CN111675490A - Lead-free and cadmium-free glass powder and preparation method thereof, and conductive silver paste and preparation method thereof - Google Patents
Lead-free and cadmium-free glass powder and preparation method thereof, and conductive silver paste and preparation method thereof Download PDFInfo
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- CN111675490A CN111675490A CN202010570595.XA CN202010570595A CN111675490A CN 111675490 A CN111675490 A CN 111675490A CN 202010570595 A CN202010570595 A CN 202010570595A CN 111675490 A CN111675490 A CN 111675490A
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- free
- oxide
- lead
- cadmium
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- 239000011521 glass Substances 0.000 title claims abstract description 87
- 239000000843 powder Substances 0.000 title claims abstract description 43
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000007797 corrosion Effects 0.000 claims abstract description 14
- 238000005260 corrosion Methods 0.000 claims abstract description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 6
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002667 nucleating agent Substances 0.000 claims abstract description 6
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 6
- 239000011787 zinc oxide Substances 0.000 claims abstract description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 5
- 239000011737 fluorine Substances 0.000 claims abstract description 5
- 239000008395 clarifying agent Substances 0.000 claims abstract description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims abstract description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910001947 lithium oxide Inorganic materials 0.000 claims abstract description 3
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000000049 pigment Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000013008 thixotropic agent Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 4
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 4
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000004902 Softening Agent Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 2
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 claims description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 239000001856 Ethyl cellulose Substances 0.000 claims description 2
- 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 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920001249 ethyl cellulose Polymers 0.000 claims description 2
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 2
- -1 polypropylene Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 2
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 2
- 229940116411 terpineol Drugs 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
- 239000003623 enhancer Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 12
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- YADSGOSSYOOKMP-UHFFFAOYSA-N dioxolead Chemical compound O=[Pb]=O YADSGOSSYOOKMP-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000011775 sodium fluoride Substances 0.000 description 4
- 235000013024 sodium fluoride Nutrition 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010257 thawing Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- QNVRIHYSUZMSGM-UHFFFAOYSA-N hexan-2-ol Chemical class CCCCC(C)O QNVRIHYSUZMSGM-UHFFFAOYSA-N 0.000 description 2
- 239000006060 molten glass Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- BSWXAWQTMPECAK-UHFFFAOYSA-N 6,6-diethyloctyl dihydrogen phosphate Chemical class CCC(CC)(CC)CCCCCOP(O)(O)=O BSWXAWQTMPECAK-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical class [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 239000001913 cellulose Chemical class 0.000 description 1
- 229920002678 cellulose Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001522 polyglycol ester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/004—Refining agents
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/11—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen
- C03C3/112—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine
- C03C3/115—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron
- C03C3/118—Glass compositions containing silica with 40% to 90% silica, by weight containing halogen or nitrogen containing fluorine containing boron containing aluminium
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/90—Electrical properties
- C04B2111/94—Electrically conducting materials
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Ceramic Engineering (AREA)
- Dispersion Chemistry (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Glass Compositions (AREA)
Abstract
The application relates to lead-free and cadmium-free glass powder and a preparation method thereof, and conductive silver paste and a preparation method thereof, belonging to the technical field of conductive paste, and the lead-free and cadmium-free glass powder comprises the following components in parts by weight: 15-45 parts of silicon dioxide; 5-30 parts of zinc oxide; 10-35 parts of bismuth oxide; 2-15 parts of titanium dioxide; 3-20 parts of diboron trioxide; 0.1-5 parts of aluminum oxide; 0.1-5 parts of lithium oxide; 0.015-5 parts of fluorine gas; 0.1-40 parts of a softener; 0-20 parts of nucleating agent; 0-7 parts of corrosion-resistant reinforcing agent; 0-10 parts of glass clarifying agent; 0-15 parts of filler. The coating has the advantage of good corrosion resistance.
Description
Technical Field
The application belongs to the technical field of conductive paste, and particularly relates to lead-free cadmium glass powder and a preparation method thereof, and conductive silver paste and a preparation method thereof.
Background
The conductive silver paste is a viscous paste of a mechanical mixture consisting of high-purity metal silver particles, an adhesive, a solvent and an auxiliary agent, and can be used in multiple fields of solar cells and automobile windshields.
The principle that the conductive silver paste is used for defrosting and demisting of the automobile windshield is as follows: conductive silver paste is printed on automobile glass and is coated on the surface of the glass through sintering after toughening treatment, so that the surface of the glass has certain resistance, and heat is emitted during power-on to remove frost and mist on the surface of the glass, thereby achieving the effects of defrosting and demisting.
The existing conductive silver paste comprises polymer silver conductive paste (dried or solidified into a film, and an organic polymer is used as a bonding phase); and secondly, sintering type silver conductive paste (sintering film forming, sintering temperature is higher than 500 ℃, and glass powder or oxide is used as a bonding phase) is adopted, the common glass powder in the sintering type silver conductive paste takes lead dioxide as a main raw material, although the lead dioxide component can effectively perform oxidation-reduction reaction with silicon to be converted into simple substance lead, the melting assisting effect is achieved, but the lead-containing glass is gradually replaced by lead-free glass powder due to the toxicity of the lead-containing glass. For example, chinese patent publication No. 201010118869.8 discloses a lead-free glass powder for solar cell aluminum paste, in which the content of bismuth oxide is as high as 30-60%.
The above prior art solutions have the following drawbacks: in the prior art, the conductive silver paste has poor corrosion resistance, is easy to age after being used for a long time, and influences the efficiency and the service life of the windshield.
Disclosure of Invention
Aiming at the defects in the prior art, one of the purposes of the application is to provide the lead-free and cadmium-free glass powder with good corrosion resistance;
another objective of the present application is to provide a method for preparing lead-free and cadmium-free glass powder, which is used for preparing the lead-free and cadmium-free glass powder;
the third purpose of the application is to provide a conductive silver paste which can be stably attached to the surface of a windshield and prolong the service life of the windshield;
the fourth objective of the present application is to provide a method for preparing conductive silver paste, which is used for preparing the conductive silver paste.
The above object of the present application is achieved by the following technical solutions:
the lead-free and cadmium-free glass powder comprises the following raw materials in parts by weight: 15-45 parts of silicon dioxide; 5-30 parts of zinc oxide; 10-35 parts of bismuth oxide; 2-15 parts of titanium dioxide; 3-20 parts of diboron trioxide; 0.1-5 parts of aluminum oxide; 0.1-5 parts of lithium oxide; 0.015-5 parts of fluorine gas; 0.1-40 parts of a softener; 0-20 parts of nucleating agent; 0-7 parts of corrosion-resistant reinforcing agent; 0-10 parts of glass clarifying agent; 0-15 parts of filler.
By adopting the technical scheme, the silicon dioxide is a component for forming the glass and is a key factor for forming stable glass, and when the content is 15-45 parts, the softening point and the viscosity are increased along with the increase of the content of the silicon dioxide; boron oxide is a component forming glass like silica, and boron trioxide makes glass easily meltable and suppresses an excessive increase in expansion coefficient, and has appropriate fluidity at the time of firing; the addition of the aluminum oxide can replace a part of silicon dioxide, improve the chemical stability and acid resistance of the glass and reduce the crystallization degree; the zinc oxide and the bismuth oxide have the effect of reducing the softening point, so that the glass can have proper fluidity when melted, the glass is adjusted to have proper thermal expansion coefficient, the addition of the zinc oxide is controlled to be 10-40 parts, and the influence of excessive zinc oxide and bismuth oxide on the quality of the glass powder can be avoided; the introduction of fluorine gas can generate sodium fluoride, and the sodium fluoride can reduce the softening point of glass and improve the corrosion resistance of glass powder.
The present application may be further configured in a preferred example to: the softening agent is a mixture of three or more of barium oxide, sodium oxide, potassium oxide and copper oxide.
By adopting the technical scheme, the softening temperature of the glass can be reduced by adding the softening agent, and the operation of the glass powder is facilitated.
The present application may be further configured in a preferred example to: the nucleating agent is a mixture of three or more of calcium oxide, magnesium oxide, strontium oxide, manganese dioxide and nickel oxide.
By adopting the technical scheme, the crystallization speed of the glass powder can be increased by adding the nucleating agent, the welding performance of the surface of the conductive silver paste is improved, and the wear resistance of the surface of the silver paste is submitted.
The present application may be further configured in a preferred example to: the corrosion-resistant reinforcing agent is one or two of ferric oxide and zirconium dioxide.
By adopting the technical scheme, the corrosion resistance of the glass powder can be improved by adding the corrosion-resistant reinforcing agent, so that the service life of the glass powder is prolonged.
The present application may be further configured in a preferred example to: the glass refining agent is a mixture of phosphorus pentoxide and antimony pentoxide.
By adopting the technical scheme, the glass clarifying agent can reduce the viscosity of the molten glass in the glass melting process, and promote the raw materials for eliminating bubbles in the molten glass.
The present application may be further configured in a preferred example to: the raw material also comprises 0-5 parts of vanadium pentoxide.
By adopting the technical scheme, the vanadium pentoxide can be widely used as a regulator of glass performance, and the softening temperature and the sealing temperature of the glass can be obviously reduced by adding the vanadium pentoxide.
The present application may be further configured in a preferred example to: the raw material also comprises 2-3 parts of sulfur trioxide.
The second application object of the present application is achieved by the following technical scheme:
a preparation method of lead-free and cadmium-free glass powder comprises the following steps:
s1, weighing and uniformly mixing the raw materials in corresponding parts by weight, and carrying out heat preservation at the temperature of 1000-1300 ℃ for 2-3h to obtain glass liquid;
s2, pouring the glass liquid into water for water quenching, then adding alcohol, ball-milling to 1-3 mu m, and drying to obtain the lead-free and cadmium-free glass powder.
Through adopting above-mentioned technical scheme, before carrying out the ball-milling with glass powder, make the glass liquid after the cooling soften through alcohol, be convenient for carry out the ball-milling to the glass liquid after the cooling to shorten ball-milling time, improved ball-milling efficiency.
The third objective of the present application is achieved by the following technical solutions:
the conductive silver paste is characterized by comprising the following components in parts by weight: 2-5 parts of lead-free and cadmium-free glass powder; 9-34 parts of resin; 0.1-1 part of metal and oxide pigment thereof; 60-85 parts of silver powder; 0.2-0.3 part of dispersant; 0.2-0.3 part of leveling agent; 0.1-0.3 part of thixotropic agent; 10-20 parts of a solvent.
By adopting the technical scheme, the coating formed on the surface of the glass by the conductive silver paste has good acid resistance and is not easy to fall off; the conductivity is good, and the sheet resistance is 2.5-3.0 omega/□; most of the metal and oxide pigments are suitable for the formula and can be adjusted according to actual requirements.
The present application may be further configured in a preferred example to: the resin is one or more of ethyl cellulose, polyvinyl butyral, polypropylene resin and water white rosin resin.
The present application may be further configured in a preferred example to: the metal and the oxide pigment thereof are at least one selected from copper powder, zinc powder, titanium powder, bismuth powder or oxides thereof.
The present application may be further configured in a preferred example to: the solvent is selected from any one of terpineol, diethylene glycol butyl ether and ethylene glycol butyl ether acetate.
The present application may be further configured in a preferred example to: the dispersing agent is one or more of triethyl hexyl phosphoric acid, sodium dodecyl sulfate, methyl amyl alcohol, cellulose derivatives, polyacrylamide, Guel gum and fatty acid polyglycol ester.
By adopting the technical scheme, the silver powder can be uniformly dispersed in the solvent by adding the dispersing agent, and the production efficiency of the conductive silver paste is improved.
The present application may be further configured in a preferred example to: the leveling agent is polyether polyester modified organic siloxane.
By adopting the technical scheme, the addition of the leveling agent can promote the coating to form a flat, smooth and uniform coating film in the drying film-forming process, effectively reduce the surface tension of the coating liquid and improve the leveling property and uniformity of the coating liquid.
The present application may be further configured in a preferred example to: the thixotropic agent is one or more of fumed silica, organic bentonite, castor oil and polyamide.
By adopting the technical scheme, the thixotropic agent is added into the resin, so that the resin glue solution has higher consistency when being static and can be changed into a low-consistency fluid substance under the action of external force.
The fourth application purpose of the present application is achieved by the following technical solutions:
the preparation method of the conductive silver paste comprises the following steps:
mixing and stirring the lead-free and cadmium-free glass powder, the silver powder, the resin, the metal and metal oxide pigment, the dispersing agent, the flatting agent, the thixotropic agent and the solvent uniformly in corresponding parts by weight, and grinding the mixture by using a three-roll machine until the particle size is less than or equal to 10 microns.
By adopting the technical scheme, the conductive silver paste has the particle size of less than or equal to 10 microns, and the conductive performance of the conductive silver paste can be ensured, so that the performance of the conductive silver paste is ensured, heat is emitted when the conductive silver paste is electrified to remove frost on the surface of glass, and the defrosting and demisting effects are achieved.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the introduction of fluorine gas can generate sodium fluoride, and the sodium fluoride can reduce the softening point of glass and improve the corrosion resistance of glass powder;
2. the corrosion resistance of the glass powder can be improved by adding the corrosion resistance reinforcing agent, so that the service life of the glass powder is prolonged;
3. before the glass powder is subjected to ball milling, the cooled glass liquid is softened by alcohol, so that the cooled glass liquid is subjected to ball milling conveniently, the ball milling time is shortened, and the ball milling efficiency is improved.
Detailed Description
The following examples describe the invention in detail.
Preparation examples 1 to 8
The production methods in production examples 1 to 8 were the same except that the amounts of the raw materials were different (see Table 1). The following description will be made by taking preparation example 1 as an example.
The lead-free and cadmium-free glass powder disclosed by the embodiment 1 of the invention is prepared by the following steps:
s1, weighing and uniformly mixing the raw materials in parts by weight, and keeping the temperature at 1000 ℃ for 3 hours to obtain glass liquid;
s2, pouring the glass liquid into water for water quenching, then adding alcohol, ball-milling to 1 mu m, and drying to obtain the lead-free and cadmium-free glass powder.
TABLE 1 composition and amount of lead-free and cadmium-free glass powder
Preparation example 9 differs from preparation example 1 in that:
uniformly mixing the raw materials, keeping the temperature at 1150 ℃ for 2.5h to obtain glass liquid, pouring the glass liquid into water for water quenching, adding alcohol, ball-milling to 2 mu m, and drying to obtain the lead-cadmium-free glass powder
Preparation example 10 differs from preparation example 1 in that:
the raw materials are uniformly mixed, the temperature is kept for 2h at 1200 ℃ to obtain glass liquid, then the glass liquid is poured into water for water quenching, then alcohol is added, the ball milling is carried out until the ball milling reaches 3 mu m, and the lead-cadmium-free glass powder is obtained after the drying.
Preparation example 11 differs from preparation example 1 in that:
the raw material also comprises 1 part of vanadium pentoxide.
Preparation example 12 differs from preparation example 1 in that:
the raw material also comprises 3 parts of vanadium pentoxide.
Preparation example 13 differs from preparation example 1 in that:
the raw material also comprises 5 parts of vanadium pentoxide.
Examples 1-3, a conductive silver paste, were prepared according to the same method as in examples 1-3, except that the starting materials and amounts used were different (see table 2). The following description will be made by taking example 1 as an example
Adding silver powder, resin, metal and oxide pigment thereof, dispersing agent, leveling agent, thixotropic agent, solvent and the lead-free and cadmium-free glass powder in the preparation example 1 into a reaction kettle in corresponding parts by weight, mixing and stirring uniformly, and then grinding the mixture by using a three-roll machine until the particle size is less than or equal to 10 microns.
TABLE 2 conductive silver paste compositions
Examples 4 to 15, a conductive silver paste, differ from example 1 in that:
the lead-free and cadmium-free glass frit of preparation example 1 was replaced with the lead-free and cadmium-free glass frit of preparation examples 2 to 13.
Comparative example 1: a lead-free glass powder for solar cell aluminum paste is prepared by adopting the lead-free glass powder for solar cell aluminum paste in the background art in the example 1.
Performance testing
The adhesion of examples 1-15 and comparative example 1 was tested, and the adhesion of examples 1-15 was above grade 1, while the adhesion of comparative examples 1-3 was only grade 2, indicating that the conductive paste of the present application has stronger adhesion.
Acid resistance test
The conductive wires are formed on the surfaces of the automobile glass in the examples 1-15 and the comparative example 1, the examples 1-15 are soaked in 0.05mol/L sulfuric acid at 80 ℃, the examples 1-3 begin to fall off after 24H, the example 4 begins to fall off after 48H, the examples 5-15 begin to fall off after 2H, and the comparative example 1 falls off after 1H, so that compared with the prior art, the conductive wires are good in acid resistance and not easy to fall off.
The embodiments of the present invention are preferred embodiments of the present application, and the scope of protection of the present application is not limited by the embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. The lead-free and cadmium-free glass powder is characterized by comprising the following raw materials in parts by weight:
15-45 parts of silicon dioxide;
5-30 parts of zinc oxide;
10-35 parts of bismuth oxide;
2-15 parts of titanium dioxide;
3-20 parts of diboron trioxide;
0.1-5 parts of aluminum oxide;
0.1-5 parts of lithium oxide;
0.015-5 parts of fluorine gas;
0.1-40 parts of a softener;
0-20 parts of nucleating agent;
0-7 parts of corrosion-resistant reinforcing agent;
0-10 parts of glass clarifying agent;
0-15 parts of filler.
2. The lead-free and cadmium-free glass frit as claimed in claim 1, wherein the softening agent is a mixture of three or more of barium oxide, sodium oxide, potassium oxide and copper oxide.
3. The lead-free and cadmium-free glass frit as claimed in claim 1, wherein the nucleating agent is a mixture of three or more of calcium oxide, magnesium oxide, strontium oxide, manganese dioxide and nickel oxide.
4. The lead-free and cadmium-free glass frit as claimed in claim 1, wherein the corrosion resistance enhancer is one or both of ferric oxide and zirconium dioxide.
5. The preparation method of the lead-free and cadmium-free glass powder is characterized by comprising the following steps:
s1, weighing and uniformly mixing the raw materials in corresponding parts by weight, and carrying out heat preservation at the temperature of 1000-1300 ℃ for 2-3h to obtain glass liquid;
s2, pouring the glass liquid into water for water quenching, then adding alcohol, ball-milling to 1-3 mu m, and drying to obtain the lead-free and cadmium-free glass powder.
6. The conductive silver paste is characterized by comprising the following components in parts by weight:
2-5 parts of lead-free and cadmium-free glass powder;
9-34 parts of resin;
0.1-1 part of metal and oxide pigment thereof;
60-85 parts of silver powder;
0.2-0.3 part of dispersant;
0.2-0.3 part of leveling agent;
0.1-0.3 part of thixotropic agent;
10-20 parts of a solvent.
7. The conductive silver paste of claim 6, wherein the resin is one or more of ethyl cellulose, polyvinyl butyral, polypropylene resin, and rosin size resin.
8. The conductive silver paste of claim 6, wherein the metal and its oxide pigment is selected from any one or more of copper powder, zinc powder, titanium powder, bismuth powder or their oxides.
9. The conductive silver paste of claim 6, wherein said solvent is selected from any one or more of terpineol, diethylene glycol butyl ether and ethylene glycol butyl ether acetate.
10. The preparation method of the conductive silver paste is characterized by comprising the following steps:
mixing and stirring the lead-free and cadmium-free glass powder, the silver powder, the resin, the metal and metal oxide pigment, the dispersing agent, the flatting agent, the thixotropic agent and the solvent in corresponding parts by weight uniformly, and grinding the mixture until the particle size is less than or equal to 10 microns.
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Application publication date: 20200918 |