CN114974658A - High-adhesion low-temperature silver paste for fluorocarbon film and preparation method thereof - Google Patents
High-adhesion low-temperature silver paste for fluorocarbon film and preparation method thereof Download PDFInfo
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- CN114974658A CN114974658A CN202210733335.9A CN202210733335A CN114974658A CN 114974658 A CN114974658 A CN 114974658A CN 202210733335 A CN202210733335 A CN 202210733335A CN 114974658 A CN114974658 A CN 114974658A
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- silver paste
- resin
- fluorocarbon film
- temperature
- fluorocarbon
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 85
- 239000004332 silver Substances 0.000 title claims abstract description 85
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 48
- 229920005989 resin Polymers 0.000 claims abstract description 34
- 239000011347 resin Substances 0.000 claims abstract description 34
- 239000013034 phenoxy resin Substances 0.000 claims abstract description 27
- 229920006287 phenoxy resin Polymers 0.000 claims abstract description 27
- 239000003960 organic solvent Substances 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 19
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 18
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011737 fluorine Substances 0.000 claims abstract description 18
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 18
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 17
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical class CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 15
- 239000002952 polymeric resin Substances 0.000 claims abstract description 15
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 239000006185 dispersion Substances 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 28
- 239000002245 particle Substances 0.000 claims description 24
- 238000001723 curing Methods 0.000 claims description 23
- 239000011159 matrix material Substances 0.000 claims description 18
- 238000005303 weighing Methods 0.000 claims description 13
- 239000006254 rheological additive Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 6
- 229910021485 fumed silica Inorganic materials 0.000 claims description 6
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 claims description 5
- 239000004952 Polyamide Substances 0.000 claims description 5
- 239000012948 isocyanate Substances 0.000 claims description 5
- 150000002513 isocyanates Chemical class 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- 229920002620 polyvinyl fluoride Polymers 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- KKYDYRWEUFJLER-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F KKYDYRWEUFJLER-UHFFFAOYSA-N 0.000 claims description 4
- PAAZPARNPHGIKF-UHFFFAOYSA-N 1,2-dibromoethane Chemical compound BrCCBr PAAZPARNPHGIKF-UHFFFAOYSA-N 0.000 claims description 4
- LBTSNEJGMVFUEW-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,8,8,8-dodecafluorooctoxy-dimethoxy-propylsilane Chemical compound FC(C(C(C(C(F)(F)CO[Si](OC)(OC)CCC)(F)F)(F)F)(F)F)CC(F)(F)F LBTSNEJGMVFUEW-UHFFFAOYSA-N 0.000 claims description 4
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-UHFFFAOYSA-N 0.000 claims description 4
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 claims description 4
- 229920009638 Tetrafluoroethylene-Hexafluoropropylene-Vinylidenefluoride Copolymer Polymers 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- XTDYIOOONNVFMA-UHFFFAOYSA-N dimethyl pentanedioate Chemical compound COC(=O)CCCC(=O)OC XTDYIOOONNVFMA-UHFFFAOYSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 4
- 150000002460 imidazoles Chemical class 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- BPCXHCSZMTWUBW-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F BPCXHCSZMTWUBW-UHFFFAOYSA-N 0.000 claims description 4
- IJROHELDTBDTPH-UHFFFAOYSA-N trimethoxy(3,3,4,4,5,5,6,6,6-nonafluorohexyl)silane Chemical compound CO[Si](OC)(OC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)F IJROHELDTBDTPH-UHFFFAOYSA-N 0.000 claims description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 4
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 claims description 4
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 3
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims description 3
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 claims description 3
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- FJDJVBXSSLDNJB-LNTINUHCSA-N cobalt;(z)-4-hydroxypent-3-en-2-one Chemical compound [Co].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O FJDJVBXSSLDNJB-LNTINUHCSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- 230000009477 glass transition Effects 0.000 claims description 3
- 239000003094 microcapsule Chemical class 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 239000013008 thixotropic agent Substances 0.000 claims description 3
- PMQIWLWDLURJOE-UHFFFAOYSA-N triethoxy(1,1,2,2,3,3,4,4,5,5,6,6,7,7,10,10,10-heptadecafluorodecyl)silane Chemical compound CCO[Si](OCC)(OCC)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)CCC(F)(F)F PMQIWLWDLURJOE-UHFFFAOYSA-N 0.000 claims description 3
- NYIKUOULKCEZDO-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,6-nonafluorohexyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)F NYIKUOULKCEZDO-UHFFFAOYSA-N 0.000 claims description 3
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 claims description 2
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims 1
- 238000005452 bending Methods 0.000 abstract description 8
- 230000009471 action Effects 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000002966 varnish Substances 0.000 description 3
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 239000002318 adhesion promoter Substances 0.000 description 2
- 239000000440 bentonite Substances 0.000 description 2
- 229910000278 bentonite Inorganic materials 0.000 description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 2
- 229920006026 co-polymeric resin Polymers 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920005749 polyurethane resin Polymers 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- OQMIRQSWHKCKNJ-UHFFFAOYSA-N 1,1-difluoroethene;1,1,2,3,3,3-hexafluoroprop-1-ene Chemical group FC(F)=C.FC(F)=C(F)C(F)(F)F OQMIRQSWHKCKNJ-UHFFFAOYSA-N 0.000 description 1
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000000007 visual effect Effects 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
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Conductive Materials (AREA)
- Paints Or Removers (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a high-adhesion low-temperature silver paste for a fluorocarbon film and a preparation method thereof, wherein the low-temperature silver paste comprises the following components in parts by weight: high-molecular resin: 4-15 parts; organic solvent: 5-35 parts; curing the crosslinking agent: 0.2-2 parts of a solvent; rheological aid: 0.5-5 parts; tackifier: 0.5-5 parts; conductive powder: 45-80 parts of a solvent; the high polymer resin is a combination of phenoxy resin and fluorocarbon resin, so that the low-temperature silver paste is flexible and bending-resistant and is matched with the flexibility of the fluorocarbon film material, the fluorocarbon resin has good adhesion to the fluorocarbon film material, and the phenoxy resin has higher polarity, so that the adhesion force of the low-temperature silver paste and the fluorocarbon film material can be effectively improved by the phenoxy resin and the fluorocarbon resin; the tackifier is the combination of fluorine-containing siloxane, a silane coupling agent and acetylacetone salt, and the compatibility of the fluorine-containing siloxane and the fluorocarbon film material is utilized to generate a synergistic effect of adhesion promotion with the bridging action of the silane coupling agent and the acetylacetone salt, so that the stable adhesion of the polymer resin and the conductive powder to the fluorocarbon film material is effectively ensured.
Description
Technical Field
The invention relates to a high-adhesion low-temperature silver paste for a fluorocarbon film and a preparation method thereof, belonging to the technical field of paste.
Background
The low-temperature silver paste is also called polymer conductive silver paste, and is a viscous uniform mixture formed by using high-molecular resin as a binding phase, silver powder as conductive powder and a solvent and an auxiliary agent as auxiliary materials. The low-temperature silver paste is dried or solidified at the temperature of below 200 ℃, and the solvent is volatilized to form a binding phase film, so that a circuit with a conductive function is formed. Compared with sintered conductive silver paste taking glass powder as a binder phase, the low-temperature silver paste can be applied to flexible base materials which cannot be subjected to high-temperature sintering, such as PET, TPU, Teslin, fiber fabrics and the like, and is one of essential base materials in the field of electronic technology at present.
As electronic technology advances, the power density and integration of electronic devices are increasing, and this trend presents new challenges to the performance of materials. The conventional high polymer flexible base material has the performance disadvantages of weather resistance, aging resistance, corrosion resistance and the like, and becomes a key factor influencing the operation stability and the service life of an electronic device. In order to solve the problem, fluorocarbon film materials represented by polyvinylidene fluoride (PVDF) and polyvinyl fluoride (PVF) have good processability and cost performance while having higher thermal stability, chemical resistance and permeability resistance than common base materials, and have entered the visual field of people and obtained a certain degree of popularization and application. However, the fluorocarbon film material has low surface energy and a large contact angle, so that the binder phase of the general low-temperature silver paste cannot be sufficiently adhered to the substrate, a conductive circuit with good adhesion is difficult to form on the substrate, and the development requirement of a novel electronic device cannot be met.
Chinese patent CN 104538083 a uses a combination of a silane coupling agent and a titanate coupling agent as an adhesion promoter to prepare a high-adhesion low-temperature curing conductive silver paste, but the invention only considers the common situation that the base material is a PET film, and does not develop a fluorocarbon film material. At present, in order to solve the problem that the fluorocarbon film is difficult to adhere to, a common technical method is surface modification or plasma surface treatment, so that the process difficulty and the cost are greatly increased, and meanwhile, a chemical reagent used for surface modification easily causes the problems of human health and environmental protection.
Therefore, there is a need to develop a low-temperature silver paste with good matching property and high adhesion with fluorocarbon film material to meet the wide application of fluorocarbon film material.
Disclosure of Invention
The invention aims to provide a high-adhesion low-temperature silver paste for a fluorocarbon film and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme: the high-adhesion low-temperature silver paste for the fluorocarbon film comprises the following components in parts by weight:
high molecular resin: 4-15 parts;
organic solvent: 5-35 parts;
curing the crosslinking agent: 0.2-2 parts of a solvent;
rheological aid: 0.5-5 parts;
tackifier: 0.5-5 parts;
conductive powder: 45-80 parts of a solvent;
wherein the polymer resin is a combination of phenoxy resin and fluorocarbon resin;
the organic solvent is one or a combination of ester and ketone organic solvents, and the boiling point is 150-230 ℃;
the curing crosslinking agent is a latent curing agent, and the deblocking temperature is 80-120 ℃;
the rheological additive is a thixotropic agent;
the tackifier is a combination of fluorine-containing siloxane, a silane coupling agent and acetylacetone salt;
the conductive powder is a combination of large-particle-size flake silver powder, micron-sized flake silver powder and micron-sized spherical silver powder.
Further, the weight average molecular weight of the phenoxy resin is 30000-70000, the epoxy equivalent is 6000-9000 g/eq, and the glass transition temperature is 60-110 ℃; the fluorocarbon resin is selected from one of polyvinyl fluoride, polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, fluoroolefin-vinyl ether copolymer and tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride copolymer.
Further, in the polymer resin, the phenoxy resin accounts for 60-80% by weight, and the fluorocarbon resin accounts for 20-40% by weight.
Further, in the tackifier, by weight, the fluorine-containing siloxane accounts for 40-60%, the silane coupling agent accounts for 20-40%, and the acetylacetone salt accounts for 10-30%.
Further, the fluorine-containing siloxane is one of nonafluorohexyltrimethoxysilane, nonafluorohexyltriethoxysilane, dodecafluoroheptylpropyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, tridecafluorooctyltriethoxysilane, heptadecafluorodecyltrimethoxysilane and heptadecafluorodecyltriethoxysilane; the silane coupling agent is one of gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, gamma-aminopropyltriethoxysilane and gamma-mercaptopropyltriethoxysilane; the acetylacetone salt is one of titanium acetylacetonate, aluminum acetylacetonate, cobalt acetylacetonate, molybdenum acetylacetonate and zinc acetylacetonate.
Further, the organic solvent is one or more of glycol ether acetate, glycol butyl ether acetate, diethylene glycol ether acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, DBE, cyclohexanone, diisobutyl ketone and isophorone.
Further, the curing crosslinking agent is one or more of a combination of blocked isocyanate, modified amine, modified imidazole and microcapsule curing agent.
Further, the rheological additive is one or more of fumed silica, organic bentonite, carbon black, polyethylene wax and polyamide wax.
Further, the large-particle-diameter flake silver powder has a particle diameter of 5.0 to 12.0 μm and a tap density of 1.5 to 2.5g/cm 3 (ii) a The micron-sized flake silver powder has the particle diameter of 1.0-3.0 mu m and the tap density of 2.8-4.0 g/cm 3 (ii) a The micron-sized spherical silver powder has the particle diameter of 0.5-2.0 mu m and the tap density of 3.5-4.5 g/cm 3 。
The invention also provides a preparation method of the high-adhesion low-temperature silver paste for the fluorocarbon film material, which is used for preparing the high-adhesion low-temperature silver paste for the fluorocarbon film material and comprises the following steps:
s1, preparation of organic carrier: weighing the polymer resin and the organic solvent according to the weight ratio, mixing and stirring for 4-8 hours at the temperature of 60-100 ℃ until the polymer resin and the organic solvent are uniformly dissolved and dispersed, and cooling to room temperature for later use after dissolving;
s2, preparation of a tackifier: weighing fluorine-containing siloxane, a silane coupling agent and acetylacetone salt according to the weight ratio, and uniformly mixing in a high-speed dispersion machine, wherein the dispersion speed is 500-1000 rpm, and the time is 20-40 min;
s3, preparing a silver paste matrix: uniformly mixing a curing cross-linking agent, a rheological additive, the organic carrier prepared by S1 and the tackifier prepared by S2 in a dispersion machine according to the weight ratio, wherein the dispersion speed is 600-1200 rpm, and the dispersion time is 30-60 min;
s4, preparation of low-temperature silver paste: and adding conductive powder into the silver paste matrix prepared in the S3 according to the weight ratio, uniformly mixing in a dispersion machine, dispersing at the rotating speed of 1000-1600 rpm for 30-60 min, and grinding until the fineness is less than 10 mu m to obtain the high-adhesion low-temperature silver paste for the fluorocarbon film material.
The invention has the beneficial effects that:
(1) according to the invention, the combination of the phenoxy resin and the fluorocarbon resin is used as a binding phase of the low-temperature silver paste, the fluorocarbon resin has good adhesion to fluorocarbon film materials with similar structures, the benzene epoxy resin has higher polarity compared with common thermoplastic resins such as saturated polyester resin, polyurethane resin and acrylic resin, and has stronger interaction with a base material, and the combination of the phenoxy resin and the fluorocarbon resin can effectively improve the adhesive force of the low-temperature silver paste and the fluorocarbon film materials.
(2) The phenoxy resin has the characteristics of high hardness and high toughness after being cured and crosslinked, the fluorocarbon resin has the characteristic of high flexibility, and the combination of the phenoxy resin and the fluorocarbon resin is used as a binding phase, so that the low-temperature silver paste has the characteristics of flexibility and bending resistance, is matched with the flexibility of a fluorocarbon film material, and is more suitable for the application of novel flexible electronic devices.
(3) The tackifier prepared by using the fluorine-containing siloxane as the main component generates a synergistic effect of adhesion promotion by utilizing the compatibility of the fluorine-containing siloxane and the fluorocarbon film material and the bridging action of a silane coupling agent and acetylacetone salt, and effectively ensures the stable adhesion of the high molecular resin and the conductive powder to the fluorocarbon film material.
(4) The silver paste prepared by adopting the combination of silver powders with different particle sizes and morphologies as the conductive powder and using the rheological additive to adjust the thixotropy of the silver paste has low resistance and is suitable for screen printing.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a high-adhesion low-temperature silver paste for a fluorocarbon film, which comprises the following components in parts by weight:
high molecular resin: 4-15 parts;
organic solvent: 5-35 parts;
curing the crosslinking agent: 0.2-2 parts of a solvent;
rheological aid: 0.5-5 parts;
tackifier: 0.5-5 parts;
conductive powder: 45-80 parts.
In a preferred embodiment, the high-adhesion low-temperature silver paste for fluorocarbon film comprises the following components in parts by weight:
high molecular resin: 6-12 parts of a solvent;
organic solvent: 15-30 parts of a solvent;
curing the crosslinking agent: 0.3-1 part;
rheological aid: 1-3 parts;
tackifier: 1-3 parts;
conductive powder: 55-75 parts.
Wherein the polymer resin is a combination of phenoxy resin and fluorocarbon resin. In the polymer resin, the weight percentage of the phenoxy resin is 60-80%, and the weight percentage of the fluorocarbon resin is 20-40%. The specific ratio of the phenoxy resin to the fluorocarbon resin may be selected according to actual needs. The phenoxy resin ratio may be 65%, 60%, 75%, etc., and the fluorocarbon resin ratio may be 25%, 30%, 35%, etc.
The weight average molecular weight of the phenoxy resin is 30000-70000, the epoxy equivalent is 6000-9000 g/eq, and the glass transition temperature is 60-110 ℃. The fluorocarbon resin is selected from one of polyvinyl fluoride, polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, fluoroolefin-vinyl ether copolymer and tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride copolymer.
The combination of phenoxy resin and fluorocarbon resin is used as the binder phase of low-temperature silver paste, the fluorocarbon resin has good adhesion to fluorocarbon film materials with similar structures, the phenoxy resin has higher polarity relative to common thermoplastic resins such as saturated polyester resin, polyurethane resin and acrylic resin, and has stronger interaction with a substrate, and the combination of the phenoxy resin and the fluorocarbon resin can effectively improve the adhesive force of the low-temperature silver paste and the fluorocarbon film materials.
The phenoxy resin has the characteristics of high hardness and high toughness after being cured and crosslinked, the fluorocarbon resin has the characteristic of high flexibility, and the combination of the phenoxy resin and the fluorocarbon resin is used as a binding phase, so that the low-temperature silver paste has the characteristics of flexibility and bending resistance, is matched with the flexibility of a fluorocarbon film material, and is more suitable for application of novel flexible electronic devices.
The organic solvent is one or more of ester and ketone, and has a boiling point of 150 deg.C
230 ℃ to. The organic solvent is one or more of glycol ether acetate, ethylene glycol butyl ether acetate, diethylene glycol ether acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, DBE, cyclohexanone, diisobutyl ketone and isophorone. The organic solvent may also be other esters or ketones, which are not listed here.
The curing crosslinking agent is a latent curing agent, and the deblocking temperature is 80-120 ℃. Specifically, the curing crosslinking agent is one or a combination of more of blocked isocyanate, modified amine, modified imidazole and a microcapsule curing agent. The curing crosslinking agent can also be other latent curing agents, which are not listed here.
The rheological additive is a thixotropic agent, wherein the rheological additive is one or a combination of more of fumed silica, organic bentonite, carbon black, polyethylene wax and polyamide wax.
The adhesion promoter is a combination of fluorine-containing siloxane, a silane coupling agent and acetylacetone salt. In the tackifier, by weight, 40-60% of fluorine-containing siloxane, 20-40% of silane coupling agent and 10-30% of acetylacetone salt are contained. The tackifier prepared by using the fluorine-containing siloxane as the main component generates a synergistic effect of adhesion promotion by utilizing the compatibility of the fluorine-containing siloxane and the fluorocarbon film material and the bridging action of a silane coupling agent and acetylacetone salt, and effectively ensures the stable adhesion of the high molecular resin and the conductive powder to the fluorocarbon film material.
The fluorine-containing siloxane is one of nonafluorohexyltrimethoxysilane, nonafluorohexyltriethoxysilane, dodecafluoroheptylpropyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, tridecafluorooctyltriethoxysilane, heptadecafluorodecyltrimethoxysilane and heptadecafluorodecyltriethoxysilane.
The silane coupling agent is one of gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, gamma-aminopropyltriethoxysilane and gamma-mercaptopropyltriethoxysilane.
The acetylacetone salt is one of titanium acetylacetonate, aluminum acetylacetonate, cobalt acetylacetonate, molybdenum acetylacetonate and zinc acetylacetonate.
The conductive powder is large-particle-size flake silver powder and micron-scale flakeCombination of silver powder and micron-sized spherical silver powder. The flake silver powder with large particle size has a particle size of 5.0 to 12.0 μm and a tap density of 1.5 to 2.5g/cm 3 (ii) a The micron-sized flake silver powder has a particle size of 1.0-3.0 μm and a tap density of 2.8-4.0 g/cm 3 (ii) a The micron-sized spherical silver powder has a particle size of 0.5-2.0 μm and a tap density of 3.5-4.5 g/cm 3 . The silver powder with different particle sizes and shapes is used as conductive powder, the thixotropy of the silver paste is adjusted by using a rheological additive, and the prepared low-temperature silver paste is low in resistance and suitable for screen printing.
The invention also provides a preparation method of the high-adhesion low-temperature silver paste for the fluorocarbon film material, which is used for preparing the high-adhesion low-temperature silver paste for the fluorocarbon film material and comprises the following steps:
s1, preparation of organic carrier: weighing the polymer resin and the organic solvent according to the weight ratio, mixing and stirring for 4-8 hours at the temperature of 60-100 ℃ until the polymer resin and the organic solvent are uniformly dissolved and dispersed, and cooling to room temperature for later use after dissolving;
s2, preparation of a tackifier: weighing fluorine-containing siloxane, a silane coupling agent and acetylacetone salt according to the weight ratio, and uniformly mixing in a high-speed dispersion machine, wherein the dispersion speed is 500-1000 rpm, and the time is 20-40 min;
s3, preparing a silver paste matrix: uniformly mixing the curing cross-linking agent, the rheological additive, the organic carrier prepared from S1 and the tackifier prepared from S2 in a dispersion machine according to the weight ratio, wherein the dispersion speed is 600-1200 rpm, and the dispersion time is 30-60 min;
s4, preparation of low-temperature silver paste: adding the conductive powder into the silver paste matrix prepared in S3 according to the weight ratio, uniformly mixing in a dispersion machine, dispersing at the rotating speed of 1000-1600 rpm for 30-60 min, grinding until the fineness is less than 10 mu m, and obtaining the high-adhesion low-temperature silver paste for the fluorocarbon film material.
Among them, the dispersers in S3 and S4 may be planetary vacuum dispersers to improve the efficiency of mixing the reactants. In S4, the grinding may be performed using a three-roll grinder, which is an example and not particularly limited herein.
The following describes the high-adhesion low-temperature silver paste for fluorocarbon film in detail with reference to specific examples.
Example 1
A high-adhesion low-temperature silver paste for a fluorocarbon film is prepared by the following steps:
(1) preparation of organic vehicle:
weighing 55g of phenoxy resin, 25g of polyvinylidene fluoride resin, 125g of ethylene glycol monobutyl ether acetate and 50g of isophorone, mixing and stirring at 80 ℃ for 5h until the mixture is uniformly dissolved and dispersed, and cooling to room temperature for later use after dissolution to prepare the organic carrier.
(2) Preparing a tackifier:
weighing 11g of tridecafluorooctyltriethoxysilane, 5g of gamma-glycidoxypropyltrimethoxysilane and 4g of aluminum acetylacetonate, and uniformly mixing in a high-speed dispersion machine at the dispersion rotating speed of 800rpm for 30min to prepare the tackifier.
(3) Preparing a silver paste matrix:
and (3) uniformly mixing 7g of blocked isocyanate and 18g of fumed silica with the organic carrier prepared in the step (1) and the tackifier prepared in the step (2) in a planetary vacuum dispersion machine, and preparing the silver paste matrix by dispersing at the rotating speed of 1000rpm for 40 min.
(4) Preparing low-temperature silver paste:
200g of a large-particle-diameter plate-like silver powder (particle diameter of 5.0 to 8.0 μm, tap density of 2.2 g/cm) 3 ) 350g of micron-sized flake silver powder (the particle diameter is 1.5-2.0 mu m, and the tap density is 3.5 g/cm) 3 ) And 150g of micron-sized spherical silver powder (the particle diameter is 1.0-1.5 mu m, and the tap density is 4.1 g/cm) 3 ) And (4) adding the mixture into the silver paste matrix prepared in the step (3), uniformly mixing in a planetary vacuum dispersion machine, dispersing at the rotating speed of 1500rpm for 45min, and grinding in a three-roll grinder until the fineness is less than 10 mu m to form the high-adhesion low-temperature silver paste for the fluorocarbon film material.
Example 2
A high-adhesion low-temperature silver paste for a fluorocarbon film is prepared by the following steps:
(1) preparation of organic vehicle:
weighing 55g of phenoxy resin, 25g of vinylidene fluoride-hexafluoropropylene copolymer resin, 75g of ethylene glycol ethyl ether acetate and 150g of DBE, mixing and stirring at 80 ℃ for 5h until the mixture is uniformly dissolved and dispersed, and cooling to room temperature for later use after dissolution to prepare the organic carrier.
(2) Preparing a tackifier:
weighing 10g of nonafluorohexyltrimethoxysilane, 6.5g of vinyltriethoxysilane and 3.5g of zinc acetylacetonate, and uniformly mixing in a high-speed dispersion machine at the dispersion rotation speed of 800rpm for 30min to obtain the tackifier.
(3) Preparing a silver paste matrix:
and (3) uniformly mixing 7g of blocked isocyanate and 18g of fumed silica with the organic carrier prepared in the step (1) and the tackifier prepared in the step (2) in a planetary vacuum dispersion machine, and preparing the silver paste matrix by dispersing at the rotating speed of 1000rpm for 40 min.
(4) Preparing low-temperature silver paste:
300g of a large-particle-diameter plate-like silver powder (particle diameter of 5.0 to 8.0 μm, tap density of 2.2 g/cm) 3 ) 200g of micron-sized flake silver powder (particle diameter of 1.5-2.0 μm, tap density of 3.5 g/cm) 3 ) And 150g of micron-sized spherical silver powder (the particle diameter is 1.0-1.5 mu m, and the tap density is 4.1 g/cm) 3 ) And (4) adding the mixture into the silver paste matrix prepared in the step (3), uniformly mixing in a planetary vacuum dispersion machine, dispersing at the rotating speed of 1500rpm for 45min, and grinding in a three-roll grinder until the fineness is less than 10 mu m to form the high-adhesion low-temperature silver paste for the fluorocarbon film material.
Example 3
A high-adhesion low-temperature silver paste for a fluorocarbon film is prepared by the following steps:
(1) preparation of organic vehicle:
weighing 60g of phenoxy resin, 30g of fluoroolefin-vinyl ether copolymer resin, 190g of diethylene glycol ethyl ether acetate and 75g of cyclohexanone, mixing and stirring at 90 ℃ for 6h until the mixture is uniformly dissolved and dispersed, and cooling to room temperature for later use after dissolution to obtain the organic carrier.
(2) Preparing a tackifier:
14g of heptadecafluorodecyltrimethoxysilane, 8g of gamma- (methacryloyloxy) propyltrimethoxysilane and 3g of titanium acetylacetonate are weighed and uniformly mixed in a high-speed dispersion machine, and the dispersion speed is 800rpm and the dispersion time is 30min, so that the tackifier is prepared.
(3) Preparing a silver paste matrix:
and (3) uniformly mixing 5g of modified imidazole curing agent, 5g of carbon black and 10g of polyamide wax with the organic carrier prepared in the step (1) and the tackifier prepared in the step (2) in a planetary vacuum dispersion machine, and dispersing at the rotating speed of 1000rpm for 40min to obtain the silver paste matrix.
(4) Preparing low-temperature silver paste:
400g of a large-particle-diameter plate-like silver powder (particle diameter 8.0 to 10.0 μm, tap density 1.8 g/cm) 3 ) 120g of micron-sized flake silver powder (particle size of 2.0-3.0 μm, tap density of 3.2 g/cm) 3 ) And 80g of micron-sized spherical silver powder (the particle diameter is 1.0-1.5 mu m, and the tap density is 4.1 g/cm) 3 ) And (4) adding the mixture into the silver paste matrix prepared in the step (3), uniformly mixing in a planetary vacuum dispersion machine, dispersing at the rotating speed of 1200rpm for 40min, and grinding in a three-roll grinder until the fineness is less than 10 mu m to form the high-adhesion low-temperature silver paste for the fluorocarbon film material.
Example 4
A high-adhesion low-temperature silver paste for a fluorocarbon film is prepared by the following steps:
(1) preparation of organic vehicle:
weighing 70g of phenoxy resin, 30g of tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride copolymer resin, 150g of dimethyl glutarate and 100g of diisobutyl ketone, mixing and stirring at 90 ℃ for 6h until the materials are uniformly dissolved and dispersed, and cooling to room temperature for later use after dissolution to prepare the organic carrier.
(2) Preparing a tackifier:
weighing 13g of dodecafluoroheptyl propyl trimethoxy silane, 7g of gamma-aminopropyl triethoxy silane and 5g of titanium acetylacetonate, and uniformly mixing in a high-speed dispersion machine at the dispersion rotating speed of 800rpm for 30min to prepare the tackifier.
(3) Preparing a silver paste matrix:
and (3) uniformly mixing 8g of modified amine curing agent, 8g of fumed silica and 9g of polyamide wax, the organic carrier prepared in the step (1) and the tackifier prepared in the step (2) in a planetary vacuum dispersion machine, and dispersing at the rotating speed of 1000rpm for 40min to obtain the silver paste matrix.
(4) Preparing low-temperature silver paste:
420g of a large-particle-diameter plate-like silver powder (particle diameter 8.0 to 10.0 μm, tap density 1.8 g/cm) 3 ) 90g of micron-sized flake silver powder (particle size of 2.0-3.0 μm, tap density of 3.2 g/cm) 3 ) And 90g of micron-sized spherical silver powder (the particle diameter is 1.5-2.0 mu m, and the tap density is 3.8 g/cm) 3 ) And (4) adding the mixture into the silver paste matrix prepared in the step (3), uniformly mixing in a planetary vacuum dispersion machine, dispersing at the rotating speed of 1200rpm for 40min, and grinding in a three-roll grinder until the fineness is less than 10 mu m to form the high-adhesion low-temperature silver paste for the fluorocarbon film material.
Test method
The high-adhesion low-temperature silver paste for fluorocarbon film materials prepared in the above examples 1 to 4 were sampled, respectively, and the samples were printed on a PVDF film using a 250-mesh screen with a photosensitive resist thickness of 15 μm, and then baked and cured at 120 ℃ for 30 min.
After the silver paste is cured, a film thickness meter is used for testing the thickness of a film layer, a four-probe tester is used for testing the square resistance, the hardness is tested according to GB/T6739-jar 2006 paint and varnish pencil method for determining the hardness of the paint film, and the adhesion is tested according to GB/T9286-jar 2021-paint and varnish lattice test. The constant temperature and humidity test is carried out at the temperature of 85 ℃ and the relative humidity of 85 percent for 360 hours, and the adhesive force is tested according to GB/T9286-doped 2021 paint and varnish test. Bending diameter of the bending resistance test is 5mm, forward and backward bending is performed for 100 times by using a bending tester, and the change of the silver paste film layer after the test is observed and the resistance change rate is calculated. The test results are shown in table 1:
TABLE 1
The test results show that the high-adhesion low-temperature silver paste for the fluorocarbon film material has good conductivity, high hardness and excellent and stable adhesion to the fluorocarbon film material. Meanwhile, the resistance change rate of the silver paste after repeated bending is less than 5%, which shows that the silver paste has good matching property with fluorocarbon film materials, and has wide application prospect in the field of novel flexible electronic devices.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, but should be considered as the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The high-adhesion low-temperature silver paste for the fluorocarbon film material is characterized by comprising the following components in parts by weight:
high molecular resin: 4-15 parts;
organic solvent: 5-35 parts;
curing the crosslinking agent: 0.2-2 parts of a solvent;
rheological aid: 0.5-5 parts;
tackifier: 0.5-5 parts;
conductive powder: 45-80 parts of a solvent;
wherein the polymer resin is a combination of phenoxy resin and fluorocarbon resin;
the organic solvent is one or a combination of ester and ketone organic solvents, and the boiling point is 150-230 ℃;
the curing crosslinking agent is a latent curing agent, and the deblocking temperature is 80-120 ℃;
the rheological additive is a thixotropic agent;
the tackifier is a combination of fluorine-containing siloxane, a silane coupling agent and acetylacetone salt;
the conductive powder is a combination of large-particle-size flake silver powder, micron-sized flake silver powder and micron-sized spherical silver powder.
2. The high-adhesion low-temperature silver paste for fluorocarbon film materials as claimed in claim 1, wherein the weight average molecular weight of the phenoxy resin is 30000-70000, the epoxy equivalent is 6000-9000 g/eq, and the glass transition temperature is 60-110 ℃; the fluorocarbon resin is selected from one of polyvinyl fluoride, polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, fluoroolefin-vinyl ether copolymer and tetrafluoroethylene-hexafluoropropylene-vinylidene fluoride copolymer.
3. The high-adhesion low-temperature silver paste for fluorocarbon film material of claim 1, wherein the phenoxy resin accounts for 60-80% of the polymer resin, and the fluorocarbon resin accounts for 20-40% of the polymer resin.
4. The high-adhesion low-temperature silver paste for fluorocarbon film materials as claimed in claim 1, wherein in the tackifier, by weight, the fluorine-containing siloxane accounts for 40-60%, the silane coupling agent accounts for 20-40%, and the acetylacetone salt accounts for 10-30%.
5. The high-adhesion low-temperature silver paste for fluorocarbon film according to claim 1, wherein the fluorine-containing siloxane is one of nonafluorohexyltrimethoxysilane, nonafluorohexyltriethoxysilane, dodecafluoroheptylpropyltrimethoxysilane, tridecafluorooctyltrimethoxysilane, tridecafluorooctyltriethoxysilane, heptadecafluorodecyltrimethoxysilane and heptadecafluorodecyltriethoxysilane; the silane coupling agent is one of gamma-glycidoxypropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, gamma-aminopropyltriethoxysilane and gamma-mercaptopropyltriethoxysilane; the acetylacetone salt is one of titanium acetylacetonate, aluminum acetylacetonate, cobalt acetylacetonate, molybdenum acetylacetonate and zinc acetylacetonate.
6. The high-adhesion low-temperature silver paste for fluorocarbon film according to claim 1, wherein the organic solvent is one or more of glycol ethyl ether acetate, glycol butyl ether acetate, diethylene glycol ethyl ether acetate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, DBE, cyclohexanone, diisobutyl ketone and isophorone.
7. The high-adhesion low-temperature silver paste for fluorocarbon film according to claim 1, wherein the curing cross-linking agent is one or more of a combination of blocked isocyanate, modified amine, modified imidazole and microcapsule curing agent.
8. The high-adhesion low-temperature silver paste for fluorocarbon film of claim 1, wherein the rheological aid is one or more of fumed silica, organobentonite, carbon black, polyethylene wax and polyamide wax.
9. The high-adhesion low-temperature silver paste for fluorocarbon film of claim 1, wherein the large-particle-size flake silver powder has a particle size of 5.0-12.0 μm and a tap density of 1.5-2.5 g/cm 3 (ii) a The micron-sized flake silver powder has the particle diameter of 1.0-3.0 mu m and the tap density of 2.8-4.0 g/cm 3 (ii) a The micron-sized spherical silver powder has the particle diameter of 0.5-2.0 mu m and the tap density of 3.5-4.5 g/cm 3 。
10. The preparation method of the high-adhesion low-temperature silver paste for the fluorocarbon film is used for preparing the high-adhesion low-temperature silver paste for the fluorocarbon film as claimed in any one of claims 1 to 9, and comprises the following steps:
s1, preparation of organic carrier: weighing the polymer resin and the organic solvent according to the weight ratio, mixing and stirring for 4-8 hours at the temperature of 60-100 ℃ until the polymer resin and the organic solvent are uniformly dissolved and dispersed, and cooling to room temperature for later use after dissolving;
s2, preparation of a tackifier: weighing fluorine-containing siloxane, a silane coupling agent and acetylacetone salt according to the weight ratio, and uniformly mixing in a high-speed dispersion machine, wherein the dispersion speed is 500-1000 rpm, and the time is 20-40 min;
s3, preparing a silver paste matrix: uniformly mixing a curing cross-linking agent and a rheological additive, the organic carrier prepared from S1 and the tackifier prepared from S2 in a dispersion machine according to the weight ratio, wherein the dispersion speed is 600-1200 rpm, and the time is 30-60 min;
s4, preparation of low-temperature silver paste: and adding conductive powder into the silver paste matrix prepared in the S3 according to the weight ratio, uniformly mixing in a dispersion machine, dispersing at the rotating speed of 1000-1600 rpm for 30-60 min, and grinding until the fineness is less than 10 mu m to obtain the high-adhesion low-temperature silver paste for the fluorocarbon film material.
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