CN106024100A - Low-temperature conductive silver paste and preparation method and application thereof - Google Patents
Low-temperature conductive silver paste and preparation method and application thereof Download PDFInfo
- Publication number
- CN106024100A CN106024100A CN201610571169.1A CN201610571169A CN106024100A CN 106024100 A CN106024100 A CN 106024100A CN 201610571169 A CN201610571169 A CN 201610571169A CN 106024100 A CN106024100 A CN 106024100A
- Authority
- CN
- China
- Prior art keywords
- silver paste
- low
- conductive silver
- temperature conductive
- silver
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 161
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 22
- 229920005989 resin Polymers 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000003431 cross linking reagent Substances 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 229920000180 alkyd Polymers 0.000 claims description 5
- -1 alkyl phenol Chemical compound 0.000 claims description 5
- 229920003063 hydroxymethyl cellulose Polymers 0.000 claims description 5
- 229940031574 hydroxymethyl cellulose Drugs 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920002907 Guar gum Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000001913 cellulose Chemical class 0.000 claims description 3
- 229920002678 cellulose Chemical class 0.000 claims description 3
- HGAZMNJKRQFZKS-UHFFFAOYSA-N chloroethene;ethenyl acetate Chemical compound ClC=C.CC(=O)OC=C HGAZMNJKRQFZKS-UHFFFAOYSA-N 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 239000000665 guar gum Substances 0.000 claims description 3
- 235000010417 guar gum Nutrition 0.000 claims description 3
- 229960002154 guar gum Drugs 0.000 claims description 3
- PHNWGDTYCJFUGZ-UHFFFAOYSA-N hexyl dihydrogen phosphate Chemical compound CCCCCCOP(O)(O)=O PHNWGDTYCJFUGZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 3
- JHJUUEHSAZXEEO-UHFFFAOYSA-M sodium;4-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C=C1 JHJUUEHSAZXEEO-UHFFFAOYSA-M 0.000 claims description 3
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 claims 1
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 abstract description 25
- 239000004332 silver Substances 0.000 abstract description 25
- 239000002245 particle Substances 0.000 abstract description 13
- 238000005452 bending Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002042 Silver nanowire Substances 0.000 abstract 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000010408 film Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 5
- 239000002070 nanowire Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- VKEQBMCRQDSRET-UHFFFAOYSA-N Methylone Chemical compound CNC(C)C(=O)C1=CC=C2OCOC2=C1 VKEQBMCRQDSRET-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical class CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- FEPBITJSIHRMRT-UHFFFAOYSA-N 4-hydroxybenzenesulfonic acid Chemical compound OC1=CC=C(S(O)(=O)=O)C=C1 FEPBITJSIHRMRT-UHFFFAOYSA-N 0.000 description 1
- 235000003826 Artemisia Nutrition 0.000 description 1
- 235000003261 Artemisia vulgaris Nutrition 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- PHOQVHQSTUBQQK-SQOUGZDYSA-N D-glucono-1,5-lactone Chemical compound OC[C@H]1OC(=O)[C@H](O)[C@@H](O)[C@@H]1O PHOQVHQSTUBQQK-SQOUGZDYSA-N 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 244000030166 artemisia Species 0.000 description 1
- 235000009052 artemisia Nutrition 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 235000012209 glucono delta-lactone Nutrition 0.000 description 1
- 229960003681 gluconolactone Drugs 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 description 1
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 description 1
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 description 1
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- VQEHIYWBGOJJDM-UHFFFAOYSA-H lanthanum(3+);trisulfate Chemical compound [La+3].[La+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VQEHIYWBGOJJDM-UHFFFAOYSA-H 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- 238000004017 vitrification 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
- H01B1/20—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
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The invention discloses low-temperature conductive silver paste and a preparation method and application thereof. Silver nano wires and silver powder in conventional conductive silver paste are mixed to form novel low temperature conductive silver paste. The content of silver powder in conventional conductive silver paste is greatly reduced, and a few silver nano wires play good conductive effect. Conventional conductive silver paste requires circular silver particles which contact point-to-point to realize conduction, the silver nano wires can serially connect original silver particles, and the silver nano wires form a conductive network in a network shape. Conductive films, conductive switches, flexible print circuit boards, electromagnetic shields, potentiometers, wireless radio frequency identification systems and solar cells formed by the low-temperature conductive silver paste have better bending resistance performance.
Description
Technical field
The present invention relates to conductive silver paste technical field, particularly relate to a kind of low-temperature conductive silver paste and preparation method thereof and
Application.
Background technology
In recent years, along with developing rapidly of electronics industry, thin film switch, flexible printed circuit board, electromagnetic shielding, current potential
The demand of device, radio frequency identification system, solaode etc. is increasing sharply, and conductive silver paste is as preparing this electron-like
The key function material of components and parts, its development and application also get more and more people's extensive concerning.According to analysis, only conductive silver paste market and
Speech, has the market scale of multi-million dollar every year.In the high speed development process of information industry, slurry is as a kind of crucial material
Material has consequence.High-performance, low cost not only can greatly improve the competitiveness of product, are also that electric slurry is sent out simultaneously
The inexorable trend of exhibition.
Along with the development of microelectronic component technology, for preparing the requirement of the thick-film electronic silver electronic paste of electrode
It is: good conductivity；Slurry printing fine line；Sintering or baking temperature is the lowest more good；Cost of sizing agent is low；Adhesive force wants height；Wear-resisting
Property is good；The most leaded harmful element such as grade, meets environmental requirement etc..
According to statistics, whole nation Ge great electric slurry company competitively releases the silver electrode electrocondution slurry of oneself in recent years, and it is annual
The output value all more than billions of dollars, and this scale is along with the development of electronics industry is in the trend increased year by year.
Wherein, low-temperature cured conductive silver slurry is the one in silver slurry, refers to the class silver slurry that solidification temperature is relatively low, can print
On vitrification point plastics relatively low and with low cost or flexible board, this kind of conductive silver paste should have the electric conductivity of excellence, resistance to
Bending property, adhesive force and certain hardness, be widely used in carbon-film potentiometer, circle (or lamellar) tantalum capacitor, thin film switch/
The aspect such as flexible circuit, conducting resinl.Low-temperature cured conductive silver slurry is usually by silver powder, macromolecule resin Binder Phase, solvent
And other auxiliary agents mix under certain mechanical force, the freedom that its conducting function provides mainly by the argentum powder particle added
Electronic carrier realizes.
In commercial Application, the shape of argentum powder is usually lamellar or spherical.With face or linear contact lay, Ke Yiti between flake silver powder
High silver slurry electric conductivity, it is thus achieved that the silver slurry of low silver content high conductivity, such silver slurry more application is in the electricity such as thin film switch, wave filter
Sub-components and parts, shortcoming is that silver starches printability and bending resistance folding endurance can decline accordingly.And general, flake silver powder made silver slurry
Argentum powder content is 50～60wt%.With point cantact between spherical argentum powder, silver slurry rheological characteristic can be improved, it is adaptable to printing characteristic and
The occasion that the mechanical performances such as bending resistance folding endurance have higher requirements, shortcoming is that electric conductivity can decline accordingly, it is therefore desirable to higher silver
Content (general silver slurry argentum powder content reaches 60～83%), not only increases production cost, and high solids content also can cause slurry to glue
Degree rises affects printability in turn.
Therefore, the present inventor needs a kind of new technique of design badly to improve its problem.
Summary of the invention
It is desirable to provide a kind of low-temperature conductive silver paste and its preparation method and application, it both can reduce argentum powder and admittedly contain
Amount, can guarantee that again electric conductivity and bend-resistance performance simultaneously.
For solving above-mentioned technical problem, the technical scheme is that
A kind of low-temperature conductive silver paste, including the raw material of following weight portion:
Preferably, described resin is modified epoxy, TDI modified alkyd resin, propylene glycol methyl ether acetate, ethylene glycol
One or more in ether acetate, vinyl chloride-vinyl acetate resin and acrylic resin.
Preferably, described surfactant is alkylphenol polyoxyethylene, isomeric alcohol polyethenoxy ether, lauryl sulphate acid
One or more in sodium, dodecylbenzene sodium sulfonate.
Preferably, described dispersant is polyvinylpyrrolidone, triethyl group hexyl phosphoric acid, sodium lauryl sulphate, methyl
One or more in amylalcohol, cellulose derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester.
Preferably, described cross-linking agent is organosilicon cross-linking agent.
Preferably, a length of 10-40 μm of described nano silver wire, diameter of section is 20-80nm.
Preferably, one or more during described carrier solvent is isopropanol, water, ethanol.
Preferably, described argentum powder is spherical argentum powder.
A kind of preparation method based on low-temperature conductive silver paste described above, comprises the steps:
S1: nano silver wire is mixed homogeneously according to aforementioned proportion with argentum powder；
S2: proportionally surfactant, dispersant, resin, hydroxymethyl cellulose, cross-linking agent, levelling agent are joined
In carrier solvent, stir, rise high-temperature and be 75-80 DEG C, stirring mixing 10-13 minute, obtain organic carrier；
S3: join in organic carrier by the mixed liquor of argentum powder nano silver wire Yu argentum powder, sends into and carries out on three-roll grinder
Mixing, ground slurry granularity, to 8-15 micron, gets product.
The application of a kind of low-temperature conductive silver paste, by low-temperature conductive silver paste described above or low-temperature conductive silver paste preparation method
The low-temperature conductive silver paste prepared is applied to conductive film, conductive switch, flexible printed circuit board, electromagnetic shielding, potentiometer, nothing
Line radio-frequency recognition system, solaode preparation in.
Using technique scheme, the present invention at least includes following beneficial effect:
Low-temperature conductive silver paste of the present invention and its preparation method and application, selects nano silver wire and traditional conductive silver
Argentum powder mixing in slurry, forms new low-temperature conductive silver paste, and it can be greatly reduced the content of argentum powder in conventional conductive silver slurry, few
It is to need circular Argent grain point-to-point that the nano silver wire of amount plays the electric action arrived very much, i.e. conventional conductive silver slurry wherein
Contact could be conducted electricity, and the addition of nano silver wire can be connected original Argent grain, and nano silver wire is formed as netted simultaneously
Conductive network.And use conductive film that this low-temperature conductive silver paste formed, conductive switch, flexible printed circuit board, electromagnetic screen
Cover, the folding resistance such as potentiometer, radio frequency identification system, solaode more excellent.
Detailed description of the invention
Below by way of specific instantiation, embodiments of the present invention being described, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also be by the most different concrete realities
The mode of executing is carried out or applies, the every details in this specification can also based on different viewpoints and application, without departing from
Various modification or change is carried out under the spirit of the present invention.
A kind of low-temperature conductive silver paste, including the raw material of following weight portion:
Preferably, table 1 is seen, including below embodiment:
Table 1
Preferably, described resin is modified epoxy, TDI modified alkyd resin, propylene glycol methyl ether acetate, ethylene glycol
One or more in ether acetate, vinyl chloride-vinyl acetate resin and acrylic resin.
Preferably, described surfactant is alkylphenol polyoxyethylene, isomeric alcohol polyethenoxy ether, lauryl sulphate acid
One or more in sodium, dodecylbenzene sodium sulfonate.
Preferably, described dispersant is polyvinylpyrrolidone, triethyl group hexyl phosphoric acid, sodium lauryl sulphate, methyl
One or more in amylalcohol, cellulose derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester.
Preferably, described cross-linking agent is organosilicon cross-linking agent.
Preferably, a length of 10-40 μm of described nano silver wire, diameter of section is 20-80nm.Most preferably silver is received
A length of 30 μm of rice noodle, diameter of section is 50nm.
Preferably, one or more during described carrier solvent is isopropanol, water, ethanol.
Preferably, described argentum powder is spherical argentum powder.
It is known that in conductive silver powder, size is crucial on the impact of conductive silver paste electric conductivity.Argentum powder
The particle diameter of grain is the least, and resistivity is the least, and the temperature needed for its solidification is the lowest.If the particle diameter of silver powder particles is excessive, argentum powder ionic bond
Contact rate the lowest, the space between example is likely to be filled by resin-bonded phase, significantly hinders the conduction of continuous-stable
Path and formed, cause the conductive silver paste poorly conductive after solidification, resistance rises.Meanwhile, when silk screen printing probably due to
Particle diameter is excessive and normal through silk screen, can not can have a strong impact on printing and the coating of silver slurry.But, if on the other hand silver
The particle diameter of powder particles is too small, and the surface of particle can be bigger, it is easy to is formed and reunites, thus affects argentum powder dispersion in the slurry.
Therefore size is very important on the impact of electric conductivity.
Nano wire is the line of a kind of nanoscale.Being said differently, nano wire can be defined as one to be had laterally
On be limited in the one-dimentional structure of below 100 nanometers (longitudinally do not limit).According to the difference of composition material, nano wire can be divided into
Different types, including metal nanometer line (such as: Ni, Pt, Au etc.), semiconductor nanowires (such as: InP, Si, GaN etc.) and insulation
Body nano wire (such as: SiO2, TiO2 etc.).Nano silver wire is the one of metal nanometer line, in addition to there is the electric conductivity that silver is excellent,
Simultaneously because the dimensional effect of Nano grade, also there is the light transmission of excellence, flexible resistance.The present invention selects nano silver wire and biography
Argentum powder mixing in the conductive silver paste of system, forms new low-temperature conductive silver paste, and it can be greatly reduced silver in conventional conductive silver slurry
The content of powder, it is to need circular silver that a small amount of nano silver wire plays good electric action, i.e. conventional conductive silver slurry wherein
The point-to-point contact of granule could be conducted electricity, and the addition of nano silver wire can be connected original Argent grain, and nano silver wire is such as simultaneously
Netted equally form conductive network.
In order to avoid the reunion of particle, the present invention selects use polyvinylpyrrolidone (polyvinyl
Pyrrolidone, is called for short PVP, is a kind of non-ionic macromolecule compound) as dispersant.Because each structure of PVP molecule
Unit has a pyrrole radicals, can adsorb behind the surface of nano-Ag particles, due to steric effect can suppress nano-Ag particles because of
Collision that random motion produces and the bulky grain that agglomerates into, keep its stability in the solution.Thus reach scattered
Purpose.I.e. select PVP, the size of nano-particle can well be controlled, and make it not reunite, play extraordinary surely
It is set for using.
Except argentum powder, resin-bonded phase is also the critical material determining low-temperature conductive silver paste performance, determines conduction simultaneously
The combination properties such as the pliability of silver slurry, hardness, adhesive force, bend-resistance.
In a preferred embodiment, described resin is modified epoxy, and it is with isocyanate terminated polyurethane as toughener,
Reacted with the secondary hydroxyl on epoxy resin by terminal isocyanate group, epoxy resin introduces the ehter bond of people's toughness, thus changes
The toughness of kind epoxy resin.Good adhesive force is had, print between conductive silver paste and the PET film prepared with modified epoxy
The conducting wire bending resistance folding endurance of system has reached 10000 times, greatly improves the performance of flexible circuit board.
In another preferred embodiment, described resin is TDI modified alkyd resin and modified epoxy is used in mixed way, its
Not only having good adhesive force and bending resistance folding endurance, in terms of drying property and hardness, relatively ordinary resin is significantly improved, surface drying
Time shortens to 30min from 5-6h, and the time of doing solid work shortens to 4h from 15-18h, substantially increases efficiency.
Owing to nano silver wire is easily dispersed in isopropanol, aqueous solution, the dispersion that ethanol solution also can be suitable, the most preferably carry
Body solvent is aqueous solution.In view of the low content of nano silver wire, therefore the content of resin is lower, between 1-5 part, it is to avoid too much
Embedding nano silver wire and non-conductive after causing cured later.A small amount of hydroxymethyl cellulose, has thickening power, provides viscous after solidification
Relay.
Heretofore described levelling agent preferably includes following component:
Butyl acrylate 5-10 part,
Siloxane-Oxyalkylene Copolymers 3-9 part,
Tetrasodium pyrophosphate 2-7 part,
Sodium chloride 3-7 part,
Bamboo powder 4-9 part,
Curing polyester resin 2-7 part,
Epoxy resin 3-9 part.
This levelling agent has preferable levelability and decoration performance, accelerates and the volatilization of balanced solvent, can reduce and produce
Absorption to dust in journey, improves the releasability of solvent, accelerates and the volatilization of balanced solvent, promotes levelling and feel.
A kind of preparation method based on low-temperature conductive silver paste described above, comprises the steps:
1: nano silver wire is mixed homogeneously according to aforementioned proportion with argentum powder；
S2: proportionally surfactant, dispersant, resin, hydroxymethyl cellulose, cross-linking agent, levelling agent are joined
In carrier solvent, stir, rise high-temperature and be 75-80 DEG C, stirring mixing 10-13 minute, obtain organic carrier；
S3: join in organic carrier by the mixed liquor of argentum powder nano silver wire Yu argentum powder, sends into and carries out on three-roll grinder
Mixing, ground slurry granularity, to 8-15 micron, gets product.
The application of a kind of low-temperature conductive silver paste, by low-temperature conductive silver paste described above or low-temperature conductive silver paste preparation method
The low-temperature conductive silver paste prepared is applied to conductive film, conductive switch, flexible printed circuit board, electromagnetic shielding, potentiometer, nothing
Line radio-frequency recognition system, solaode preparation in.
The experiment effect of the present invention can be proved by following contrast experiment:
Sample 1, a kind of low-temperature conductive silver paste, including cladding argentum powder 80-90, ethyl cellulose 6-10, methylcellulose 6-
8, ethylene glycol monobutyl ether 10-13, carbitol 10-12, p-hydroxybenzenyl sulfonate 0.1-0.2, polyoxyethylene polyoxypropylene propylene glycol
0.5-1, titanium nitride 0.6-1, polyadipate ethylene glycol 0.8-1, gluconolactone 0.4-1, artemisia glue 1-2, lead-free glass powder 10-
13, aluminium oxide 1-2, methyl-silicone oil 0.2-0.3, phthalandione butyl benzyl ester 2-3；
Described cladding argentum powder is made up of the raw material of following weight parts:
Nano-sized iron oxide 4-6, lanthanum sulfate 0.1-0.2, deionized water 300-400, butyl acrylate 10-13, carboxymethyl are fine
Dimension element sodium 0.9-2, silane coupler KH560 0.06-0.1, benzoyl peroxide 0.01-0.02, ascorbic acid 45-60, Semen sophorae
Glue 1-2, sodium tetraborate 0.1-0.14, silver nitrate 100-110；
Sample 2, a kind of conductive silver paste, comprise nano silver wire aqueous dispersions 60～80 parts, 0.5% hydroxypropyl methyl cellulose
Aqueous solution 2～8 parts, 1% polyvinyl alcohol water solution 2～8 parts, 5% water-soluble resin liquid 5～10 parts, cross-linking agent XR-501 0.5
～1 part, levelling agent 0.5～1 part, high 670 dispersants 0.4 of enlightening～0.8 part, high 845 defoamer 0.3 of enlightening～0.6 part.
Sample 3, a kind of low temperature-sintered nano silver paste, nanometer silver paste component is as follows with weight mass percent: mean diameter
It it is the nanometer silver powder 78.5～89.5% of 20～50nm；Organic carrier polyvinyl alcohol 5.0～10.0%；Organic solvent citric acid three
Butyl ester 5.0～10.0%；Surfactant rosin acid 0.5～1.5%.
Sample 4, a kind of conductive nano silver slurry, it is made up of the component comprising following weight portion: nanometer silver 0.5～5 parts；Resin
10～30 parts；Dispersant 0.01～2 parts；Surface modifier 0.01～2 parts；Anti-settling agent 0.01～2 parts；Levelling agent 0.01～2 parts；Receive
Rice auxiliary agent 0.1～2 parts；Thickening agent 0.5～2 parts；Organic solvent 50～95 parts；Pigment 0.01～10 parts；Firming agent 0.01～5
Part.
Sample 5a, the low-temperature conductive silver paste described in embodiment 1.
Sample 5b, the low-temperature conductive silver paste described in embodiment 2.
Sample 5c, the low-temperature conductive silver paste described in embodiment 3, wherein said resin is modified epoxy.
Sample 5d, the low-temperature conductive silver paste described in embodiment 4, wherein said resin is TDI modified alkyd resin and modification
Epoxy resin is used in mixed way according to the ratio of 1:1.
Above-mentioned sample 1-5 is used for printed circuit board (PCB), and experimental result sees table 2.
Table 2
By above-mentioned contrast test, we are it appeared that the low-temperature conductive silver paste of the present invention is for printed circuit board (PCB), and it is solid
Change temperature and be significantly lower than other samples, process costs and difficulty can be reduced.Folding resistance and adhesive force are all substantially better than on market
Conductive silver paste, performance is more excellent.And surface drying time and time of doing solid work all are greatly shortened, greatly improve efficiency.Separately
Outer surface resistance is relatively low, and electric energy loss is less, and electric conductivity is good.What is more important, still will not be at table without defoamer
Face produces bubble, saves production cost while improving product presentation quality.The electric conductivity of nano silver wire is relatively good, a small amount of
Application can keep good electric conductivity, the most cost-effective.And need the content of argentum powder relatively low, also will not produce a huge sum of money
Belonging to and polluting, environmental-protecting performance is good, has preferable market application foreground.
For such as conductive film, conductive switch, electromagnetic shielding, potentiometer, radio frequency identification system, solaode
Deng, use low-temperature conductive silver paste of the present invention all can obtain preferable technique effect, those skilled in the art can be led to
The experiment crossing limited number of time is known, the present invention does not repeats them here.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It is right to it should be pointed out that,
For those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out
Some improvement and modification, these improve and modify in the protection domain that also should fall into the claims in the present invention.
Described above to the disclosed embodiments, makes those skilled in the art be capable of or uses the present invention.To this
The multiple amendment of a little embodiments will be apparent from for those skilled in the art, as defined herein typically
Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention will not
Can be intended to be limited to the embodiments shown herein, and be to fit to consistent with principles disclosed herein and features of novelty
The widest scope.
Claims (10)
1. a low-temperature conductive silver paste, it is characterised in that include the raw material of following weight portion:
Nano silver wire 0.1-1 part；
Argentum powder 20-35 part；
Surfactant 0.1-5 part；
Dispersant 1-3 part；
Resin 1-5 part；
Hydroxymethyl cellulose 1-2 part；
Cross-linking agent 0.5-1 part；
Levelling agent 1-3 part；
Carrier solvent 50-75 part.
2. low-temperature conductive silver paste as claimed in claim 1, it is characterised in that: described resin is modified epoxy, TDI modification
One in alkyd resin, propylene glycol methyl ether acetate, ethyl cellosolve acetate, vinyl chloride-vinyl acetate resin and acrylic resin or many
Kind.
3. low-temperature conductive silver paste as claimed in claim 1 or 2, it is characterised in that: described surfactant is alkyl phenol polyoxy
One or more in vinyl Ether, isomeric alcohol polyethenoxy ether, sodium lauryl sulphate, dodecylbenzene sodium sulfonate.
4. the low-temperature conductive silver paste as described in claim 1-3 is arbitrary, it is characterised in that: described dispersant is polyvinylpyrrolidine
Ketone, triethyl group hexyl phosphoric acid, sodium lauryl sulphate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum, fat
One or more in acid polyethylene glycol ester.
5. the low-temperature conductive silver paste as described in claim 1-4 is arbitrary, it is characterised in that: described cross-linking agent is organosilicon crosslinked
Agent.
6. the low-temperature conductive silver paste as described in claim 1-5 is arbitrary, it is characterised in that: a length of 10-of described nano silver wire
40 μm, diameter of section is 20-80nm.
7. the low-temperature conductive silver paste as described in claim 1-6 is arbitrary, it is characterised in that: described carrier solvent be isopropanol, water,
One or more in ethanol.
8. the low-temperature conductive silver paste as described in claim 1-7 is arbitrary, it is characterised in that: described argentum powder is spherical argentum powder.
9. a preparation method based on the arbitrary described low-temperature conductive silver paste of claim 1-8, it is characterised in that include as follows
Step:
S1: nano silver wire is mixed homogeneously according to aforementioned proportion with argentum powder；
S2: proportionally surfactant, dispersant, resin, hydroxymethyl cellulose, cross-linking agent, levelling agent are joined carrier
In solvent, stir, rise high-temperature and be 75-80 DEG C, stirring mixing 10-13 minute, obtain organic carrier；
S3: join in organic carrier by the mixed liquor of argentum powder nano silver wire Yu argentum powder, sends into and mixes on three-roll grinder,
Ground slurry granularity, to 8-15 micron, gets product.
10. the application of a low-temperature conductive silver paste, it is characterised in that: by arbitrary for claim 1-8 described low-temperature conductive silver paste
Or the low-temperature conductive silver paste that the low-temperature conductive silver paste preparation method described in claim 9 is prepared is applied to conductive film, conduction
Switch, flexible printed circuit board, electromagnetic shielding, potentiometer, radio frequency identification system, solaode preparation in.
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