CN108806823A - Environment-friendlyconductive conductive silver paste material and preparation method thereof and crystal silicon solar batteries prepared therefrom - Google Patents
Environment-friendlyconductive conductive silver paste material and preparation method thereof and crystal silicon solar batteries prepared therefrom Download PDFInfo
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- CN108806823A CN108806823A CN201810612413.3A CN201810612413A CN108806823A CN 108806823 A CN108806823 A CN 108806823A CN 201810612413 A CN201810612413 A CN 201810612413A CN 108806823 A CN108806823 A CN 108806823A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000000463 material Substances 0.000 title claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 29
- 239000010703 silicon Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000013078 crystal Substances 0.000 title claims abstract description 17
- 239000011521 glass Substances 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000013329 compounding Methods 0.000 claims abstract description 25
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 claims abstract description 16
- 239000004332 silver Substances 0.000 claims abstract description 16
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 15
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 230000007613 environmental effect Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- OTCVAHKKMMUFAY-UHFFFAOYSA-N oxosilver Chemical class [Ag]=O OTCVAHKKMMUFAY-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 20
- 239000002002 slurry Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical group CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims description 8
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 239000000908 ammonium hydroxide Substances 0.000 claims description 7
- 239000004359 castor oil Substances 0.000 claims description 7
- 235000019438 castor oil Nutrition 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 7
- 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 claims description 7
- 239000004519 grease Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920002689 polyvinyl acetate Polymers 0.000 claims description 6
- 239000011118 polyvinyl acetate Substances 0.000 claims description 6
- 230000009974 thixotropic effect Effects 0.000 claims description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- -1 polyethylene Acetate Polymers 0.000 claims description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 claims 1
- 244000248349 Citrus limon Species 0.000 claims 1
- 235000005979 Citrus limon Nutrition 0.000 claims 1
- 238000013019 agitation Methods 0.000 claims 1
- 230000005496 eutectics Effects 0.000 claims 1
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000000969 carrier Substances 0.000 description 6
- 238000007639 printing Methods 0.000 description 5
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- KTADSLDAUJLZGL-UHFFFAOYSA-N 1-bromo-2-phenylbenzene Chemical group BrC1=CC=CC=C1C1=CC=CC=C1 KTADSLDAUJLZGL-UHFFFAOYSA-N 0.000 description 1
- 229910017982 Ag—Si Inorganic materials 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- 229910020617 PbO—B2O3—SiO2 Inorganic materials 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- ZCILODAAHLISPY-UHFFFAOYSA-N biphenyl ether Natural products C1=C(CC=C)C(O)=CC(OC=2C(=CC(CC=C)=CC=2)O)=C1 ZCILODAAHLISPY-UHFFFAOYSA-N 0.000 description 1
- 150000004074 biphenyls Chemical class 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- YGBMCLDVRUGXOV-UHFFFAOYSA-N n-[6-[6-chloro-5-[(4-fluorophenyl)sulfonylamino]pyridin-3-yl]-1,3-benzothiazol-2-yl]acetamide Chemical group C1=C2SC(NC(=O)C)=NC2=CC=C1C(C=1)=CN=C(Cl)C=1NS(=O)(=O)C1=CC=C(F)C=C1 YGBMCLDVRUGXOV-UHFFFAOYSA-N 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of 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
-
- 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
- H01L31/022433—Particular geometry of the grid contacts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Landscapes
- Engineering & Computer Science (AREA)
- Electromagnetism (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Conductive Materials (AREA)
Abstract
The present invention is disclosed for a kind of environment-friendlyconductive conductive silver paste material and preparation method thereof and crystal silicon solar batteries prepared therefrom, environment-friendlyconductive conductive silver paste material is by compounding silver powder, high-performance Pb-free glass powder and organic carrier composition, wherein the compounding silver powder is to contain the micro-silver powder that mass fraction is 4-9% superfine silver oxides.Compared with prior art, the present invention is compounded using superfine silver oxide with micro-silver powder, be conducive to the formation of fine and close smooth silver film, with larger tap density and higher sintering activity, the unleaded of crystal silicon solar batteries front conductive silver slurry is realized using high-performance Pb-free glass powder, pass through the adjusting of organic carrier component and content, improve the surface tension and itself rheological property of conductive silver paste, the environment-friendlyconductive conductive silver paste material of the present invention has good thixotropy, low contact resistance, the crystal silicon solar cell sheet photoelectric conversion efficiency of preparation reaches 17.9%~18.1%, new energy can be developed, meet environmental protection concept again, it has broad application prospects.
Description
Technical field
The present invention relates to technical field of solar batteries, more particularly to a kind of environment-friendlyconductive conductive silver paste material and preparation method thereof,
With crystal silicon solar batteries prepared therefrom.
Background technology
Solar cell is as a kind of green energy resource, inexhaustible with its, pollution-free, the advantages that not limited by resource advantage
Increasingly it is valued by people, thus, in recent years, crystal silicon solar energy battery is as main solar energy power generating unit
It is rapidly developed, wherein solar battery front side is the important component of crystal silicon solar energy battery, is used as and directly connects
The one side for receiving solar energy is consumed by multilayered structure in the hope of reaching widest reception spectral line and minimum light reflection.It is conventional commercial
Crystal silicon solar energy battery front include silver electrode grid line, antireflection layer, n-type diffusion layer, four floor primary structures of p-n junction area.
Currently, the production method of commercial crystal silicon solar cell front electrode, generally use printing and inkjet printing are led
Electric silver paste forms depth-width ratio grid line structure as big as possible, then passes through Fast Sintering process, and formation closely connects with n-type diffusion layer
Tactile conductive electrode typically contains silver powder, glass powder and organic carrier in the conductive silver paste.In crystal silicon solar energy battery
In, electric conductivity will be got well in the case of obtaining maximum light-receiving area, and the electric energy that silicon chip is generated to the greatest extent, which exports, to be come, this
It requires the thixotropy of front electronic silver paste good, the big grid line of depth-width ratio can be printed off, open-circuit voltage is big after sintering, series resistance
It is small, parallel resistance is big etc..And the RoHS instructions of European Union are also followed (without Pb, Cd, Hg, Cr (VI), polybrominated biphenyls PBB, more
Bromo biphenyl ether PBDE) and European Union RoHS about phthalic acid ester instruction 2005/84/EC industry environmental protection standard.
Invention content
In order to solve the above technical problems, the present invention provides a kind of environment-friendlyconductive conductive silver paste material and preparation method thereof and by its system
Standby crystal silicon solar batteries improve electricity conversion, meet the requirement of environmental protection, improve silver to solve to reduce series resistance
Conductor paste sintering quality and with good thixotropic problem.
The technical solution adopted by the present invention is as follows：A kind of environment-friendlyconductive conductive silver paste material, key are by following mass fraction
Raw material forms：Compound 75-85 parts of silver powder, 8-15 parts of high-performance Pb-free glass powder, 15-25 parts of organic carrier；
The wherein described compounding silver powder is to contain the micro-silver powder that mass fraction is 4-9% superfine silver oxides.
Preferably, the mass fraction of the raw material is：Compound 82 parts of silver powder, 9 parts of high-performance Pb-free glass powder, organic carrier
20 parts, wherein the compounding silver powder is to contain the micro-silver powder that mass fraction is 5% superfine silver oxide.
Preferably, the compounding silver powder is made using following methods：It is 0.5mol/L's that ammonium hydroxide, which is added dropwise to mass concentration,
In silver nitrate solution, the molar ratio of ammonium hydroxide and silver nitrate is (1-4)：1, it is uniformly mixed and obtains mixed solution A, be 1 by mass ratio：
The oleic acid of (1-1.2) is uniformly mixed to obtain mixed solution B with the ascorbic acid solution that mass concentration is 1.5mol/L, then will be molten
Liquid A is added dropwise in reactor simultaneously with solution B, and the mass ratio of solution A and solution B is (18-40)：1, reaction temperature 15-45
DEG C, after the completion of reaction, filter residue is obtained by filtration in reactant by reaction time 2-5h, and filter residue is used deionized water and anhydrous successively
Ethyl alcohol washs, and washed product dry 4h under 50 DEG C of vacuum obtains the micro-silver powder, and the grain size of the micro-silver powder is 0.8-
2.5 μm, tap density 3.8-5.5g/cm3, then superfine silver oxide and micro-silver powder are uniformly mixed and obtain the compounding silver
Powder.
Preferably, the high-performance Pb-free glass powder is glass powder with low melting point, and softening point is 370 DEG C~480 DEG C.
Preferably, the inorganic constituents of the high-performance Pb-free glass powder and corrresponding quality percentage are：Bi2O3 60-
80%, SiO210-20%, TiO24-8%, ZrO56-12%.
Preferably, the organic carrier presses following mass percentage composition：Organic solvent 70-80%, urea-base grease 13-
16%, polyvinyl acetate 6-9%, castor oil 1-5%.
Preferably, the organic solvent be terpinol, tributyl citrate and butyl carbitol acetate mixed solvent,
The mass ratio of terpinol, tributyl citrate and butyl carbitol acetate is (8-5)：(4-2)：1.
Preferably, the organic carrier is made using following methods：Organic solvent is heated to 50-80 DEG C, urea groups is added
Lubricating grease stirs and is warming up to 250-290 DEG C, and polyvinyl acetate is added, and stirs and is warming up to 150-200 DEG C, is then added
Castor oil continues to stir 5-15min, is cooled to room temperature to obtain the organic carrier.
A kind of preparation method of environment-friendlyconductive conductive silver paste material, key are to include the following steps：
Step 1: preparing compounding silver powder and organic carrier respectively；
Step 2: by Bi2O3、SiO2、TiO2、ZrO5After mixing well, in 1100-1250 DEG C of 30~50min of melting, it will melt
The glass melted is poured into quenching-in water, and quenched glass blocks is passed through secondary grinding, obtains the high-performance that grain size is 1 μm~4 μm
Lead-free glass powder；
Step 3: heating stirring is uniform at 70~110 DEG C after the organic carrier for compounding silver powder and 3/5 is mixed, then
Silver powder slurry is obtained after ground machine dispersion, at 70~110 DEG C after the organic carrier of high-performance Pb-free glass powder and 2/5 is mixed
Lower heating stirring is uniform, then obtains glass paste after ground machine dispersion；
Step 4: silver powder slurry and the further mixed grinding of glass paste are uniformly obtained into the environment-friendlyconductive conductive silver paste material,
The granularity of the environment-friendlyconductive conductive silver paste material is 2.0-8.0 μm, viscosity 250-290Pas, and thixotropic index is 5.0~7.0.
A kind of crystal silicon solar batteries, the solar cell include silicon chip and the silver electrode grid line on silicon chip, are closed
Key is：The silver electrode grid line is by the environment-friendlyconductive conductive silver paste material described in the silk-screen printing any of the above item on silicon chip, then
It is obtained after drying, sintering.
Advantageous effect：Compared with prior art, the present invention provides a kind of environment-friendlyconductive conductive silver paste material and preparation method thereof and
Crystal silicon solar batteries prepared therefrom, are compounded using superfine silver oxide and micro-silver powder, are conducive to fine and close smooth silver
The formation of film layer can effectively improve electrode aspect ratio, reduce resistivity, and the granularity of micro-silver powder is moderate, has larger
The silver micro-crystallite size and number of tap density and higher sintering activity, the interfaces Ag-Si is moderate, with make battery with higher
Transfer efficiency；Enhance the properties of conductive silver paste；Crystal silicon solar batteries are being realized just using high-performance Pb-free glass powder
Face conductive silver slurry it is unleaded, and basically reach the performance of leaded slurry；By the adjusting of organic carrier component and content,
The evaporation rate of effective control organic carrier, makes the surface tension of conductive silver paste and itself rheological property be improved, makes
It is significantly improved in the levelling ability of silicon chip surface, and the electrode formed after silver paste printing actually connects with the silicon chip of its bottom
Contacting surface product increases, and the contact resistance of electrode and silicon chip reduces, and corresponding battery strings resistance reduces, and the transfer efficiency of battery is carried
It rises.The present invention environment-friendlyconductive conductive silver paste material have good thixotropy, low contact resistance and low monolithic need to the amount of slurry, preparation
Crystal silicon solar cell sheet photoelectric conversion efficiency reaches 17.9%~18.1%.The present invention both meets the need of development new energy
Ask, and meet environmental protection concept, can high-volume continuous production, have broad application prospects.
Specific implementation mode
To make those skilled in the art be better understood from technical scheme of the present invention, With reference to embodiment to this
Invention elaborates.
The preparation of 1 environment-friendlyconductive conductive silver paste material I of embodiment
Step 1: the preparation of compounding silver powder：Ammonium hydroxide is added dropwise in the silver nitrate solution that mass concentration is 0.5mol/L, ammonia
The molar ratio of water and silver nitrate is 1：1, it is uniformly mixed and obtains mixed solution A, be 1 by mass ratio：1 oleic acid is with mass concentration
The ascorbic acid solution of 1.5mol/L is uniformly mixed and obtains mixed solution B, is then added dropwise to solution A simultaneously with solution B and reacts
In device, the mass ratio of solution A and solution B is 18：1, reaction temperature is 15-45 DEG C, reaction time 2-5h, after the completion of reaction,
Filter residue is obtained by filtration in reactant, filter residue is washed with deionized water and absolute ethyl alcohol successively, washed product is under 50 DEG C of vacuum
Dry 4h obtains the micro-silver powder, and the grain size of the micro-silver powder is 0.8 μm, tap density 3.8g/cm3, then by matter
Amount is than being 4：96 superfine silver oxide and micro-silver powder is uniformly mixed and obtains the compounding silver powder, the grain size of the superfine silver oxide
It is 1.2-5 μm；
The preparation of organic carrier：It is 8 by mass ratio：4：1 terpinol, tributyl citrate and butyl carbitol acetate
It is mixed into organic solvent, the organic solvent that mass percent is 70% is then heated to 50-80 DEG C, mass percent is added
For 16% urea-base grease, stirs and be warming up to 250-290 DEG C, the polyvinyl acetate that addition mass percent is 9% stirs
It mixes and is warming up to 150-200 DEG C, the castor oil that mass percent is 5% is then added, continue to stir 5-15min, be cooled to room
Temperature obtains the organic carrier；
Step 2: by Bi2O360%, SiO220%, TiO28%, ZrO5After 12% mixes well, at 1100-1250 DEG C
The glass of melting is poured into quenching-in water by 30~50min of melting, and quenched glass blocks is passed through secondary grinding, obtains grain size
It is 1 μm, the high-performance Pb-free glass powder that softening point is 480 DEG C,；
Step 3: heating stirring is uniform at 70~110 DEG C after 75 parts of compounding silver powder and 9 parts of organic carriers are mixed, so
Silver powder slurry is obtained after disperseing by grinder, after 8 parts of high-performance Pb-free glass powders and 6 parts of organic carriers are mixed 70~
Heating stirring is uniform at 110 DEG C, then obtains glass paste after ground machine dispersion；
Step 4: it is 2.0 μm that silver powder slurry and the further mixed grinding of glass paste, which are uniformly obtained granularity, viscosity is
290Pas, the conductive silver paste I that thixotropic index is 5.0.
The preparation of 2 environment-friendlyconductive conductive silver paste material II of embodiment
Step 1: the preparation of compounding silver powder：Ammonium hydroxide is added dropwise in the silver nitrate solution that mass concentration is 0.5mol/L, ammonia
The molar ratio of water and silver nitrate is 4：1, it is uniformly mixed and obtains mixed solution A, be 1 by mass ratio：1.2 oleic acid and mass concentration
It is uniformly mixed for the ascorbic acid solution of 1.5mol/L and obtains mixed solution B, be then added dropwise to solution A and solution B instead simultaneously
It answers in device, the mass ratio of solution A and solution B is 40：1, reaction temperature is 15-45 DEG C, reaction time 2-5h, and reaction is completed
Afterwards, filter residue is obtained by filtration in reactant, filter residue is washed with deionized water and absolute ethyl alcohol successively, washed product is in 50 DEG C of vacuum
Lower dry 4h obtains the micro-silver powder, and the grain size of the micro-silver powder is 2.5 μm, tap density 5.5g/cm3, then will
Mass ratio is 9：91 superfine silver oxide and micro-silver powder is uniformly mixed and obtains the compounding silver powder, the grain of the superfine silver oxide
Diameter is 1.2-5 μm；
The preparation of organic carrier：It is 5 by mass ratio：2：1 terpinol, tributyl citrate and butyl carbitol acetate
It is mixed into organic solvent, the organic solvent that mass percent is 80% is then heated to 50-80 DEG C, mass percent is added
For 13% urea-base grease, stirs and be warming up to 250-290 DEG C, the polyvinyl acetate that addition mass percent is 6% stirs
It mixes and is warming up to 150-200 DEG C, the castor oil that mass percent is 1% is then added, continue to stir 5-15min, be cooled to room
Temperature obtains the organic carrier；
Step 2: by Bi2O380%, SiO210%, TiO24%, ZrO5After 6% mixes well, melted at 1100-1250 DEG C
30~50min is refined, the glass of melting is poured into quenching-in water, quenched glass blocks is passed through into secondary grinding, it is 4 to obtain grain size
μm, the high-performance Pb-free glass powder that softening point is 430 DEG C；
Step 3: heating stirring is uniform at 70~110 DEG C after 85 parts of compounding silver powder and 15 parts of organic carriers are mixed, so
Silver powder slurry is obtained after disperseing by grinder, after 8 parts of high-performance Pb-free glass powders and 10 parts of organic carriers are mixed 70~
Heating stirring is uniform at 110 DEG C, then obtains glass paste after ground machine dispersion；
Step 4: it is 8.0 μm that silver powder slurry and the further mixed grinding of glass paste, which are uniformly obtained granularity, viscosity is
250Pas, the conductive silver paste II that thixotropic index is 7.0.
The preparation of 3 environment-friendlyconductive conductive silver paste material III of embodiment
Step 1: the preparation of compounding silver powder：Ammonium hydroxide is added dropwise in the silver nitrate solution that mass concentration is 0.5mol/L, ammonia
The molar ratio of water and silver nitrate is 3：1, it is uniformly mixed and obtains mixed solution A, be 1 by mass ratio：1.1 oleic acid and mass concentration
It is uniformly mixed for the ascorbic acid solution of 1.5mol/L and obtains mixed solution B, be then added dropwise to solution A and solution B instead simultaneously
It answers in device, the mass ratio of solution A and solution B is 25：1, reaction temperature is 15-45 DEG C, reaction time 2-5h, and reaction is completed
Afterwards, filter residue is obtained by filtration in reactant, filter residue is washed with deionized water and absolute ethyl alcohol successively, washed product is in 50 DEG C of vacuum
Lower dry 4h obtains the micro-silver powder, and the grain size of the micro-silver powder is 1.7 μm, tap density 5.1g/cm3, then will
Mass ratio is 5：95 superfine silver oxide and micro-silver powder is uniformly mixed and obtains the compounding silver powder, the grain of the superfine silver oxide
Diameter is 1.2-5 μm；
The preparation of organic carrier：It is 7 by mass ratio：3：1 terpinol, tributyl citrate and butyl carbitol acetate
It is mixed into organic solvent, the organic solvent that mass percent is 75% is then heated to 50-80 DEG C, mass percent is added
For 15% urea-base grease, stirs and be warming up to 250-290 DEG C, the polyvinyl acetate that addition mass percent is 7% stirs
It mixes and is warming up to 150-200 DEG C, the castor oil that mass percent is 3% is then added, continue to stir 5-15min, be cooled to room
Temperature obtains the organic carrier；
Step 2: by Bi2O378%, SiO212%, TiO26%, ZrO5After 4% mixes well, at 1100-1250 DEG C
The glass of melting is poured into quenching-in water by 30~50min of melting, and quenched glass blocks is passed through secondary grinding, obtains grain size
It is 1.5 μm, the high-performance Pb-free glass powder that softening point is 370 DEG C；
Step 3: heating stirring is uniform at 70~110 DEG C after 82 parts of compounding silver powder and 12 parts of organic carriers are mixed, so
Silver powder slurry is obtained after disperseing by grinder, after 9 parts of high-performance Pb-free glass powders and 8 parts of organic carriers are mixed 70~
Heating stirring is uniform at 110 DEG C, then obtains glass paste after ground machine dispersion；
Step 4: it is 2.5 μm that silver powder slurry and the further mixed grinding of glass paste, which are uniformly obtained granularity, viscosity is
268Pas, the environment-friendlyconductive conductive silver paste material III that thixotropic index is 5.5.
4 comparative example of embodiment
Equipment and operation are with embodiment 3, the difference is that the ball shape silver powder that average grain diameter is 6.0 μm is substituted into compounding silver powder,
Other raw materials and its dosage are constant, obtained conductive silver paste IV.
5 comparative example of embodiment
Equipment and operation are with embodiment 3, the difference is that by PbO-B2O3-SiO2(wherein, PbO 70wt%) replaces high-performance
Lead-free glass powder, other raw materials and its dosage are constant, obtained conductive silver paste V.
6 comparative example of embodiment
Equipment and operation are with embodiment 3, the difference is that the ingredient of organic carrier is 65% terpinol, 25% ethyl cellulose
With 10% wetting dispersing agent, other raw materials and its dosage are constant, obtained conductive silver paste VI.
Conductive silver paste is prepared to each embodiment to be tested as follows：
(1) the size and shape test of printing, drying and sintered silver electrode grid line：
Conductive silver paste I-VI made from each embodiment is coordinated to impractical legal person's line width of thin grid by screen process press
In the polysilicon chip front of 156 × 156mm, (silicon chip used is to be had been subjected to a batch of to 290 mesh screen printings of 60 microns of degree
Cleaning, making herbs into wool, diffusion, PE steps, and printed back electrode and Al-BSF), after measuring printing using 3D light microscopes
The height and width of grid line, and see whether there is situations such as empty print and broken string, it is then dried by continuous tunnel furnace, 160 DEG C of furnace temperature, it is dry
3min reuses 3D light microscopes and measures the grid line height and width after drying, be finally printed on the silicon chip of gate electrode line 2 points 12 seconds
It is inside at the uniform velocity sintered since 300 DEG C by tunnel sintering furnace, is sintered 870 DEG C of final temperature, solar battery sheet I-VI is made,
It reuses 3D light microscopes and measures sintered grid line height and width, test result is as shown in table 1.
1 each conductive silver paste I-VI pattern test Comparative results of table
(2) electricity conversion is tested：
Using solar battery sheet special test equipment (NELC-140A), under standard test condition (STC), test is each
Electricity conversion, short circuit current and the series electrical of solar battery sheet I-VI made by conductive silver paste made from embodiment
Resistance；Standard test condition is：Light intensity：1000W/m2；Spectrum：AM1.5；Temperature：25 DEG C, test result is as shown in table 2.
2 each solar cell I-V I photoelectric properties test results of table compare
| Group | Short circuit current Isc (A) | Series resistance Rs (Ω) | Photoelectric conversion rate (%) |
| Solar cell I | 5.716 | 0.0059 | 18.06 |
| Solar cell II | 5.701 | 0.0061 | 17.92 |
| Solar cell III | 5.725 | 0.0052 | 18.13 |
| Solar cell IV | 5.718 | 0.0059 | 18.05 |
| Solar cell V | 5.689 | 0.0064 | 17.81 |
| Solar cell VI | 5.672 | 0.0069 | 17.79 |
It can be seen that from the experimental result in above-mentioned table using solar cell front side silver paste material of the present invention in printing, baking
The case where doing with during sintering process, can keep preferable depth-width ratio and grid line pattern, without empty print and breaking is printed suitable
Answering property is good, and obtained solar battery sheet short circuit current is larger, electricity conversion is high.
Finally it is to be appreciated that foregoing description is merely a preferred embodiment of the present invention, those skilled in the art is in the present invention
Enlightenment under, without prejudice to the purpose of the present invention and the claims, can make and indicate as multiple types, such change
It changes and each falls within protection scope of the present invention.
Claims (10)
1. a kind of environment-friendlyconductive conductive silver paste material, it is characterised in that be made of the raw material of following mass fraction：75-85 parts of silver powder is compounded,
8-15 parts of high-performance Pb-free glass powder, 15-25 parts of organic carrier；
The wherein described compounding silver powder is to contain the micro-silver powder that mass fraction is 4-9% superfine silver oxides.
2. environment-friendlyconductive conductive silver paste material according to claim 1, it is characterised in that the mass fraction of the raw material is：Compounding silver
82 parts of powder, 9 parts of high-performance Pb-free glass powder, 20 parts of organic carrier, wherein it is 5% to surpass that the compounding silver powder, which is containing mass fraction,
The micro-silver powder of thin silver oxide.
3. environment-friendlyconductive conductive silver paste material according to claim 1 or 2, it is characterised in that the compounding silver powder uses following methods
It is made：Ammonium hydroxide is added dropwise in the silver nitrate solution that mass concentration is 0.5mol/L, the molar ratio of ammonium hydroxide and silver nitrate is (1-
4)：1, it is uniformly mixed and obtains mixed solution A, be 1 by mass ratio：The oleic acid of (1-1.2) is the anti-of 1.5mol/L with mass concentration
Bad hematic acid solution is uniformly mixed and obtains mixed solution B, is then added dropwise to solution A and solution B in reactor simultaneously, solution A with
The mass ratio of solution B is (18-40)：1, reaction temperature is 15-45 DEG C, reaction time 2-5h, after the completion of reaction, by reactant
Filter residue is obtained by filtration, filter residue is washed with deionized water and absolute ethyl alcohol successively, washed product dry 4h under 50 DEG C of vacuum is obtained
Grain size to the micro-silver powder, the micro-silver powder is 0.8-2.5 μm, tap density 3.8-5.5g/cm3, then will surpass
Thin silver oxide and micro-silver powder, which are uniformly mixed, obtains the compounding silver powder.
4. environment-friendlyconductive conductive silver paste material according to claim 3, it is characterised in that the high-performance Pb-free glass powder is eutectic
Point glass powder, softening point are 370 DEG C~480 DEG C.
5. according to claim 1,2 or 4 any one of them environment-friendlyconductive conductive silver paste material, it is characterised in that the high-performance Pb-free glass
The inorganic constituents and corrresponding quality percentage of glass powder be：Bi2O360-80%, SiO210-20%, TiO24-8%, ZrO5 6-
12%.
6. environment-friendlyconductive conductive silver paste material according to claim 5, it is characterised in that the organic carrier presses following quality percentage
Than composition：Organic solvent 70-80%, urea-base grease 13-16%, polyvinyl acetate 6-9%, castor oil 1-5%.
7. environment-friendlyconductive conductive silver paste material according to claim 6, it is characterised in that：The organic solvent is terpinol, lemon
The mixed solvent of sour tributyl and butyl carbitol acetate, terpinol, tributyl citrate and butyl carbitol acetate
Mass ratio is (8-5)：(4-2)：1.
8. environment-friendlyconductive conductive silver paste material according to claim 5 or 6, it is characterised in that the organic carrier uses following methods
It is made：Organic solvent is heated to 50-80 DEG C, urea-base grease is added, stir and is warming up to 250-290 DEG C, addition polyethylene
Acetate stirs and is warming up to 150-200 DEG C, castor oil is then added, and continues to stir 5-15min, is cooled to room temperature to obtain institute
State organic carrier.
9. a kind of preparation method of the environment-friendlyconductive conductive silver paste material described in claim 1-8, it is characterised in that include the following steps：
Step 1: preparing compounding silver powder and organic carrier respectively；
Step 2: by Bi2O3、SiO2、TiO2、ZrO5After mixing well, in 1100-1250 DEG C of 30~50min of melting, by melting
Glass is poured into quenching-in water, and quenched glass blocks is passed through secondary grinding, obtains the high-performance Pb-free that grain size is 1 μm~4 μm
Glass powder；
Step 3: heating stirring is uniform at 70~110 DEG C after the organic carrier for compounding silver powder and 3/5 is mixed, then through grinding
Silver powder slurry is obtained after grinding machine dispersion, is added at 70~110 DEG C after the organic carrier of high-performance Pb-free glass powder and 2/5 is mixed
Thermal agitation is uniform, then obtains glass paste after ground machine dispersion；
Step 4: silver powder slurry and the further mixed grinding of glass paste are uniformly obtained into the environment-friendlyconductive conductive silver paste material, it is described
The granularity of environment-friendlyconductive conductive silver paste material is 2.0-8.0 μm, viscosity 250-290Pas, and thixotropic index is 5.0~7.0.
10. a kind of crystal silicon solar batteries, the solar cell includes silicon chip and the silver electrode grid line on silicon chip, spy
Sign is：The silver electrode grid line passes through silk-screen printing such as claim 1-8 any one of them environmental protection conductive silver on silicon chip
Then slurry obtains after drying, sintering.
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| CN112750552A (en) * | 2020-12-25 | 2021-05-04 | 邯郸学院 | Sintered silver paste and preparation method thereof |
| CN114446510A (en) * | 2022-02-23 | 2022-05-06 | 东莞市山盟科技有限公司 | Environment-friendly compound modified conductive silver paste and preparation method thereof |
| CN114464338A (en) * | 2021-11-29 | 2022-05-10 | 无锡帝科电子材料股份有限公司 | Solar cell front conductive silver paste and preparation method thereof |
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Application publication date: 20181113 |