVEPIN-UHFFFAOYSA-N 0.000 claims description 2
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 2
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims description 2
- NZIDBRBFGPQCRY-UHFFFAOYSA-N octyl 2-methylprop-2-enoate Chemical compound CCCCCCCCOC(=O)C(C)=C NZIDBRBFGPQCRY-UHFFFAOYSA-N 0.000 claims description 2
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 claims description 2
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 claims description 2
- YOTGRUGZMVCBLS-UHFFFAOYSA-N pentadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCOC(=O)C(C)=C YOTGRUGZMVCBLS-UHFFFAOYSA-N 0.000 claims description 2
- GOZDOXXUTWHSKU-UHFFFAOYSA-N pentadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCOC(=O)C=C GOZDOXXUTWHSKU-UHFFFAOYSA-N 0.000 claims description 2
- ULDDEWDFUNBUCM-UHFFFAOYSA-N pentyl prop-2-enoate Chemical compound CCCCCOC(=O)C=C ULDDEWDFUNBUCM-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- 238000007639 printing Methods 0.000 claims description 2
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 claims description 2
- 150000004671 saturated fatty acids Chemical class 0.000 claims description 2
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims description 2
- KEROTHRUZYBWCY-UHFFFAOYSA-N tridecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCOC(=O)C(C)=C KEROTHRUZYBWCY-UHFFFAOYSA-N 0.000 claims description 2
- XOALFFJGWSCQEO-UHFFFAOYSA-N tridecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCOC(=O)C=C XOALFFJGWSCQEO-UHFFFAOYSA-N 0.000 claims description 2
- RRLMGCBZYFFRED-UHFFFAOYSA-N undecyl prop-2-enoate Chemical compound CCCCCCCCCCCOC(=O)C=C RRLMGCBZYFFRED-UHFFFAOYSA-N 0.000 claims description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims 2
- 230000001070 adhesive effect Effects 0.000 abstract description 10
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- 238000011161 development Methods 0.000 abstract description 7
- 239000005416 organic matter Substances 0.000 description 18
- -1 1, 1-dimethyl-2-oxo-2-phenylethyl Chemical group 0.000 description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 14
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 14
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- 239000005642 Oleic acid Substances 0.000 description 14
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 14
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- 238000012360 testing method Methods 0.000 description 10
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- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- CXJQCHSHDWVBKU-UHFFFAOYSA-N [2-methyl-1-oxo-1-(4-propan-2-ylphenyl)propan-2-yl] prop-2-enoate Chemical compound CC(C)C1=CC=C(C(=O)C(C)(C)OC(=O)C=C)C=C1 CXJQCHSHDWVBKU-UHFFFAOYSA-N 0.000 description 1
- SXNMNCCJMOBSOS-UHFFFAOYSA-N [4-(2-hydroxy-2-methylpropanoyl)phenyl] 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=C(C(=O)C(C)(C)O)C=C1 SXNMNCCJMOBSOS-UHFFFAOYSA-N 0.000 description 1
- CZPPSIWKPLPVPG-UHFFFAOYSA-N [4-(2-hydroxy-2-methylpropanoyl)phenyl] prop-2-enoate Chemical compound CC(C)(O)C(=O)C1=CC=C(OC(=O)C=C)C=C1 CZPPSIWKPLPVPG-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- ISXDVFNOXYQPIA-UHFFFAOYSA-N dibutyl pentanedioate Chemical compound CCCCOC(=O)CCCC(=O)OCCCC ISXDVFNOXYQPIA-UHFFFAOYSA-N 0.000 description 1
- NFKGQHYUYGYHIS-UHFFFAOYSA-N dibutyl propanedioate Chemical compound CCCCOC(=O)CC(=O)OCCCC NFKGQHYUYGYHIS-UHFFFAOYSA-N 0.000 description 1
- 229960002097 dibutylsuccinate Drugs 0.000 description 1
- OUWSNHWQZPEFEX-UHFFFAOYSA-N diethyl glutarate Chemical compound CCOC(=O)CCCC(=O)OCC OUWSNHWQZPEFEX-UHFFFAOYSA-N 0.000 description 1
- WYACBZDAHNBPPB-UHFFFAOYSA-N diethyl oxalate Chemical compound CCOC(=O)C(=O)OCC WYACBZDAHNBPPB-UHFFFAOYSA-N 0.000 description 1
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- HBGGXOJOCNVPFY-UHFFFAOYSA-N diisononyl phthalate Chemical compound CC(C)CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC(C)C HBGGXOJOCNVPFY-UHFFFAOYSA-N 0.000 description 1
- BEPAFCGSDWSTEL-UHFFFAOYSA-N dimethyl malonate Chemical compound COC(=O)CC(=O)OC BEPAFCGSDWSTEL-UHFFFAOYSA-N 0.000 description 1
- XTDYIOOONNVFMA-UHFFFAOYSA-N dimethyl pentanedioate Chemical compound COC(=O)CCCC(=O)OC XTDYIOOONNVFMA-UHFFFAOYSA-N 0.000 description 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- HZHMMLIMOUNKCK-UHFFFAOYSA-N dipropyl oxalate Chemical compound CCCOC(=O)C(=O)OCCC HZHMMLIMOUNKCK-UHFFFAOYSA-N 0.000 description 1
- IXAVSISAEGUDSL-UHFFFAOYSA-N dipropyl pentanedioate Chemical compound CCCOC(=O)CCCC(=O)OCCC IXAVSISAEGUDSL-UHFFFAOYSA-N 0.000 description 1
- LWIWFCDNJNZEKB-UHFFFAOYSA-N dipropyl propanedioate Chemical compound CCCOC(=O)CC(=O)OCCC LWIWFCDNJNZEKB-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- JQCXWCOOWVGKMT-UHFFFAOYSA-N phthalic acid diheptyl ester Natural products CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC JQCXWCOOWVGKMT-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003466 welding Methods 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
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0016—Apparatus or processes specially adapted for manufacturing conductors or cables for heat treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Conductive Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention particularly relates to high-temperature sintering type yellow light conductive paste, a conductive circuit and a preparation method. The high-temperature sintered yellow light conductive paste comprises the following components in percentage by weight: 75-90% of noble metal powder; 1% -5% of glass powder; 8% -25% of a photosensitive organic carrier; wherein the glass phase transition temperature Tg of the glass powder is 400-500 ℃, and the melting temperature Tf is 500-600 ℃. The noble metal powder, the glass powder and the photosensitive organic carrier are matched, the conductive paste is suitable for high-temperature sintering, the obtained conductive paste can realize the superfine wire diameter resolution, and the sintered conductive paste has good resistivity and adhesive force. Glass powder with proper glass phase transition temperature and melting temperature is added to provide proper adhesive force for the metal conducting layer and the base material, and the optimized noble metal powder and the glass powder ensure that the sintered circuit does not have shrinkage cavity and broken line and can reduce the resistivity; the photosensitive organic carrier with the proper types and proportions of the monomers and the initiator has high resolution and superfine wire diameter after development.
Description
Technical Field
The invention relates to the technical field of electronic materials, in particular to high-temperature sintering type yellow light conductive paste, a conductive circuit and a preparation method.
Background
Today electronic products are already flooded in human daily life. With continuous discovery of user experience and technology, various electronic products have more and more perfect functions and smaller sizes and weights. Light, thin and small are inevitable trends of electronic products.
The miniaturization, the light weight and the integration of hardware are system engineering, and a chip, a passive component and a circuit substrate in a circuit need to be simultaneously reduced.
In general, the conductive paste is cured to allow metal particles to effectively contact each other, thereby removing an excessive organic component and forming a wiring having sufficient mechanical strength. The general curing is divided into two modes of low-temperature (lower than 300 ℃) curing and high-temperature (higher than 600 ℃) sintering, and aiming at inorganic material substrates such as general passive electronic components and ceramic-based PCB boards, when the low-temperature curing is adopted, because organic resin still exists in the conducting layer and conducting particles are only conducted in a contact mode, a good conducting path cannot be formed among the conducting particles, the circuit resistance is overhigh, and the mechanical property is not good enough.
In the current high-temperature conductive paste, the traditional high-density and fine-wire diameter microelectronic production process is completed in a clean room by high-vacuum evaporation and material reduction manufacturing technologies. The outstanding defects are shown in the following: the evaporation equipment and the process have high cost and expensive operating cost; the time and material consumption for manufacturing the circuit board are reduced, the discharge cost is high, and the waste liquid causes heavy metal and chemical pollution; in addition, the circuit board also has subsequent processes such as chip and other components and circuit board surface mount package. Therefore, there is a need for an environment-friendly, high-performance conductive paste process suitable for mass application.
Disclosure of Invention
The invention aims to provide a high-temperature sintering type yellow light conductive paste, and solves the defect of poor resistance performance caused by low-temperature sintering of an inorganic material substrate in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the high-temperature sintering type yellow light conductive paste comprises the following components in percentage by weight:
75-90% of noble metal powder;
1% -5% of glass powder;
8% -24% of a photosensitive organic carrier;
wherein the glass phase transition temperature Tg of the glass powder is 400-500 ℃, and the melting temperature Tf is 500-600 ℃.
The combination of the glass powder, the noble metal and the photosensitive organic carrier is utilized to realize the combination of the noble metal powder as the conductive filler, the glass powder as the adhesive and the photosensitive organic carrier providing the photosensitive characteristic.
The selected glass powder is a high-temperature binding phase, and the glass powder is a direct connecting layer of the metal conducting layer and the base material and can provide proper adhesive force; and secondly, the liquid glass phase can play a role in melting the sintering of the noble metal powder at high temperature, meanwhile, the glass powder can dissolve part of noble metals (such as silver and the like) after being melted, in the cooling process after sintering, the noble metals dissolved in the glass liquid can be separated out due to temperature reduction and solubility reduction, because the separation is microscopic atomic-level behavior, the noble metals are crystallized into nano metal particles after being separated out, and because the number of the particles in the medium is increased, and the number of conductive paths among original metal particles can be increased and the conductive capacity is enhanced due to particle chains formed by the nano particles. Therefore, the glass frit in the conductive paste is an important factor for determining the adhesion and the electrical properties.
The glass powder has proper glass phase transition temperature Tg and melting temperature Ts, so that the glass powder can be matched with the sintering process of the noble metal powder body to play a role in fluxing, and a molten ball generated by overburning cannot be caused. Meanwhile, the glass powder has good adhesive force to the ceramic substrate, and meets the requirement of subsequent welding tension.
Further, the noble metal powder is one or more of silver powder, gold powder, silver-palladium powder and silver-coated copper powder, wherein the noble metal powder is coated with fatty acid on the surface, and the method comprises the following steps:
the average particle diameter is 1.5-2.5 μm, and the comparative area is 0.7-1.5m270-95% of noble metal powder per gram,
average particle diameter of 0.7-1.5 μm, and specific surface area of 1.0-2.5m25-30% of noble metal powder per gram.
The conductive performance is realized by depending on noble metal powder filler, the resistivity of the sintered metal circuit is ensured, the resistance is increased due to the fact that the conductive layer is too thin when the metal content is too low, and cavities and through holes are possibly caused due to powder shrinkage, so that wire breakage is caused.
In the invention, the selected noble metal powder is spherical or sphere-like, and two noble metal powders with particle size intervals are selected and matched, wherein the average particle size interval 1 is 1.5-2.5 mu m, the noble metal powder accounts for 70-95% in the noble metal powder according to weight percentage, and the specific surface of the noble metal powder in the average particle size interval 1 is controlled to be 0.7-1.5m2Between/g and tap density of 4.5-6.0g/cm3In the middle of (1). The average grain diameter interval 2 is 0.7-1.5 μm, and the content of the average grain diameter interval in the noble metal powder is 5-30% according to the weight percentage, and the specific surface area is 1.0-2.5m2Between/g; the tap density is 5-6.5g/cm3In the middle of (1). The noble metal powder is matched with different particle sizes, so that effective dense accumulation can be formed, a conductive path is guaranteed, and the resistance is reduced.
Further, the fatty acid is an unsaturated fatty acid or a saturated fatty acid having twelve or more carbons.
The selected fatty acid is preferably unsaturated fatty acid containing more than twelve carbons, and preferably, the fatty acid is oleic acid. The spherical or spheroidal noble metal powder is coated with fatty acid, the burning loss of the corresponding noble metal powder is 0.3-0.9% at 538 ℃, and the dispersibility of the noble metal powder can be improved by coating the fatty acid on the surface of the noble metal powder. The fatty acid may also be stearic acid or palmitic acid.
According to the noble metal powder, the organic matter is coated on the surface, the corresponding particle size is matched, the spherical shape or the similar spherical shape is selected, the surface appearance, the tap density and the specific surface area are limited, so that the noble metal powder can completely show a circuit through exposure and development, effective interconnection and intercommunication can be formed after sintering, the resistivity is reduced, the sintering shrinkage is uniform, and the wire breakage caused by shrinkage cavities can be avoided.
Further, the glass powder comprises Bi in percentage by weight2O3:70-90％；SiO25-15 percent; ZnO: 5-20%, and the average grain diameter of the glass powder is 1-2 um.
Further, the photosensitive organic vehicle comprises, in weight percent: photoinitiator (2): 1 to 8 percent; hydrophilic monomer: 5 to 20 percent; hydrophobic monomer: 0.5-4%; thermal initiator: 0.1-2.5%; reaction solvent: 30 to 65 percent; slurry solvent: 15% -50%; additive: 0.5 to 10 percent.
According to the photosensitive organic carrier, the types and proportions of the monomers and the initiator are adjusted, so that the photosensitive organic carrier can be crosslinked and cured under ultraviolet irradiation under the condition of low content, high resolution is realized, the wire diameter and wire distance of 5-20 um level are realized, the linear shape is neat, and no burrs are generated.
Wherein the photoinitiator is a polymerizable cleavage type photoinitiator which can perform chain extension on the initiator to realize the purposes of chain extension and crosslinking, and the selected photoinitiator can be 1, 1-dimethyl-2-oxo-2-phenylethyl 2-acrylate (CAS:103658-85-1), 1-dimethyl-2-oxo-2-phenylethyl 2-methacrylate (CAS:135899-40-0), (2-methyl-1-oxo-1-phenylpropan-2-yl) 2-methylpropan-2-enoic acid ethyl ester, 4-isopropylphenyl 2-acryloyloxy-2-propyl ketone (CAS:135899-38-6), 4-acryloyloxyphenyl 2-hydroxy-2-propyl ketone (CAS:110430-11-0) One or more, preferably one or two, of 4-methacryloxyphenyl 2-hydroxy-2-propyl ketone (CAS:133160-09-5) and 1-hydroxy-2-prop-2-enylcyclohexyl-phenyl ketone (CAS:99937-16-3), wherein the added photoinitiator accounts for 1-8% of the weight of the photosensitive organic carrier.
Further, the hydrophilic monomer and the hydrophobic monomer both contain a carbon-carbon double bond.
Wherein the hydrophilic monomer is one or more of polyethylene glycol methacrylate, ethylene glycol methacrylate, polyethylene glycol ethyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate and hydroxypropyl methacrylate, preferably one or two; the added hydrophilic monomer accounts for 5-20% of the weight of the photosensitive organic carrier.
The hydrophobic monomer is styrene, methyl methacrylate, methyl acrylate, ethyl methacrylate, ethyl acrylate, propyl methacrylate, propyl acrylate, n-butyl methacrylate, n-butyl acrylate, isobutyl methacrylate, isobutyl acrylate, isobutyl methacrylate, pentyl acrylate, n-hexyl methacrylate, n-hexyl acrylate, n-heptyl methacrylate, n-heptyl acrylate, n-octyl methacrylate, n-octyl acrylate, n-undecyl methacrylate, undecyl acrylate, tridecyl methacrylate, tridecyl acrylate, pentadecyl methacrylate, pentadecyl acrylate, hexadecyl methacrylate, hexadecyl acrylate, octadecyl methacrylate, octadecyl acrylate, eicosyl methacrylate, or mixtures thereof, One or more, preferably one or two, of eicosyl acrylate, docosyl methacrylate and docosyl acrylate, and the added hydrophobic monomer accounts for 1-8% of the weight of the photosensitive organic carrier.
The thermal initiator comprises one or more selected from azodiethylbutyronitrile, azodiisoheptonitrile and azodiisobutyronitrile, preferably one, and the thermal initiator is added in an amount of 0.1-2.5 wt% based on the photosensitive organic carrier.
Reaction solvents include, but are not limited to, solvents selected from: one or more of ethylene glycol monobutyl ether, propylene glycol monomethyl ether, diethylene glycol monobutyl ether, diethylene glycol monomethyl ether, ethylene glycol methyl ether acetate and propylene glycol methyl ether acetate, preferably one or a mixture of 2.
Further: comprises a slurry solvent with the boiling point of 100-150 ℃, the boiling point of 150-250 ℃ and the boiling point of 250-300 ℃, wherein:
the weight percentage of the slurry solvent with the boiling point of 100-150 ℃ in the photosensitive organic carrier is 7-25 percent;
the weight percentage of the slurry solvent with the boiling point of 150-250 ℃ in the photosensitive organic carrier is 5-15 percent;
the slurry solvent with the boiling point of 250-300 ℃ accounts for 3-10% of the weight of the photosensitive organic carrier.
The first interval is solvent with boiling point at 100-150 deg.c and includes one or several of dipropyl oxalate, dimethyl adipate and propylene glycol methyl ether acetate. The mass of the slurry solvent in the first interval accounts for 7-25% of the mass of the photosensitive organic carrier.
The second interval is solvent with boiling point at 150-250 deg.C, which comprises one or more of dimethyl oxalate, diethyl oxalate, dibutyl oxalate, dimethyl malonate, diethyl malonate, dipropyl malonate, dimethyl succinate, diethyl succinate, dimethyl glutarate, diethyl glutarate, dipropyl adipate, ethylene glycol methyl ether acetate, ethylene glycol ethyl ether acetate, diethylene glycol methyl ether acetate, diethylene glycol ethyl ether acetate, dipropylene glycol methyl ether acetate and 2,2, 4-trimethyl-1, 3-pentanediol diisobutyrate. The mass of the slurry solvent in the second interval accounts for 5-15% of the mass of the photosensitive organic carrier.
The third interval is solvent with boiling point of 250-300 deg.C, one or more of dibutyl malonate, dipropyl succinate, dibutyl succinate, dipropyl glutarate, dibutyl glutarate, diethyl adipate and dibutyl adipate. The mass of the slurry solvent in the third interval accounts for 3-10% of the mass of the photosensitive organic carrier.
Through the adjustment of the boiling point proportion of the organic matter, the organic matter is stably volatilized in the glue discharging process, the conditions of bumping, residue, air holes and the like can not occur, and the disconnection situation is prevented, so that the adhesive force of the high-temperature sintering type yellow light conductive paste is ensured.
Further: the additive comprises: the coating comprises a thixotropic agent, a leveling agent, a defoaming agent and a plasticizer, wherein the thixotropic agent accounts for 0.5-2% of the photosensitive organic carrier; the mass of the leveling agent accounts for 0.5-2% of the mass of the photosensitive organic carrier; the mass of the defoaming agent accounts for 1% -3% of the mass of the photosensitive organic carrier; the mass percentage of the plasticizer in the photosensitive organic carrier is 0.1-3%.
Wherein the thixotropic agent is selected from gas-phase SiO2 and amide wax, and the mass percentage of the thixotropic agent in the photosensitive organic carrier is 0.5-2%; the leveling agent is selected from acrylated polysiloxane, polyether modified polysiloxane, polysiloxane polyether copolymer and polysiloxane, and the mass of the leveling agent accounts for 0.5-2% of that of the photosensitive organic carrier; the defoaming agent is selected from tributyl phosphate, trimethyl siloxane, polyether, polyacrylate and organic silicon resin, and the defoaming agent accounts for 1% -3% of the photosensitive organic carrier by mass;
the plasticizer is selected from di (2-ethylhexyl) phthalate, dioctyl phthalate, di-n-octyl phthalate, butyl benzyl phthalate, di-sec-octyl phthalate, dicyclohexyl phthalate, dibutyl phthalate, diisobutyl phthalate, dimethyl phthalate, diethyl phthalate, diisononyl phthalate and diisodecyl phthalate, and the mass of the plasticizer accounts for 0.1-3% of the mass of the photosensitive organic carrier;
the invention also provides a preparation method of the high-temperature sintering type yellow light conductive paste, which comprises the following steps: comprises that
Step A: preparation of photosensitive organic vehicle: carrying out ultrasonic mixing on a photoinitiator, a hydrophilic monomer, a hydrophobic monomer and a thermal initiator to obtain a homogeneous mixture; dripping the homogeneous mixture into a reaction solvent preheated to 80-90 ℃, stirring and reacting at the temperature, introducing inert gas for protection to obtain an intermediate, and then uniformly mixing and stirring the intermediate, a slurry solvent and an additive to obtain a photosensitive organic carrier;
and B: and B, mixing and stirring the photosensitive organic carrier in the step A, glass powder and noble metal powder according to a weight ratio, and then fully grinding to obtain the high-temperature sintering type yellow light conductive paste.
Preferably, the introduced inert gas is argon, in the step a, the reaction solvent is firstly added into a glass reaction kettle with a reflux condenser, stirring is carried out at a stirring speed of 100-.
In the step B, the photosensitive organic carrier in the step A is mixed with glass powder and noble metal powder according to the weight ratio, and after the mixture is fully stirred, a three-roll grinder is used for grinding the mixture for 6 times according to different fineness, and then uniform conductive slurry is obtained.
The invention also provides a method for preparing a conductive circuit by applying the high-temperature sintering type yellow light conductive paste, which comprises the following steps: and printing the high-temperature sintered yellow-light conductive paste on a base material through a screen, drying at the temperature of 100-150 ℃, carrying out 200-fold energy exposure at 500mj, developing by using a weak alkaline aqueous solution, carrying out glue discharge at the temperature of 350-fold energy of 450 ℃, then sintering at the temperature of 700-fold energy of 850 ℃, cooling, wherein the cooling speed is 10-30 ℃/min.
The base material can comprise PET, PP, PE, PA, glass, a silicon wafer or a ceramic wafer, the obtained high-temperature sintering type yellow light slurry is printed on a sheet-shaped base material by utilizing screen printing, then drying is carried out, a conductive film with a solvent removed is obtained, after exposure, development is carried out by utilizing a weak alkaline aqueous solution, the selected weak alkaline aqueous solution can be one or more of sodium bicarbonate, sodium carbonate, potassium carbonate and the like, and the solubility of the weak alkaline aqueous solution is adjusted to be pH 9-11. And developing to obtain a conductive circuit pattern. In order to obtain a conductive circuit with better performance, a high-temperature sintering mode is adopted, specifically, the developed conductive circuit is subjected to glue removal for 2 hours at the temperature of 350-450 ℃, the temperature is gradually increased, the temperature increasing rate is preferably 20-30 ℃/min, then sintering is carried out at the temperature of 700-850 ℃, the temperature is preferably 750-800 ℃, the temperature is kept for 5-25 minutes, then cooling is carried out, and the conductive circuit with a good passage is obtained, and the temperature decreasing rate is preferably 10-30 ℃/min.
The invention has the beneficial effects that the noble metal powder, the glass powder and the photosensitive organic carrier are matched, the high-temperature sintering is applicable, the superfine wire diameter resolution can be realized by the obtained conductive slurry, and the sintered conductive slurry has good resistivity and adhesive force. The glass powder with proper glass phase transition temperature and melting temperature is added to provide proper adhesive force for the metal conducting layer and the base material, the preferable metal powder ensures that the sintered circuit does not have shrinkage cavity and broken line, the resistivity can be reduced, and the metal powder can be well matched with inorganic glass powder filler. Meanwhile, the boiling point of the slurry solvent of the gradient grade is matched, so that the stability in the glue discharging process is ensured.
The conductive circuit prepared from the high-temperature sintering type yellow conductive paste utilizes an exposure and development process, is more environment-friendly in preparation process, and is suitable for mass production. The high-temperature-resistant conductive material is prepared under high-temperature sintering, has a better conductive path, is lower in resistance and more excellent in mechanical property, is suitable for application scenes with high reliability, and has a larger application prospect and a larger market scale.
Detailed Description
The invention is further illustrated by the following preferred embodiments. It should be noted that these examples are merely illustrative and are not to be construed as limiting the present invention.
Example 1:
(1) preparing an organic carrier:
1-hydroxy-2-prop-2-enylcyclohexyl-phenyl ketone (2.5%), methacrylic acid (7.5%), polyethylene glycol methacrylic acid (2.5%), hydroxyethyl methacrylate (7.5%), ethyl methacrylate (7.5%), styrene (2%), azobisisobutyronitrile (0.5%) were ultrasonically dissolved and mixed. Adding propylene glycol methyl ether (70%) into a glass reaction kettle with a reflux condenser, introducing argon at 85 ℃ for protection and stirring, gradually dripping the mixture into the glass reaction kettle through a dropping funnel, keeping the temperature at 85 ℃, and stirring for 4 hours to obtain an intermediate.
Intermediate, 60%;
dimethyl adipate, 23%;
diethylene glycol ethyl ether acetate, 7%;
dibutyl adipate, 7%;
0.5 percent of modified polyether;
1 percent of trimethylsiloxane
1.5 percent of methyl phthalate;
the photosensitive organic carrier is obtained by weighing the raw materials according to the weight ratio, mixing, heating to 90-120 ℃, and electrically stirring until all the materials are dissolved to form uniform liquid.
(2) Preparing yellow light slurry:
spherical silver powder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃, and the weight ratio of the conductive slurry is 55 percent;
spherical silver powder (particle diameter 0.9um, specific surface area 0.8 g/m)2The tap density is 5.0g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.5 percent at 538 ℃, and the weight ratio of the conductive slurry is 25 percent;
glass powder (the component proportions are Bi2O 375%, SiO 212%, ZnO 5%, and other components 8%, Tg 438 ℃, Tf 510 ℃, and the particle size is 2um), and the weight ratio of the conductive paste is 3%;
and (4) fully stirring 17% of the photosensitive organic carrier, and grinding for 6 times by using a three-roll mill to obtain uniformly dispersed conductive slurry.
(3) And (3) testing the performance of the conductive paste:
the selected base materials are as follows: and (3) polishing the 96% aluminum oxide ceramic until the roughness is below 1 um.
The screen printing conditions were: 360 mesh stainless steel screen printing
The drying conditions are as follows: 130 ℃ for 5 minutes
The exposure conditions were: 200mj energy, 20um open film mask
The developing solution conditions were: 0.5% aqueous NaHCO3 solution, development pressure 0.2kg
The sintering conditions are as follows: discharging glue at 400 ℃ for 2 hours, heating at the rate of 20 ℃/min, keeping the temperature at 800 ℃ for 20 minutes, and cooling at the rate of 30 ℃/min.
The cured slurry was tested for properties:
1. appearance: after standing at room temperature for 24 hours, the film was visually observed.
2. Fineness: the fineness measurement is carried out according to the standard GB/T17473.2-2008 noble metal slurry test method for microelectronic technology.
3. Resistivity: the resistance value R at two ends of the test line is measured by a milliohm meter, the pattern length of the test line is L-4.5 cm, the line width d is 20um, the thickness h is measured by a screw micrometer, and the resistivity rho is calculated as rho-R-d-h/L.
4. Adhesion force: adhesion of the cured slurry to a substrate was tested according to standard "GB/T17473.4-2008 for microelectronic technology with noble metal slurry test methods adhesion determination, ceramic substrate".
5. Wire diameter: the line width/line pitch of the observation measurement was 20/20 μm, using a 50-fold microscope for observation measurement.
6. Surface through hole: in the case of strong light on the back side, the measurement was observed with a 200-fold microscope.
Example 2:
(1) preparing a photosensitive organic carrier:
(2-methyl-1-oxo-1-phenylprop-2-yl) ethyl 2-methylpropan-2-enoate (3%), acrylic acid (7.5%), polyethylene glycol methacrylate (9%), propyl acrylate (7%), styrene (2%), azobisisobutyronitrile (0.5%) were ultrasonically dissolved and mixed. Adding ethylene glycol monomethyl ether acetate (71%) into a glass reaction kettle with a reflux condenser, introducing argon at 85 ℃ for protection and stirring, gradually dripping the mixture into the glass reaction kettle through a dropping funnel, keeping the temperature at 85 ℃, and stirring for 4 hours to obtain an intermediate.
Intermediate, 60%;
dimethyl adipate, 22%;
5% of ethylene glycol monoethyl ether acetate;
hexanediol diacrylate, 8%;
diethyl adipate, 2%;
gas phase SiO2, 1%;
acrylated polysiloxane, 0.5%;
1% of tributyl phosphate;
0.5 percent of methyl phthalate;
weighing the above raw materials, mixing, heating to 90-120 deg.C, and stirring under electric power until all materials are dissolved to obtain uniform liquid, to obtain photosensitive organic vehicle.
(2) Preparing yellow silver paste:
spherical silver powder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃, and the weight ratio of the conductive paste is 63 percent;
spherical silver powder (particle diameter 0.9um, specific surface area 0.8 g/m)2The tap density is 5.0g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.5 percent at 538 ℃, and the weight ratio of the conductive slurry is 20 percent;
glass powder (the component proportions are Bi2O 375%, SiO 212%, ZnO 5%, and other components 8%, Tg 438 ℃, Tf 510 ℃, and the particle size is 2um), and the weight ratio of the conductive paste is 1%;
16% of photosensitive organic carrier, fully stirring, grinding by a three-roll machine for 6 times to obtain uniformly dispersed conductive slurry.
(3) The performance test of the high-temperature sintered yellow conductive paste obtained in this embodiment is as follows:
the test conditions were the same as in example 1
Example 3:
(1) preparing a photosensitive organic carrier:
the intermediate was the same as in example 2.
Intermediate, 62%;
adipic acid dimethyl ester, 18%;
ethylene glycol monoethyl ether acetate, 8%;
hexanediol diacrylate, 7%;
diethyl adipate, 2%;
gas phase SiO2, 1%;
acrylated polysiloxane, 0.5%;
1% of tributyl phosphate;
0.5 percent of methyl phthalate;
weighing the above raw materials, mixing, heating to 90-120 deg.C, and stirring under electric power until all materials are dissolved to obtain uniform liquid, to obtain photosensitive organic vehicle.
(2) Preparing yellow silver paste:
spherical silver powder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃,according to the weight ratio of the conductive paste of 60 percent;
spherical silver powder (particle diameter 0.8um, specific surface area 1.02 g/m)2The tap density is 5.0g/cm3Surface organic matter is palmitic acid, burning loss is 0.6 percent at 538 ℃, and the weight ratio of the conductive paste is 30 percent;
glass powder (the component proportions are Bi2O 375%, SiO 212%, ZnO 5%, and other components 8%, Tg 438 ℃, Tf 510 ℃, and the particle size is 2um), and the weight ratio of the conductive paste is 1%;
9% of photosensitive organic carrier, fully stirring, grinding by a three-roll machine for 6 times to obtain uniformly dispersed conductive slurry.
(3) The performance test of the high-temperature sintered yellow conductive paste obtained in this embodiment is as follows:
the test conditions were the same as in example 1
Example 4 (comparative example 1)
(1) Preparing an organic carrier:
commercially available photopolymer inserman 9720, 60%;
photoinitiator TPO819, 4%
Diethylene glycol monoethyl ether acetate, 25%;
hexanediol diacrylate, 12%;
gas phase SiO2, 1%.
0.5 percent of modified polyether;
1.5 percent of methyl phthalate;
the organic carrier is obtained by weighing the components and the raw materials in weight ratio, mixing, heating to 90-120 ℃, and electrically stirring until all the materials are dissolved into uniform liquid.
(2) Preparing yellow silver paste:
spherical silver powder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃, and the weight ratio of the conductive paste is 63 percent;
spherical silver powder (particle diameter 0.9um, specific surface area 0.8 g/m)2The tap density is 5.0g/cm3Surface organic matter is oleic acid, burning loss is 0.5% at 538 deg.C, according to the conductive pasteThe material weight ratio is 20%;
glass powder (the component proportions are Bi2O 375%, SiO 212%, ZnO 5%, and other components 8%, Tg 438 ℃, Tf 510 ℃, and the particle size is 2um), and the weight ratio of the conductive paste is 1%;
16% of photosensitive organic carrier, fully stirring, grinding by a three-roll machine for 6 times to obtain uniformly dispersed conductive slurry.
(3) The performance test of the high-temperature sintered yellow conductive paste obtained in this embodiment is as follows:
the test conditions were the same as in example 1
Example 5 (comparative example 2):
(1) preparing a photosensitive organic carrier:
(2-methyl-1-oxo-1-phenylprop-2-yl) ethyl 2-methylpropan-2-enoate (3%), acrylic acid (7.5%), polyethylene glycol methacrylate (9%), propyl acrylate (7%), styrene (2%), azobisisobutyronitrile (0.5%) were ultrasonically dissolved and mixed. Adding ethylene glycol monomethyl ether acetate (71%) into a glass reaction kettle with a reflux condenser, introducing argon at 85 ℃ for protection and stirring, gradually dripping the mixture into the glass reaction kettle through a dropping funnel, keeping the temperature at 85 ℃, and stirring for 4 hours to obtain an intermediate.
Intermediate, 60%;
dimethyl adipate, 22%;
5% of ethylene glycol monoethyl ether acetate;
hexanediol diacrylate, 8%;
diethyl adipate, 2%;
gas phase SiO2, 1%;
acrylated polysiloxane, 0.5%;
1% of tributyl phosphate;
0.5 percent of methyl phthalate;
weighing the above raw materials, mixing, heating to 90-120 deg.C, and stirring under electric power until all materials are dissolved to obtain uniform liquid, to obtain photosensitive organic vehicle.
(2) Preparing yellow silver paste:
silver spheresPowder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃, and the weight ratio of the conductive paste is 83 percent;
glass powder (the component proportions are Bi2O 375%, SiO 212%, ZnO 5%, and other components 8%, Tg 438 ℃, Tf 510 ℃, and the particle size is 2um), and the weight ratio of the conductive paste is 2%;
15% of photosensitive organic carrier, fully stirring, grinding by a three-roll machine for 6 times to obtain uniformly dispersed conductive slurry.
(3) The performance test of the high-temperature sintered yellow conductive paste obtained in this embodiment is as follows:
the test conditions were the same as in example 1
Example 6 (comparative example 3):
(1) preparing a photosensitive organic carrier:
(2-methyl-1-oxo-1-phenylprop-2-yl) ethyl 2-methylpropan-2-enoate (3%), acrylic acid (7.5%), polyethylene glycol methacrylate (9%), propyl acrylate (7%), styrene (2%), azobisisobutyronitrile (0.5%) were ultrasonically dissolved and mixed. Adding ethylene glycol monomethyl ether acetate (71%) into a glass reaction kettle with a reflux condenser, introducing argon at 85 ℃ for protection and stirring, gradually dripping the mixture into the glass reaction kettle through a dropping funnel, keeping the temperature at 85 ℃, and stirring for 4 hours to obtain an intermediate.
Intermediate, 60%;
dimethyl adipate, 2%;
ethylene glycol monoethyl ether acetate, 15%;
hexanediol diacrylate, 18%;
diethyl adipate, 2%;
gas phase SiO2, 1%;
acrylated polysiloxane, 0.5%;
1% of tributyl phosphate;
0.5 percent of methyl phthalate;
weighing the above raw materials, mixing, heating to 90-120 deg.C, and stirring under electric power until all materials are dissolved to obtain uniform liquid, to obtain photosensitive organic vehicle.
(2) Preparing yellow silver paste:
spherical silver powder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃, and the weight ratio of the conductive paste is 63 percent;
spherical silver powder (particle diameter 0.9um, specific surface area 0.8 g/m)2The tap density is 5.0g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.5 percent at 538 ℃, and the weight ratio of the conductive slurry is 20 percent;
the glass powder for the commercially available conductive silver paste has the Tg of 550 ℃, the Tf of 630 ℃ and the particle size of 4 mu m, and is 5 percent of the weight of the conductive paste;
16% of photosensitive organic carrier, fully stirring, grinding by a three-roll machine for 6 times to obtain uniformly dispersed conductive slurry.
(3) The performance test of the high-temperature sintered yellow conductive paste obtained in this embodiment is as follows:
the test conditions were the same as in example 1
Example 7 (comparative example 4):
(1) preparing a photosensitive organic carrier:
the photosensitive organic vehicle was the same as in comparative example 2.
(2) Preparing yellow silver paste:
spherical silver powder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃, and the weight ratio of the conductive slurry is 30 percent;
spherical silver powder (particle diameter 0.9um, specific surface area 0.8 g/m)2The tap density is 5.0g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.5 percent at 538 ℃, and the weight ratio of the conductive slurry is 40 percent;
the glass powder for the commercially available conductive silver paste has the Tg of 550 ℃, the Tf of 630 ℃ and the particle size of 4 mu m, and is 5 percent of the weight of the conductive paste;
25% of photosensitive organic carrier, fully stirring, grinding by a three-roll machine for 6 times to obtain uniformly dispersed conductive slurry.
(3) The performance test of the high-temperature sintered yellow conductive paste obtained in this embodiment is as follows:
the test conditions were the same as in example 1
Example 8 (comparative example 5)
(1) Preparing a photosensitive organic carrier:
the photosensitive organic vehicle was the same as in example 1.
(2) Preparing yellow silver paste:
spherical silver powder (particle diameter 2.0um, specific surface area 0.4 g/m)2The tap density is 5.5g/cm3The organic matter on the surface is oleic acid, the burning loss is 0.7 percent at 538 ℃, and the weight ratio of the conductive slurry is 60 percent;
spherical silver powder (particle diameter 0.8um, specific surface area 0.7 g/m)2The tap density is 5.5g/cm3No surface organic matter, 0.15% of burning loss at 538 ℃ and 20% of the weight ratio of the conductive paste;
the glass powder for the commercially available conductive silver paste has the Tg of 550 ℃, the Tf of 630 ℃ and the particle size of 5 mu m, and is 5 percent of the weight of the conductive paste;
15% of photosensitive organic carrier, fully stirring, grinding by a three-roll machine, and grinding for 8 times to obtain the conductive slurry.
(3) The performance test of the high-temperature sintered yellow conductive paste obtained in this embodiment is as follows:
the test conditions were the same as in example 1
TABLE 1 comparison of the Properties of high-temperature sintered yellow conductive paste
Comparison of the above examples gives
Combining examples 1, 2, 3, and 5, it can be seen that when silver powder with small particle size is not added, the entire metal powder cannot be effectively densely packed due to steric effect of the powder itself, resulting in fewer conductive paths, greater resistance, and more through holes after sintering.
By combining the example 1, the example 2, the example 3 and the comparative example 6, it can be seen that when the solvent system cannot form a volatilization gradient, bumping is easy to occur in the glue removing process, so that the silver layer bulges and falls off, and further, the wire breakage and the overall adhesion are reduced.
Combining example 1, example 2, example 3, and comparative example 7, it can be concluded that when too much small particle size silver powder is added, the oil absorption value of the bulk metal powder is too high due to the high surface activity of the small particle size silver powder, making it difficult to match with the photosensitive carrier, resulting in the generation of agglomerates.
Combining examples 1, 2, 3, and 7 and 8, it can be seen that when the glass frit is excessive and the glass phase transition temperature and melting temperature properties thereof are changed, the adhesive property thereof is decreased, and the curing property is decreased, the silver powder and the glass frit cannot be well matched, and a large number of light-transmitting holes are formed. When the glass powder particle size is too big, can lead to unable good lines appearance that forms when exposing and developing, if the large granule glass powder remains between the line after the development, will form the short circuit, if the large granule glass powder is washed by the development, just forms the broken string easily.
Comparing example 1 with example 4, it can be seen that the photosensitive organic carrier of the present invention can be cross-linked and cured under the irradiation of ultraviolet light at a low content by adjusting the types and the proportions of the photosensitive key resin and the monomer, so as to achieve high resolution, achieve a line diameter and a line distance of 5 to 20um, and have a regular line shape and no burrs.
In conclusion, the high-temperature sintering type yellow light conductive paste provided by the invention has the advantages of good matching and uniform dispersion, and the formed conductive circuit has the advantages of small resistance, good adhesive force and small wire diameter.
Claims (9)
1. A preparation method of a conducting circuit is characterized by comprising the following steps:
printing the high-temperature sintered yellow-light conductive paste on a base material by a screen printing method, drying at the temperature of 100-150 ℃, carrying out 200-500mj energy exposure, developing by using a weak alkaline aqueous solution, carrying out glue discharge at the temperature of 350-450 ℃, then sintering at the temperature of 700-850 ℃, cooling at the cooling speed of 10-30 ℃/min,
the high-temperature sintered yellow light conductive paste comprises the following components in percentage by weight:
75-90% of noble metal powder;
1% -5% of glass powder;
8% -24% of a photosensitive organic carrier;
wherein the glass phase transition temperature Tg of the glass powder is 400-500 ℃, and the melting temperature Tf is 500-600 ℃.
2. The conductive circuit preparation method according to claim 1, wherein the noble metal powder is one or more of silver powder, gold powder, silver-palladium powder and silver-coated copper powder, and the noble metal powder is coated with fatty acid on the surface and comprises the following components in percentage by weight:
the average particle diameter is 1.5-2.5 μm, and the specific surface area is 0.7-1.5m270-95% of noble metal powder per gram,
average particle diameter of 0.7-1.5 μm, and specific surface area of 1.0-2.5m25-30% of noble metal powder per gram.
3. The method for producing a conductive line according to claim 2, wherein the fatty acid is an unsaturated fatty acid or a saturated fatty acid having twelve or more carbons.
4. The method for manufacturing a conductive circuit according to claim 1, characterized in that: the glass powder comprises the following components in percentage by weight
Bi2O3:70-90％；
SiO2:5-15％；
ZnO：5-20％；
The average grain diameter of the glass powder is 1-2 um.
5. The method for forming an electrically conductive line according to claim 1, wherein the photosensitive organic vehicle comprises, in weight percent:
photoinitiator (2): 1 to 8 percent;
hydrophilic monomer: 5 to 20 percent of
Hydrophobic monomer: 0.5 to 4 percent
Thermal initiator: 0.1 to 2.5 percent
Reaction solvent: 30 to 65 percent
Slurry solvent: 15 to 50 percent of
Additive: 0.5 to 10 percent.
6. The method for forming an electrically conductive trace according to claim 5, wherein the hydrophilic monomer and the hydrophobic monomer each contain a carbon-carbon double bond,
the hydrophilic monomer is one or more of polyethylene glycol methacrylate, ethylene glycol methacrylate, polyethylene glycol ethyl methacrylate, hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate and hydroxypropyl methacrylate,
the hydrophobic monomer is styrene, methyl methacrylate, methyl acrylate, ethyl methacrylate, ethyl acrylate, propyl methacrylate, propyl acrylate, n-butyl methacrylate, n-butyl acrylate, isobutyl methacrylate, isobutyl acrylate, isobutyl methacrylate, pentyl acrylate, n-hexyl methacrylate, n-hexyl acrylate, n-heptyl methacrylate, n-heptyl acrylate, n-octyl methacrylate, n-octyl acrylate, n-undecyl methacrylate, undecyl acrylate, tridecyl methacrylate, tridecyl acrylate, pentadecyl methacrylate, pentadecyl acrylate, hexadecyl methacrylate, hexadecyl acrylate, octadecyl methacrylate, octadecyl acrylate, eicosyl methacrylate, or mixtures thereof, One or more of eicosyl acrylate, docosyl methacrylate, docosyl acrylate.
7. The method for manufacturing a conductive circuit according to claim 6, wherein: the slurry solvent comprises a slurry solvent with a boiling point of 100-150 ℃, a boiling point of 150-250 ℃ and a boiling point of 250-300 ℃, wherein:
the weight percentage of the slurry solvent with the boiling point of 100-150 ℃ in the photosensitive organic carrier is 7-25 percent;
the weight percentage of the slurry solvent with the boiling point of 150-250 ℃ in the photosensitive organic carrier is 5-15 percent;
the slurry solvent with the boiling point of 250-300 ℃ accounts for 3-10% of the weight of the photosensitive organic carrier.
8. The method for manufacturing a conductive circuit according to claim 6, wherein: the additive comprises: thixotropic agent, leveling agent, defoaming agent and plasticizer, wherein,
the thixotropic agent accounts for 0.5 to 2 percent of the mass percent of the photosensitive organic carrier;
the mass percentage of the flatting agent in the photosensitive organic carrier is 0.5-2%;
the defoaming agent accounts for 1-3% of the photosensitive organic carrier by mass;
the plasticizer accounts for 0.1 to 3 percent of the mass of the photosensitive organic carrier.
9. The method for manufacturing the conductive circuit according to any one of claims 1 to 8, wherein the high-temperature sintering type yellow conductive paste is manufactured by a method comprising
Step A: preparation of photosensitive organic vehicle: carrying out ultrasonic mixing on a photoinitiator, a hydrophilic monomer, a hydrophobic monomer and a thermal initiator to obtain a homogeneous mixture; dripping the homogeneous mixture into a reaction solvent preheated to 80-90 ℃, stirring and reacting at the temperature, introducing inert gas for protection to obtain an intermediate, and then uniformly mixing and stirring the intermediate, a slurry solvent and an additive to obtain a photosensitive organic carrier;
and B: and B, mixing and stirring the photosensitive organic carrier in the step A, glass powder and noble metal powder according to a weight ratio, and then fully grinding to obtain the high-temperature sintering type yellow light conductive paste.
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Correction item: Patentee|Address|Patentee Correct: Qianyu Electronic Materials (Suzhou) Co.,Ltd.|215011 room 807, floor 8, building 4, No. 209, Zhuyuan Road, high tech Zone, Suzhou, Jiangsu Province|HANYU ELECTRONIC MATERIAL (SHENZHEN) Co.,Ltd.|QIANYE TECHNOLOGY DEVELOPMENT (DONGGUAN) Co.,Ltd. False: Qianyu Micro Nano Technology (Shenzhen) Co.,Ltd.|518000 Building 1, Hengtai Yu Building, Tangwei Community, Fenghuang Street, Guangming District, Shenzhen City, Guangdong Province, 514-2 (one photo multi site enterprise)|HANYU ELECTRONIC MATERIAL (SHENZHEN) Co.,Ltd. Number: 18-02 Volume: 39 |
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| CP01 | Change in the name or title of a patent holder |
Address after: 215011 room 807, floor 8, building 4, No. 209, Zhuyuan Road, high tech Zone, Suzhou, Jiangsu Province Patentee after: Qianyu Electronic Materials (Suzhou) Co.,Ltd. Patentee after: Qianyu Micro Nano Technology (Shenzhen) Co.,Ltd. Patentee after: QIANYE TECHNOLOGY DEVELOPMENT (DONGGUAN) Co.,Ltd. Address before: 215011 room 807, floor 8, building 4, No. 209, Zhuyuan Road, high tech Zone, Suzhou, Jiangsu Province Patentee before: Qianyu Electronic Materials (Suzhou) Co.,Ltd. Patentee before: HANYU ELECTRONIC MATERIAL (SHENZHEN) Co.,Ltd. Patentee before: QIANYE TECHNOLOGY DEVELOPMENT (DONGGUAN) Co.,Ltd. |
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| TR01 | Transfer of patent right |
Effective date of registration: 20230807 Address after: 518000 Building 1, Hengtai Yu Building, Tangwei Community, Fenghuang Street, Guangming District, Shenzhen City, Guangdong Province, 514-2 (one photo multi site enterprise) Patentee after: Qianyu Micro Nano Technology (Shenzhen) Co.,Ltd. Patentee after: Qianyu Electronic Materials (Suzhou) Co.,Ltd. Address before: 215011 room 807, floor 8, building 4, No. 209, Zhuyuan Road, high tech Zone, Suzhou, Jiangsu Province Patentee before: Qianyu Electronic Materials (Suzhou) Co.,Ltd. Patentee before: Qianyu Micro Nano Technology (Shenzhen) Co.,Ltd. Patentee before: QIANYE TECHNOLOGY DEVELOPMENT (DONGGUAN) Co.,Ltd. |