CN113257482B - Preparation method of anti-aging high-adhesion high-temperature sintered conductive silver paste - Google Patents
Preparation method of anti-aging high-adhesion high-temperature sintered conductive silver paste Download PDFInfo
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- CN113257482B CN113257482B CN202110649195.2A CN202110649195A CN113257482B CN 113257482 B CN113257482 B CN 113257482B CN 202110649195 A CN202110649195 A CN 202110649195A CN 113257482 B CN113257482 B CN 113257482B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 66
- 238000010438 heat treatment Methods 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000006185 dispersion Substances 0.000 claims abstract description 23
- 230000032683 aging Effects 0.000 claims abstract description 22
- 239000011521 glass Substances 0.000 claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 22
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000004094 surface-active agent Substances 0.000 claims abstract description 21
- 239000002562 thickening agent Substances 0.000 claims abstract description 21
- 239000013538 functional additive Substances 0.000 claims abstract description 19
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 48
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 26
- 238000004381 surface treatment Methods 0.000 claims description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 20
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 20
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 20
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 17
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- UGWRVHSFESMVND-UHFFFAOYSA-N silver;ethane-1,2-diol;nitrate Chemical compound [Ag+].OCCO.[O-][N+]([O-])=O UGWRVHSFESMVND-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 239000001569 carbon dioxide Substances 0.000 claims description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 14
- 238000000889 atomisation Methods 0.000 claims description 12
- 239000012159 carrier gas Substances 0.000 claims description 12
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 10
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000005751 Copper oxide Substances 0.000 claims description 10
- MUXOBHXGJLMRAB-UHFFFAOYSA-N Dimethyl succinate Chemical compound COC(=O)CCC(=O)OC MUXOBHXGJLMRAB-UHFFFAOYSA-N 0.000 claims description 10
- 239000001856 Ethyl cellulose Substances 0.000 claims description 10
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 10
- 229920000180 alkyd Polymers 0.000 claims description 10
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 10
- 229910000431 copper oxide Inorganic materials 0.000 claims description 10
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 10
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 10
- 229920001249 ethyl cellulose Polymers 0.000 claims description 10
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 10
- 235000021388 linseed oil Nutrition 0.000 claims description 10
- 239000000944 linseed oil Substances 0.000 claims description 10
- WIBFFTLQMKKBLZ-SEYXRHQNSA-N n-butyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCCCC WIBFFTLQMKKBLZ-SEYXRHQNSA-N 0.000 claims description 10
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 10
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 10
- -1 polydimethylsiloxane Polymers 0.000 claims description 10
- 229920000647 polyepoxide Polymers 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims description 10
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 10
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 8
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 8
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000005642 Oleic acid Substances 0.000 claims description 8
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 8
- 235000001014 amino acid Nutrition 0.000 claims description 8
- 150000001413 amino acids Chemical class 0.000 claims description 8
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 8
- PWEVMPIIOJUPRI-UHFFFAOYSA-N dimethyltin Chemical compound C[Sn]C PWEVMPIIOJUPRI-UHFFFAOYSA-N 0.000 claims description 8
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 6
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 6
- 239000001630 malic acid Substances 0.000 claims description 6
- 235000011090 malic acid Nutrition 0.000 claims description 6
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 6
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 6
- 229920000120 polyethyl acrylate Polymers 0.000 claims description 6
- 229950008882 polysorbate Drugs 0.000 claims description 6
- 229920000136 polysorbate Polymers 0.000 claims description 6
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 claims description 4
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 claims description 4
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 2
- 239000004475 Arginine Substances 0.000 claims description 2
- ODKSFYDXXFIFQN-BYPYZUCNSA-P L-argininium(2+) Chemical compound NC(=[NH2+])NCCC[C@H]([NH3+])C(O)=O ODKSFYDXXFIFQN-BYPYZUCNSA-P 0.000 claims description 2
- CKLJMWTZIZZHCS-REOHCLBHSA-N L-aspartic acid Chemical compound OC(=O)[C@@H](N)CC(O)=O CKLJMWTZIZZHCS-REOHCLBHSA-N 0.000 claims description 2
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims description 2
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 2
- AYFVYJQAPQTCCC-GBXIJSLDSA-N L-threonine Chemical compound C[C@@H](O)[C@H](N)C(O)=O AYFVYJQAPQTCCC-GBXIJSLDSA-N 0.000 claims description 2
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 claims description 2
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 claims description 2
- 239000004472 Lysine Substances 0.000 claims description 2
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 claims description 2
- AYFVYJQAPQTCCC-UHFFFAOYSA-N Threonine Natural products CC(O)C(N)C(O)=O AYFVYJQAPQTCCC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004473 Threonine Substances 0.000 claims description 2
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 claims description 2
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 claims description 2
- 235000003704 aspartic acid Nutrition 0.000 claims description 2
- OQFSQFPPLPISGP-UHFFFAOYSA-N beta-carboxyaspartic acid Natural products OC(=O)C(N)C(C(O)=O)C(O)=O OQFSQFPPLPISGP-UHFFFAOYSA-N 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 229930182817 methionine Natural products 0.000 claims description 2
- 239000004474 valine Substances 0.000 claims description 2
- 238000003466 welding Methods 0.000 abstract description 16
- 230000000052 comparative effect Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 229910021419 crystalline silicon Inorganic materials 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910017107 AlOx Inorganic materials 0.000 description 1
- 229910004205 SiNX Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011267 electrode slurry Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/022441—Electrode arrangements specially adapted for back-contact solar cells
Landscapes
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Power Engineering (AREA)
- Electromagnetism (AREA)
- Computer Hardware Design (AREA)
- Inorganic Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Manufacturing & Machinery (AREA)
- Conductive Materials (AREA)
Abstract
The invention discloses a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste, which comprises the following steps: adding an organic solvent into a reactor, sequentially adding a flatting agent, a surfactant, a defoaming agent and a thickening agent under stirring, heating, and continuously stirring until the organic solvent is dissolved to obtain an organic carrier; placing an organic carrier in a stirring dispersion machine, adding glass powder and a functional additive, stirring, then adding a nano silver wire, and stirring to obtain the anti-aging high-adhesion high-temperature sintered conductive silver paste; according to the invention, the nano silver wire is added into the conductive paste, and the prepared conductive paste can improve the electrical property of the battery piece, and the welding tension and the aging welding tension of the battery piece are obviously improved.
Description
Technical Field
The invention relates to a preparation method of conductive silver paste, in particular to a preparation method of anti-aging high-adhesion high-temperature sintered conductive silver paste.
Background
The high-temperature sintered conductive silver paste is used as a key basic material for manufacturing metal electrodes of electronic components, the application field of the high-temperature sintered conductive silver paste covers computers and communication equipment (such as 5G base stations and the like), integrated circuits and communication displays, solar cells, automobile manufacturing, various consumer electronic products and the like, the cost of the conductive silver paste accounts for 30% -70% of the cost of the electronic component materials, and the performance of the conductive silver paste directly influences the technical upgrading and cost reduction of the electronic components. The conductive silver paste generally consists of an organic carrier, functional powder and glass powder with a bonding effect at high temperature, integrates electronics, chemical engineering and metallurgy into a whole and has a high technical added value, and the electronic conductive paste is greatly developed when the electronic information industry enters a high-speed development stage. The conductive silver paste is a viscous paste of a mechanical mixture consisting of high-purity metal silver particles, a binder, a solvent and an auxiliary agent. Silver powder is the main component of the conductive silver paste, the silver powder is used as the conductive paste, the factors such as the three-dimensional shape, the size, the particle size distribution and the like of the particles of the conductive paste directly influence the electric conductivity and the heat conductivity, the micron or submicron silver powder is mainly adopted in the silver conductive paste at present, the welding machine tension of the solar cell prepared by adopting the conductive paste is smaller, the welding pressure after aging at 150 ℃ is lower, and the requirements of new technology cannot be met.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing an aging-resistant high-adhesion high-temperature sintering type conductive silver paste, comprising the steps of:
adding 55-65 parts by weight of organic solvent into a reactor, sequentially adding 2-8 parts of flatting agent, 3-6 parts of surfactant, 1-3 parts of defoaming agent and 25-38 parts of thickening agent under stirring at the speed of 150-180 r/min, heating to 75-85 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier;
placing 15-20 parts by weight of organic carrier into a stirring dispersion machine, adding 3-10 parts by weight of glass powder and 1-3 parts by weight of functional additive, stirring for 15-30 min at 1000-1200 r/min, then adding 30-45 parts by weight of nano silver wire, and stirring for 45-60 min at 1000-1200 r/min to obtain the anti-aging high-adhesion high-temperature sintered conductive silver paste;
the preparation method of the nano silver wire comprises the following steps: according to the weight portion, 85 portions of polyvinylpyrrolidone, 0.8-1.2 portions of potassium chloride and 2-5 portions of oleic acid are mixed and dissolved in 3000-4000 portions of ethylene glycol, the mixture is stirred and heated to 150 ℃ at the speed of 100-120 r/min, heating is stopped, 80-120 portions of silver nitrate ethylene glycol solution is dripped into the mixture at a constant speed, the mixture is cooled to room temperature after full reaction, the reaction is stopped, the obtained reaction solution is added into acetone, and the mixture is precipitated, so that the nano silver wire is obtained.
Preferably, in the first step, the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the leveling agent is methyl silicone oil or oleamide; the surfactant is polysorbate or polyethyl acrylate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1.
Preferably, in the second step, the glass powder comprises the following components in parts by weight: 5-10 parts of silicon dioxide, 8-12 parts of diboron trioxide, 20-30 parts of bismuth oxide, 5-8 parts of zirconium oxide, 10-15 parts of antimony trioxide, 8-12 parts of strontium oxide, 5-8 parts of copper oxide and 1-5 parts of vanadium pentoxide.
Preferably, in the second step, the functional additive is a mixture of functional additives in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate.
Preferably, the mass volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g: 3-4 mL.
Preferably, the prepared nano silver wire is pretreated by the following process: adding the nano silver wire into a supercritical carbon dioxide reactor, introducing carbon dioxide, soaking for 60-120 min by using supercritical carbon dioxide under the conditions that the temperature is 35-40 ℃ and the pressure is 10-18 MPa, and then decompressing; adding the treated nano silver wire into isopropanol A, and carrying out ultrasonic treatment for 15-30 min to obtain a nano silver wire dispersion liquid; and heating the nano silver wire dispersion liquid to 30-40 ℃, then atomizing the surface treatment solution, introducing the atomized surface treatment solution into the nano silver wire dispersion liquid through carrier gas, carrying out solid-liquid separation, washing the solid, and drying in vacuum to obtain the surface modified nano silver wire.
Preferably, the mass ratio of the nano silver wire to the supercritical carbon dioxide is 1: 5-15.
Preferably, the mass-volume ratio of the nano silver wire to the isopropanol A is 1g: 50-100 mL; the mass-volume ratio of the nano silver wire to the surface treatment solution is 1g: 120-180 mL; the process of atomizing the surface treatment solution is as follows: adding the surface treatment solution into an ultrasonic atomizer for ultrasonic atomization; the power of ultrasonic atomization is 1-12 kW, the frequency is 1.5-2.5 MHz, and the atomization rate is 0.1-1.2 kg/h; the carrier gas is nitrogen, and the flow rate of the carrier gas is 500-1000 mL/min.
Preferably, the surface treatment solution is prepared by a method comprising: adding citric acid, malic acid and amino acid into isopropanol B, and stirring at the speed of 300-500 r/min for 30-45 min to obtain a surface treatment solution; the mass ratio of the citric acid to the malic acid to the amino acid is 1: 2-3: 1-3; the mass ratio of the citric acid to the isopropanol B is 1: 500-800; the amino acid is one or more of tryptophan, threonine, arginine, aspartic acid, lysine, methionine, phenylalanine, serine and valine.
The invention at least comprises the following beneficial effects: according to the invention, the nano silver wire is added into the conductive paste, and the prepared conductive paste can improve the electrical property of the battery piece, and the welding tension and the aging welding tension of the battery piece are obviously improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
adding 55g of organic solvent into a reactor, sequentially adding 3g of flatting agent, 4g of surfactant, 1g of defoaming agent and 30g of thickening agent under stirring at the speed of 150r/min, heating to 80 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the flatting agent is oleamide; the surfactant is polysorbate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 18g of organic carrier into a stirring dispersion machine, adding 5g of glass powder and 2g of functional additive, stirring for 30min at 1200r/min, then adding 40g of nano silver wire, and stirring for 60min at 1200r/min to obtain the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 8g of silicon dioxide, 12g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 2g of vanadium pentoxide; the functional additive is prepared from the following components in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate;
the preparation method of the nano silver wire comprises the following steps: mixing 85g of polyvinylpyrrolidone, 0.8g of potassium chloride and 2g of oleic acid, dissolving in 3000g of ethylene glycol, stirring and heating at the speed of 100r/min to 150 ℃, then closing heating, dropwise adding 80g of silver nitrate ethylene glycol solution at a constant speed, cooling to room temperature after full reaction, stopping reaction, adding the obtained reaction solution into acetone, and precipitating to obtain a nano silver wire; the mass volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g:4 mL.
Example 2:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
step one, adding 60g of organic solvent into a reactor, sequentially adding 2g of flatting agent, 5g of surfactant, 3g of defoaming agent and 35g of thickening agent under stirring at the speed of 180r/min, heating to 85 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the leveling agent is methyl silicone oil; the surfactant is polyethylacrylate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 20g of organic carrier into a stirring dispersion machine, adding 6g of glass powder and 2g of functional additive, stirring for 30min at 1200r/min, then adding 45g of nano silver wire, and stirring for 60min at 1200r/min to obtain the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 10g of silicon dioxide, 10g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 3g of vanadium pentoxide; the functional additive is prepared from the following components in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate;
the preparation method of the nano silver wire comprises the following steps: mixing 85g of polyvinylpyrrolidone, 0.8g of potassium chloride and 2g of oleic acid, dissolving in 3000g of ethylene glycol, stirring and heating at the speed of 100r/min to 150 ℃, then closing heating, dropwise adding 80g of silver nitrate ethylene glycol solution at a constant speed, cooling to room temperature after full reaction, stopping reaction, adding the obtained reaction solution into acetone, and precipitating to obtain a nano silver wire; the mass volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g:4 mL.
Example 3:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
adding 55g of organic solvent into a reactor, sequentially adding 3g of flatting agent, 4g of surfactant, 1g of defoaming agent and 30g of thickening agent under stirring at the speed of 150r/min, heating to 80 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the flatting agent is oleamide; the surfactant is polysorbate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 18g of organic carrier into a stirring dispersion machine, adding 5g of glass powder and 2g of functional additive, stirring for 30min at 1200r/min, then adding 40g of nano silver wire, and stirring for 60min at 1200r/min to obtain the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 8g of silicon dioxide, 12g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 2g of vanadium pentoxide; the functional additive is prepared from the following components in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate;
the preparation method of the nano silver wire comprises the following steps: mixing 85g of polyvinylpyrrolidone, 0.8g of potassium chloride and 2g of oleic acid, dissolving in 3000g of ethylene glycol, stirring and heating at the speed of 100r/min to 150 ℃, then closing heating, dropwise adding 80g of silver nitrate ethylene glycol solution at a constant speed, cooling to room temperature after full reaction, stopping reaction, adding the obtained reaction solution into acetone, and precipitating to obtain a nano silver wire; the mass volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g:4 mL;
the prepared nano silver wire is pretreated, and the process comprises the following steps: adding 1g of nano silver wire into a supercritical carbon dioxide reactor, introducing carbon dioxide, soaking 10g of supercritical carbon dioxide for 90min at the temperature of 38 ℃ and the pressure of 12MPa, and then decompressing; adding the treated nano silver wire into 80mL of isopropanol A, and carrying out ultrasonic treatment for 15min to obtain a nano silver wire dispersion liquid; heating the nano-silver wire dispersion liquid to 30 ℃, then atomizing 120mL of surface treatment solution, introducing the atomized surface treatment solution into the nano-silver wire dispersion liquid through carrier gas, carrying out solid-liquid separation, washing solids, and drying in vacuum to obtain a surface-modified nano-silver wire; the process of atomizing the surface treatment solution is as follows: adding the surface treatment solution into an ultrasonic atomizer for ultrasonic atomization; the power of ultrasonic atomization is 6kW, the frequency is 2.4MHz, and the atomization rate is 0.5 kg/h; the carrier gas is nitrogen, and the flow rate of the carrier gas is 800 mL/min; the preparation method of the surface treatment solution comprises the following steps: adding 1g of citric acid, 2g of malic acid and 2g of amino acid (1g of tryptophan and 1g of phenylalanine) into 600g of isopropanol B, and stirring at the speed of 300r/min for 45min to obtain a surface treatment solution;
example 4:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
step one, adding 60g of organic solvent into a reactor, sequentially adding 2g of flatting agent, 5g of surfactant, 3g of defoaming agent and 35g of thickening agent under stirring at the speed of 180r/min, heating to 85 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the leveling agent is methyl silicone oil; the surfactant is polyethylacrylate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 20g of organic carrier into a stirring dispersion machine, adding 6g of glass powder and 2g of functional additive, stirring for 30min at 1200r/min, then adding 45g of nano silver wire, and stirring for 60min at 1200r/min to obtain the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 10g of silicon dioxide, 10g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 3g of vanadium pentoxide; the functional additive is prepared from the following components in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate;
the preparation method of the nano silver wire comprises the following steps: mixing 85g of polyvinylpyrrolidone, 0.8g of potassium chloride and 2g of oleic acid, dissolving in 3000g of ethylene glycol, stirring and heating at the speed of 100r/min to 150 ℃, then closing heating, dropwise adding 80g of silver nitrate ethylene glycol solution at a constant speed, cooling to room temperature after full reaction, stopping reaction, adding the obtained reaction solution into acetone, and precipitating to obtain a nano silver wire; the mass volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g:4 mL;
the prepared nano silver wire is pretreated, and the process comprises the following steps: adding 1g of nano silver wire into a supercritical carbon dioxide reactor, introducing carbon dioxide, soaking for 90min by 15g of supercritical carbon dioxide at the temperature of 40 ℃ and the pressure of 15MPa, and then decompressing; adding the treated nano silver wire into 100mL of isopropanol A, and carrying out ultrasonic treatment for 15min to obtain a nano silver wire dispersion liquid; heating the nano-silver wire dispersion liquid to 30 ℃, then atomizing 120mL of surface treatment solution, introducing the atomized surface treatment solution into the nano-silver wire dispersion liquid through carrier gas, carrying out solid-liquid separation, washing solids, and drying in vacuum to obtain a surface-modified nano-silver wire; the process of atomizing the surface treatment solution is as follows: adding the surface treatment solution into an ultrasonic atomizer for ultrasonic atomization; the power of ultrasonic atomization is 6kW, the frequency is 2.4MHz, and the atomization rate is 0.5 kg/h; the carrier gas is nitrogen, and the flow rate of the carrier gas is 800 mL/min; the preparation method of the surface treatment solution comprises the following steps: adding 1g of citric acid, 2g of malic acid and 3g of amino acid (2g of tryptophan and 1g of phenylalanine) into 700g of isopropanol B, and stirring at the speed of 300r/min for 45min to obtain a surface treatment solution;
comparative example 1:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
adding 55g of organic solvent into a reactor, sequentially adding 3g of flatting agent, 4g of surfactant, 1g of defoaming agent and 30g of thickening agent under stirring at the speed of 150r/min, heating to 80 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the flatting agent is oleamide; the surfactant is polysorbate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 18g of organic carrier into a stirring dispersion machine, adding 5g of glass powder and 2g of functional additive, stirring for 30min at 1200r/min, then adding 40g of nano silver powder (D50 is 50nm), stirring for 60min at 1200r/min, and obtaining the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 8g of silicon dioxide, 12g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 2g of vanadium pentoxide; the functional additive is prepared from the following components in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate.
Comparative example 2:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
step one, adding 60g of organic solvent into a reactor, sequentially adding 2g of flatting agent, 5g of surfactant, 3g of defoaming agent and 35g of thickening agent under stirring at the speed of 180r/min, heating to 85 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the leveling agent is methyl silicone oil; the surfactant is polyethylacrylate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 20g of organic carrier into a stirring dispersion machine, adding 6g of glass powder and 2g of functional additive, stirring for 30min at 1200r/min, then adding 45g of nano silver powder (D50 is 50nm), stirring for 60min at 1200r/min, and obtaining the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 10g of silicon dioxide, 10g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 3g of vanadium pentoxide; the functional additive is prepared from the following components in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate;
comparative example 3:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
adding 55g of organic solvent into a reactor, sequentially adding 3g of flatting agent, 4g of surfactant, 1g of defoaming agent and 30g of thickening agent under stirring at the speed of 150r/min, heating to 80 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the flatting agent is oleamide; the surfactant is polysorbate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 18g of organic carrier into a stirring dispersion machine, adding 5g of glass powder, stirring for 30min at 1200r/min, then adding 40g of nano silver wire, and stirring for 60min at 1200r/min to obtain the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 8g of silicon dioxide, 12g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 2g of vanadium pentoxide; the preparation method of the nano silver wire comprises the following steps: mixing 85g of polyvinylpyrrolidone, 0.8g of potassium chloride and 2g of oleic acid, dissolving in 3000g of ethylene glycol, stirring and heating at the speed of 100r/min to 150 ℃, then closing heating, dropwise adding 80g of silver nitrate ethylene glycol solution at a constant speed, cooling to room temperature after full reaction, stopping reaction, adding the obtained reaction solution into acetone, and precipitating to obtain a nano silver wire; the mass volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g:4 mL.
Comparative example 4:
a preparation method of an anti-aging high-adhesion high-temperature sintered conductive silver paste comprises the following steps:
step one, adding 60g of organic solvent into a reactor, sequentially adding 2g of flatting agent, 5g of surfactant, 3g of defoaming agent and 35g of thickening agent under stirring at the speed of 180r/min, heating to 85 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier; the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate with the mass ratio of 1:2:2: 1; the leveling agent is methyl silicone oil; the surfactant is polyethylacrylate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1;
placing 20g of organic carrier into a stirring dispersion machine, adding 6g of glass powder, stirring for 30min at 1200r/min, then adding 45g of nano silver wire, and stirring for 60min at 1200r/min to obtain the aging-resistant high-adhesion high-temperature sintered conductive silver paste; the glass powder comprises: 10g of silicon dioxide, 10g of diboron trioxide, 25g of bismuth oxide, 5g of zirconium oxide, 10g of antimony trioxide, 8g of strontium oxide, 5g of copper oxide and 3g of vanadium pentoxide; the preparation method of the nano silver wire comprises the following steps: mixing 85g of polyvinylpyrrolidone, 0.8g of potassium chloride and 2g of oleic acid, dissolving in 3000g of ethylene glycol, stirring and heating at the speed of 100r/min to 150 ℃, then closing heating, dropwise adding 80g of silver nitrate ethylene glycol solution at a constant speed, cooling to room temperature after full reaction, stopping reaction, adding the obtained reaction solution into acetone, and precipitating to obtain a nano silver wire; the mass volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g:4 mL.
Preparing a crystalline silicon solar cell by adopting a conventional preparation method of the crystalline silicon solar cell, taking a crystalline silicon cell silicon wafer, treating an antireflection film layer on the front surface of the silicon wafer, and treating the back surface of the silicon wafer by AlOx/SiNxPassivating the laminated film; printing the prepared conductive slurry on the back of a silicon wafer of a crystalline silicon battery, and forming a back electrode on the back of the silicon waferA pole pattern; drying and sintering the back electrode pattern, wherein the drying temperature is 280 ℃, the sintering temperature is 800 ℃, and the back electrode slurry formed by drying and sintering can not burn through the passivation layer on the back; welding tension tests are carried out on the sintered battery pieces (the welding conditions are that 2X 0.2mm tin-lead welding strips are used, welding is carried out at 345 ℃, a tension tester is used for testing tension, 180-degree stripping tension tests are carried out, 6 battery pieces are tested in each group, the average value is taken), aging welding tension tests are carried out (the welding conditions are that 2X 0.2mm tin-lead welding strips are used, welding is carried out at 345 ℃, the welded battery pieces are placed in an aging box at the temperature of 150 ℃ after welding, the tension tester is taken out after 1h, 180-degree stripping tension tests are carried out, 6 battery pieces are tested in each group, the average value is taken), and electrical performance tests (6 finished products are manufactured and tested in each embodiment and comparative example, and the average value is taken); eta is the conversion efficiency in the electrical property test of the solar cell; the results are shown in table 1:
TABLE 1
| Eta (conversion efficiency) | Welding tension | Aged weld pull | |
| Example 1 | 19.15％ | 5.5N | 4.1N |
| Example 2 | 19.20％ | 5.6N | 4.2N |
| Example 3 | 20.68％ | 6.2N | 4.6N |
| Example 4 | 20.72％ | 6.4N | 4.7N |
| Comparative example 1 | 16.58％ | 3.6N | 1.7N |
| Comparative example 2 | 16.51％ | 3.4N | 1.6N |
| Comparative example 3 | 17.15％ | 4.9N | 3.5N |
| Comparative example 4 | 17.18％ | 4.8N | 3.3N |
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the examples shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (8)
1. The preparation method of the aging-resistant high-adhesion high-temperature sintered conductive silver paste is characterized by comprising the following steps of:
adding 55-65 parts by weight of organic solvent into a reactor, sequentially adding 2-8 parts of flatting agent, 3-6 parts of surfactant, 1-3 parts of defoaming agent and 25-38 parts of thickening agent under stirring at the speed of 150-180 r/min, heating to 75-85 ℃, and continuously stirring until the mixture is dissolved to obtain an organic carrier;
placing 15-20 parts by weight of organic carrier into a stirring dispersion machine, adding 3-10 parts by weight of glass powder and 1-3 parts by weight of functional additive, stirring for 15-30 min at 1000-1200 r/min, then adding 30-45 parts by weight of nano silver wire, and stirring for 45-60 min at 1000-1200 r/min to obtain the anti-aging high-adhesion high-temperature sintered conductive silver paste;
the preparation method of the nano silver wire comprises the following steps: mixing 85 parts by weight of polyvinylpyrrolidone, 0.8-1.2 parts by weight of potassium chloride and 2-5 parts by weight of oleic acid, dissolving the mixture in 3000-4000 parts by weight of ethylene glycol, stirring and heating at a speed of 100-120 r/min to 150 ℃, then turning off heating, dropwise adding 80-120 parts by weight of silver nitrate ethylene glycol solution at a constant speed, cooling to room temperature after full reaction, stopping the reaction, adding the obtained reaction solution into acetone, and precipitating to obtain a nano-silver wire;
the prepared nano silver wire is pretreated, and the process comprises the following steps: adding the nano silver wire into a supercritical carbon dioxide reactor, introducing carbon dioxide, soaking for 60-120 min by using supercritical carbon dioxide under the conditions that the temperature is 35-40 ℃ and the pressure is 10-18 MPa, and then decompressing; adding the treated nano silver wire into isopropanol A, and carrying out ultrasonic treatment for 15-30 min to obtain a nano silver wire dispersion liquid; heating the nano-silver wire dispersion liquid to 30-40 ℃, then atomizing the surface treatment solution, introducing the atomized surface treatment solution into the nano-silver wire dispersion liquid through carrier gas, carrying out solid-liquid separation, and washing the solid; and (5) drying in vacuum to obtain the surface-modified nano silver wire.
2. The method for preparing the aging-resistant high-adhesion high-temperature sintered conductive silver paste as claimed in claim 1, wherein in the first step, the organic solvent is n-butanol, butyl carbitol, dimethyl succinate and butyl oleate in a mass ratio of 1:2:2: 1; the leveling agent is methyl silicone oil or oleamide; the surfactant is polysorbate or polyethyl acrylate; the defoaming agent is polydimethylsiloxane; the thickening agent is ethyl cellulose, epoxy resin and linseed oil pentaerythritol alkyd resin in a mass ratio of 1:2: 1.
3. The method for preparing the aging-resistant high-adhesion high-temperature sintered conductive silver paste according to claim 1, wherein in the second step, the glass powder comprises the following components in parts by weight: 5-10 parts of silicon dioxide, 8-12 parts of diboron trioxide, 20-30 parts of bismuth oxide, 5-8 parts of zirconium oxide, 10-15 parts of antimony trioxide, 8-12 parts of strontium oxide, 5-8 parts of copper oxide and 1-5 parts of vanadium pentoxide.
4. The method for preparing the aging-resistant high-adhesion high-temperature sintered conductive silver paste according to claim 1, wherein in the second step, the functional additive is the mixture of functional additives in a mass ratio of 1: 3:1 dimethyltin, tellurium dioxide and tetrabutyl titanate.
5. The preparation method of the aging-resistant high-adhesion high-temperature sintered conductive silver paste as claimed in claim 1, wherein the mass-to-volume ratio of silver nitrate to ethylene glycol in the silver nitrate ethylene glycol solution is 1g: 3-4 mL.
6. The preparation method of the aging-resistant high-adhesion high-temperature sintered conductive silver paste as claimed in claim 1, wherein the mass ratio of the nano silver wires to the supercritical carbon dioxide is 1: 5-15.
7. The preparation method of the aging-resistant high-adhesion high-temperature sintered conductive silver paste as claimed in claim 1, wherein the mass-to-volume ratio of the nano silver wires to the isopropanol A is 1g: 50-100 mL; the mass-volume ratio of the nano silver wire to the surface treatment solution is 1g: 120-180 mL; the process of atomizing the surface treatment solution is as follows: adding the surface treatment solution into an ultrasonic atomizer for ultrasonic atomization; the power of ultrasonic atomization is 1-12 kW, the frequency is 1.5-2.5 MHz, and the atomization rate is 0.1-1.2 kg/h; the carrier gas is nitrogen, and the flow rate of the carrier gas is 500-1000 mL/min.
8. The method for preparing the aging-resistant high-adhesion high-temperature sintered conductive silver paste according to claim 1, wherein the method for preparing the surface treatment solution comprises the following steps: adding citric acid, malic acid and amino acid into isopropanol B, and stirring at the speed of 300-500 r/min for 30-45 min to obtain a surface treatment solution; the mass ratio of the citric acid to the malic acid to the amino acid is 1: 2-3: 1-3; the mass ratio of the citric acid to the isopropanol B is 1: 500-800; the amino acid is one or more of tryptophan, threonine, arginine, aspartic acid, lysine, methionine, phenylalanine, serine and valine.
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