CN115579171A - Easily-welded solar cell low-temperature silver paste and preparation method thereof - Google Patents
Easily-welded solar cell low-temperature silver paste and preparation method thereof Download PDFInfo
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- CN115579171A CN115579171A CN202211289558.7A CN202211289558A CN115579171A CN 115579171 A CN115579171 A CN 115579171A CN 202211289558 A CN202211289558 A CN 202211289558A CN 115579171 A CN115579171 A CN 115579171A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 47
- 239000004332 silver Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 44
- 239000011347 resin Substances 0.000 claims abstract description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920000223 polyglycerol Polymers 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 46
- 238000001914 filtration Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 16
- 238000009826 distribution Methods 0.000 claims description 14
- 238000001723 curing Methods 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 239000003822 epoxy resin Substances 0.000 claims description 9
- 229920000647 polyepoxide Polymers 0.000 claims description 9
- 238000005476 soldering Methods 0.000 claims description 9
- QYMFNZIUDRQRSA-UHFFFAOYSA-N dimethyl butanedioate;dimethyl hexanedioate;dimethyl pentanedioate Chemical compound COC(=O)CCC(=O)OC.COC(=O)CCCC(=O)OC.COC(=O)CCCCC(=O)OC QYMFNZIUDRQRSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229910000679 solder Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 4
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 4
- 239000012948 isocyanate Substances 0.000 claims description 4
- 150000002513 isocyanates Chemical class 0.000 claims description 4
- 229920001225 polyester resin Polymers 0.000 claims description 4
- 239000004645 polyester resin Substances 0.000 claims description 4
- 229920005749 polyurethane resin Polymers 0.000 claims description 4
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- UDSFAEKRVUSQDD-UHFFFAOYSA-N Dimethyl adipate Chemical compound COC(=O)CCCCC(=O)OC UDSFAEKRVUSQDD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004842 bisphenol F epoxy resin Substances 0.000 claims description 3
- -1 polypropylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 claims 1
- 229920001451 polypropylene glycol Polymers 0.000 claims 1
- 238000003466 welding Methods 0.000 abstract description 23
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 125000003700 epoxy group Chemical group 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910021417 amorphous silicon Inorganic materials 0.000 description 3
- 229910021419 crystalline silicon Inorganic materials 0.000 description 3
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000013035 low temperature curing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000011807 nanoball Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000010409 thin film 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
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
-
- 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
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Conductive Materials (AREA)
Abstract
The invention relates to an easily-welded solar cell low-temperature silver paste and a preparation method thereof. The easily-welded solar cell low-temperature silver paste comprises the following components: 85-92% of silver powder, 3-8% of resin, 3-8% of organic solvent, 0.2-1.5% of curing agent, 0.2-1% of dispersing agent and 0.5-2% of adhesion promoter; the dendritic silver powder and the nano spherical silver powder added in the invention are modified by polyglycerol, the mixed solution of polyglycerol and ethanol is added into the silver powder, and the polyglycerol is used as a silver powder surface coating agent to form coating, so that the silver powder is effectively prevented from agglomerating and the bonding strength is improved, the silver powder is more easily dispersed and uniformly distributed, the wettability of the silver powder is improved, meanwhile, surface hydroxyl groups formed on the surface of the silver powder and epoxy groups in an organic carrier participate in a curing reaction to form a better curing effect, the welding tension of the slurry is effectively improved, and the welding tension can reach more than 1.2N and is far higher than that of common low-temperature silver slurry.
Description
Technical Field
The invention belongs to the technical field of preparation of solar cell silver paste, and particularly relates to easy-to-weld solar cell low-temperature silver paste and a preparation method thereof.
Background
HIT (silicon heterojunction solar cell) was first successfully developed by the japan sanyo corporation, and since then the research on heterojunction solar cells by various research institutes in the world has been significantly increased. The HIT cell is formed by amorphous silicon and crystalline silicon materials, is an amorphous silicon film deposited on crystalline silicon, integrates the advantages of the crystalline silicon cell and a film cell, and is one of the important development directions of a high-conversion-efficiency silicon-based solar cell. The HIT cell integrates the ultra-low temperature production and manufacturing advantages of the thin-film solar cell, the traditional high-temperature process is avoided, the temperature requirement is only 200 ℃, power can be generated on two sides, and the core competitiveness of power generation is obvious.
The silver paste has the function of collecting the current generated by the solar cell, and the current is led out through the welding strip and finally enters a power grid or a use end. The traditional silver paste crystal silicon battery adopts high-temperature sintering, and silver powder and glass powder are melted and etch a silicon plate to form reliable adhesion and ohmic contact with a silicon wafer. For the HIT cell, the high temperature can damage hydrogenated amorphous silicon in the HIT cell, so that the conversion efficiency of the cell is reduced, and therefore, the low-temperature curing solar cell silver paste is required. Different from good welding tension of high-temperature silver paste melting and etching silicon plates, low-temperature silver paste is bonded with silicon wafers through organic resin, the tension is often smaller than 1N, and a welding strip falls off, so that the HIT low-temperature curing solar cell silver paste with high welding tension needs to be researched and developed.
Disclosure of Invention
In order to solve the problem that the welding tension of the conventional low-temperature silver paste for the HIT battery is smaller, the invention aims to provide the low-temperature conductive silver paste for the solar battery easy to weld and the preparation method thereof, and the service life of an HIT battery component can be effectively prolonged.
In order to achieve the purpose, the invention adopts the technical scheme that: the low-temperature silver paste for the easily-welded solar cell comprises the following components:
85 to 92 percent of silver powder,
3 to 8 percent of resin,
3 to 8 percent of organic solvent,
0.2 to 1.5 percent of curing agent,
0.2 to 1 percent of dispersant,
0.5 to 2 percent of adhesion promoter;
the silver powder is a mixture consisting of modified dendritic silver powder and modified nano spherical silver powder, wherein the mass ratio of the modified dendritic silver powder to the modified nano spherical silver powder is (2-16): 1;
the modified dendritic silver powder is polyglycerol-modified dendritic silver powder, and the modified nano spherical silver powder is polyglycerol-modified nano spherical silver powder. Further, the particle size distribution D50 of the modified dendritic silver powder is 2.0-5.0 μm, and the tap density is 4-7g/mL.
Further, the particle size distribution D50 of the modified nano spherical silver powder is 100-500nm, and the tap density is 3-8g/mL.
Further, the resin comprises a main resin and an auxiliary resin, wherein the main resin comprises one or more of bisphenol A epoxy resin, bisphenol F epoxy resin and acrylic modified epoxy resin, and the auxiliary resin comprises one or more of polyester resin, polyurethane resin and acrylic resin.
Further, the organic solvent comprises one or more of dibasic ester (DBE), diethylene glycol butyl ether acetate and dimethyl adipate.
Further, the curing agent comprises one or more of isocyanate, imidazole and modified amine.
Further, the dispersing agent comprises one or more of polyester and polyurethane, and the adhesion promoter comprises a silane coupling agent.
Further, the modified dendritic silver powder and the modified nano spherical silver powder are prepared by the following method: respectively adding the dendritic silver powder and the nano spherical silver powder into an excessive (2-5 times of the mass of the silver powder) mixed solution of polyglycerol and ethanol, and controlling the mass ratio of polyglycerol to ethanol to be 3: (1-9), setting the stirring speed to be 100-200r/min, stirring for 3-7h, filtering and drying to respectively obtain the modified dendritic silver powder and the modified nano spherical silver powder.
The invention also provides a preparation method of the easy-to-weld solar cell low-temperature silver paste, which comprises the following steps:
s1, adding the dendritic silver powder into a mixed solution of polypropylene triol and ethanol, stirring, filtering and drying to obtain modified dendritic silver powder; adding the nano spherical silver powder into a mixed solution of polypropylene triol and ethanol, stirring, filtering and drying to obtain modified nano spherical silver powder;
s2, mixing the resin, the organic solvent, the dispersant and the adhesion promoter, and dispersing in a centrifugal dispersing machine to obtain a mixed carrier A;
s3, mixing the mixed carrier A with a curing agent, and stirring at a low speed to obtain a mixed carrier B;
s4, adding the modified dendritic silver powder and the nano silver powder into the mixed carrier B in batches, and stirring while adding at the stirring speed of 100-200r/min to obtain primarily dispersed slurry;
and S5, rolling the primarily dispersed slurry for multiple times to obtain the low-temperature silver paste for the easily-welded solar cell.
Further, the step S2 specifically includes the following operations: adding main resin in the resin into a solvent, stirring at constant temperature of 300-500r/min in a water bath kettle at 60-80 ℃, and filtering impurities to obtain a low-viscosity resin carrier after the main resin is completely dissolved; mixing a low-viscosity resin carrier, the residual auxiliary resin in the resin, an organic solvent, a dispersant and an adhesion promoter, and putting the mixture into a centrifugal dispersion machine for dispersion at the rotating speed of 800-1000r/min for 1-3min to obtain a mixed carrier A;
in the steps S4 and S5, the temperature is controlled to be less than 20 ℃ during stirring.
Compared with the prior art, the invention has the following beneficial effects:
(1) The dendritic silver powder and the nano spherical silver powder added in the invention are modified by polyglycerol, the mixed solution of polyglycerol and ethanol is added into the silver powder, and the polyglycerol is used as a silver powder surface coating agent to form coating, so that the silver powder is effectively prevented from agglomerating and the bonding strength is improved, the silver powder is more easily dispersed and uniformly distributed, the wettability of the silver powder is improved, meanwhile, surface hydroxyl groups formed on the surface of the silver powder and epoxy groups in an organic carrier participate in a curing reaction, a better curing effect is formed, and the welding tension of the slurry is effectively improved.
(2) The dendritic silver powder is matched with the nano-ball powder, so that the silver powder in the slurry can be better lapped, the silver powder is melted in the drying process of the slurry, and the nano-ball powder is connected with the dendritic silver powder and the ITO film, so that the slurry has stronger welding tension after being dried.
The invention improves the tension of the low-temperature silver paste from the two aspects, so that the welding tension can reach more than 1.2N and is far higher than that of the common low-temperature silver paste.
Detailed Description
Further features and advantages of the present invention will be understood from the following detailed description. The examples provided are merely illustrative of the method of the present invention and do not limit the remainder of the disclosure in any way.
The mass percentages of the components in the following examples are shown in table 1.
Table 1 mass percentages of components in low temperature silver pastes of examples 1-4 and comparative example 1
Example 1
The invention discloses a preparation method of low-temperature silver paste for an easily-welded solar cell, which comprises the following steps of:
s1, preparing modified dendritic silver powder and modified nano spherical silver powder. Respectively adding excessive polyglycerol and ethanol mixed solution into the two silver powders, wherein the mass ratio of polyglycerol to ethanol is equal to 1:1, setting the stirring speed to be 100r/min, stirring for 5h, filtering and drying to obtain the modified dendritic silver powder and the modified nano spherical silver powder. The particle size distribution D50 of the modified dendritic silver powder is 2.3 mu m, the tap density is 4.1g/mL, the particle size distribution D50 of the modified nano spherical silver powder is 486nm, and the tap density is 7.5g/mL.
S2, preparing a high molecular resin carrier. And adding bisphenol A epoxy resin into DBE, stirring at a constant temperature of 500r/min in a water bath kettle at 60 ℃ until the epoxy resin is completely dissolved, and filtering impurities by using a 400-mesh gauze to obtain the low-viscosity resin carrier.
And S3, mixing the low-viscosity resin carrier, the polyester resin, the diethylene glycol monobutyl ether and the silane coupling agent, and putting the mixture into a centrifugal dispersion machine for dispersion at the rotating speed of 1000r/min for 1min to obtain a mixed carrier A.
And S4, mixing the mixed carrier A with an isocyanate curing agent, stirring at a low speed of 200r/min, and controlling the temperature to be lower than 20 ℃ to obtain a mixed carrier B.
S5, adding the modified dendritic silver powder and the nano spherical silver powder into the mixed carrier B in 5 batches, wherein the mass ratio of the modified dendritic silver powder to the modified nano spherical silver powder is 2:1, stirring while adding, wherein the stirring speed is 200r/min, and the temperature is controlled to be less than 20 ℃ to obtain the primarily dispersed slurry.
And S6, putting the primarily dispersed slurry into a three-roll mill to roll for 6 times to obtain conductive silver paste slurry with the fineness of less than 8 mu m and the viscosity of 60-100 pas.
Example 2
The invention discloses a preparation method of easy-to-weld solar cell low-temperature silver paste, which comprises the following steps of:
s1, preparing modified dendritic silver powder and modified nano spherical silver powder. Respectively adding excessive polyglycerol and ethanol mixed solution into the two silver powders, wherein the mass ratio of polyglycerol to ethanol is equal to 1: and 3, setting the stirring speed to be 200r/min, stirring for 3h, filtering and drying to obtain the modified dendritic silver powder and the modified nano spherical silver powder. The particle size distribution D50 of the modified dendritic silver powder is 3.5 mu m, the tap density is 5.0g/mL, the particle size distribution D50 of the modified nano spherical silver powder is 327nm, and the tap density is 4.4g/mL.
S2, preparing a high polymer resin carrier. Adding the acrylic acid modified epoxy resin into DBE, stirring at constant temperature of 300r/min in a 70 ℃ water bath kettle until the epoxy resin is completely dissolved, and filtering impurities by using a 400-mesh gauze to obtain the low-viscosity resin carrier.
And S3, mixing the low-viscosity resin carrier, the polyurethane resin, the diethylene glycol monobutyl ether and the silane coupling agent, and putting the mixture into a centrifugal dispersion machine for dispersion at the rotating speed of 1000r/min for 1min to obtain a mixed carrier A.
And S4, mixing the mixed carrier A with the modified amine latent curing agent T31, stirring at a low speed of 200r/min, and controlling the temperature to be less than 20 ℃ to obtain a mixed carrier B.
S5, adding the modified dendritic silver powder and the nano spherical silver powder into the mixed carrier B in 5 batches, wherein the mass ratio of the modified dendritic silver powder to the modified nano spherical silver powder is 11:1, stirring while adding, wherein the stirring speed is 200r/min, and the temperature is controlled to be less than 20 ℃ to obtain the primarily dispersed slurry.
And S6, putting the primarily dispersed slurry into a three-roll mill to roll for 6 times to obtain conductive silver slurry with the fineness of less than 8 mu m and the viscosity of 60-100 Pa.s.
Example 3
The invention discloses a preparation method of low-temperature silver paste for an easily-welded solar cell, which comprises the following steps of:
s1, preparing modified dendritic silver powder and modified nano spherical silver powder. Respectively adding excessive polyglycerol and ethanol mixed solution into the two silver powders, wherein the mass ratio of polyglycerol to ethanol is equal to 1: and 2, setting the stirring speed to be 200r/min, stirring for 3h, filtering and drying to obtain the modified dendritic silver powder and the modified nano spherical silver powder. The particle size distribution D50 of the modified dendritic silver powder is 4.6 mu m, the tap density is 6.7g/mL, the particle size distribution D50 of the modified nano spherical silver powder is 230nm, and the tap density is 3.2g/mL.
S2, preparing a high molecular resin carrier. Adding acrylic acid modified epoxy resin into DBE, stirring at constant temperature of 70 ℃ in a water bath kettle at the stirring speed of 300r/min until the epoxy resin is completely dissolved, and filtering impurities by using a 400-mesh gauze to obtain the low-viscosity resin carrier.
And S3, mixing the low-viscosity resin carrier, the polyurethane resin, the dimethyl adipate and the silane coupling agent, and putting the mixture into a centrifugal dispersion machine for dispersion at the rotating speed of 1000r/min for 1min to obtain a mixed carrier A.
And S4, mixing the mixed carrier A with the modified amine latent curing agent T31, stirring at a low speed of 200r/min, and controlling the temperature to be less than 20 ℃ to obtain a mixed carrier B.
S5, adding the modified dendritic silver powder and the nano spherical silver powder into the mixed carrier B in 5 batches, wherein the mass ratio of the modified dendritic silver powder to the modified nano spherical silver powder is 16:1, stirring while adding, wherein the stirring speed is 200r/min, and the temperature is controlled to be less than 20 ℃ to obtain the primarily dispersed slurry.
And S6, putting the primarily dispersed slurry into a three-roll mill to roll for 6 times to obtain conductive silver slurry with the fineness of less than 8 mu m and the viscosity of 60-100 Pa.s.
Example 4
The invention discloses a preparation method of easy-to-weld solar cell low-temperature silver paste, which comprises the following steps of:
s1, preparing modified dendritic silver powder and modified nano spherical silver powder. Respectively adding excessive polyglycerol and ethanol mixed solution into the two silver powders, wherein the mass ratio of polyglycerol to ethanol is 3: and 1, setting the stirring speed to be 200r/min, stirring for 6 hours, filtering and drying to obtain the modified dendritic silver powder and the modified nano spherical silver powder. The particle size distribution D50 of the modified dendritic silver powder is 2.9 mu m, the tap density is 5.3g/mL, the particle size distribution D50 of the modified nano spherical silver powder is 436nm, and the tap density is 5.8g/mL.
S2, preparing a high molecular resin carrier. And adding bisphenol F epoxy resin into DBE, stirring at a constant temperature of 400r/min in a water bath kettle at the temperature of 80 ℃ until the epoxy resin is completely dissolved, and filtering impurities by using a 400-mesh gauze to obtain the low-viscosity resin carrier.
And S3, mixing the low-viscosity resin carrier, acrylic resin, diethylene glycol butyl ether acetate and a silane coupling agent, and dispersing in a centrifugal dispersion machine at the rotating speed of 900r/min for 2min to obtain a mixed carrier A.
And S4, mixing the mixed carrier A with a 2-ethyl-4-methylimidazole curing agent, stirring at a low speed of 100r/min, and controlling the temperature to be lower than 20 ℃ to obtain a mixed carrier B.
S5, adding the modified dendritic silver powder and the nano spherical silver powder into the mixed carrier B in 5 batches, wherein the mass ratio of the modified dendritic silver powder to the modified nano spherical silver powder is 6:1, stirring while adding, wherein the stirring speed is 100r/min, and the temperature is controlled to be less than 20 ℃ to obtain the primarily dispersed slurry.
And S6, putting the primarily dispersed slurry into a three-roll mill to roll for 6 times to obtain conductive silver slurry with the fineness of less than 8 mu m and the viscosity of 60-100 Pa.s.
Comparative example 1
A preparation method of low-temperature silver paste for a solar cell comprises the following steps:
preparing a high molecular resin carrier. And (2) adding bisphenol A epoxy resin into DBE, stirring at a constant temperature of 500r/min in a water bath kettle at the temperature of 60 ℃ until the epoxy resin is completely dissolved, and filtering impurities by using a 400-mesh gauze to obtain the low-viscosity resin carrier.
Mixing a low-viscosity resin carrier, polyester resin, diethylene glycol monobutyl ether and a silane coupling agent, and putting the mixture into a centrifugal dispersion machine for dispersion at the rotating speed of 1000r/min for 1min to obtain a mixed carrier A.
And (3) mixing the mixed carrier A with an isocyanate curing agent, stirring at a low speed of 200r/min, and controlling the temperature to be lower than 20 ℃ to obtain a mixed carrier B.
Adding dendritic silver powder (without modification treatment) and nano spherical silver powder (without modification treatment) into the mixed carrier B in 5 batches, wherein the mass ratio of the dendritic silver powder to the nano spherical silver powder is 2:1, stirring while adding, wherein the stirring speed is 200r/min, and the temperature is controlled to be less than 20 ℃ to obtain the primarily dispersed slurry. The grain diameter distribution D50 of the dendritic silver powder is 2.3 mu m, the tap density is 4.1g/mL, the grain diameter distribution D50 of the nano spherical silver powder is 481nm, and the tap density is 7.4g/mL.
And (3) putting the primarily dispersed slurry into a three-roll mill to roll for 6 times to obtain conductive silver paste with the fineness of less than 8 mu m and the viscosity of 60-100 Pa.s.
The welding tension performance tests of the above examples 1 to 4 and comparative example 1 were carried out by the following methods:
soaking the solder strip in the soldering flux for 1min, and setting the temperature of a soldering iron to 240 ℃;
silver paste is used for printing line patterns on the surface of an ITO silicon chip by screen printing;
taking out the welding strip, and overlapping and aligning the welding strip and the line;
dipping a small amount of soldering tin by using a soldering iron, and pushing along the soldering strip to weld the soldering strip on the silver paste;
bending the redundant welding strips, fixing the welding strips on a handheld tensile machine, enabling the welding strips to be pulled at a constant speed after the data of the instrument is reset to zero, and reading the test peak data after each pulling;
the maximum value and the minimum value of a series of data are removed, the rest data are averaged to obtain welding tension test data, and the welding tension performance test results of the low-temperature silver pastes prepared in examples 1 to 4 and comparative example 1 are shown in table 2.
TABLE 2
From the test data in table 2, it can be seen that the silver paste prepared in examples 1 to 4 of the present invention has a higher welding tension by modifying the silver powder with polyglycerol, and the average welding tension is 1.4N; in the comparative example 1, the silver paste prepared from the silver powder which is not modified by the polyglycerol has the welding tension less than 1N, so that the welding strip is easy to fall off; compared with the prior art, the preparation method of the silver paste provided by the invention can effectively improve the welding tension, and when the silver paste is used in the HIT battery, the quality and the service life of the battery can be greatly improved.
Claims (10)
1. The low-temperature silver paste for the easily-welded solar cell is characterized by comprising the following components:
85 to 92 percent of silver powder,
3 to 8 percent of resin,
3 to 8 percent of organic solvent,
0.2 to 1.5 percent of curing agent,
0.2 to 1 percent of dispersant,
0.5 to 2 percent of adhesion promoter;
the silver powder is a mixture of modified dendritic silver powder and modified nano spherical silver powder, wherein the mass ratio of the modified dendritic silver powder to the modified nano spherical silver powder is (2-16): 1;
the modified dendritic silver powder is polyglycerol modified dendritic silver powder, and the modified nano spherical silver powder is polyglycerol modified nano spherical silver powder.
2. The easy-to-solder solar cell low-temperature silver paste of claim 1, wherein the modified dendritic silver powder has a particle size distribution D50 of 2.0-5.0 μm and a tap density of 4-7g/mL.
3. The easy-to-solder solar cell low-temperature silver paste of claim 1, wherein the modified nano spherical silver powder has a particle size distribution D50 of 200-500nm and a tap density of 3-8g/mL.
4. The easy-to-solder solar cell low temperature silver paste of claim 1, wherein the resin comprises a main resin and an auxiliary resin, the main resin comprises one or more of bisphenol A epoxy resin, bisphenol F epoxy resin and acrylic modified epoxy resin, and the auxiliary resin comprises one or more of polyester resin, polyurethane resin and acrylic resin.
5. The easy solder solar cell low temperature silver paste of claim 1, wherein the organic solvent comprises one or more of dibasic ester, diethylene glycol ethyl ether acetate, diethylene glycol butyl ether acetate, and dimethyl adipate.
6. The easy-to-solder solar cell low temperature silver paste of claim 1, wherein the curing agent comprises one or more of isocyanate, imidazole, modified amine.
7. The easy-to-solder solar cell low temperature silver paste of claim 1, wherein the dispersant comprises one or more of polyester and polyurethane, and the adhesion promoter comprises a silane coupling agent.
8. The easy-soldering solar cell low-temperature silver paste according to claim 1, wherein the modified dendritic silver powder and the modified nano spherical silver powder are prepared by the following method: respectively adding the dendritic silver powder and the nano spherical silver powder into a mixed solution of excessive polyglycerol and ethanol, and controlling the mass ratio of polyglycerol to ethanol to be 3: (1-9), setting the stirring speed to be 100-200r/min, stirring for 3-7h, filtering and drying to obtain the modified dendritic silver powder and the modified nano spherical silver powder.
9. The method for preparing the easy-soldering solar cell low-temperature silver paste as claimed in any one of claims 1 to 8, wherein the method comprises the following steps:
s1, adding the dendritic silver powder into a mixed solution of polypropylene triol and ethanol, stirring, filtering and drying to obtain modified dendritic silver powder; adding the nano spherical silver powder into a mixed solution of polypropylene glycol and ethanol, stirring, filtering and drying to obtain modified nano spherical silver powder;
s2, mixing the resin, the organic solvent, the dispersant and the adhesion promoter, and dispersing in a centrifugal dispersing machine to obtain a mixed carrier A;
s3, mixing the mixed carrier A with a curing agent, and stirring at a low speed to obtain a mixed carrier B;
s4, adding the modified dendritic silver powder and the modified nano spherical silver powder into the mixed carrier B in batches, and stirring while adding to obtain a primarily dispersed slurry;
and S5, rolling the primarily dispersed slurry for multiple times to obtain the low-temperature silver paste for the easily-welded solar cell.
10. The method for preparing the easy-soldering solar cell low-temperature silver paste according to claim 9, wherein the step S2 specifically comprises the following operations: adding main resin in the resin into a solvent, stirring at constant temperature of 300-500r/min in a water bath kettle at 60-80 ℃, and filtering impurities to obtain a low-viscosity resin carrier after the main resin is completely dissolved; mixing a low-viscosity resin carrier, the residual auxiliary resin in the resin, an organic solvent, a dispersant and an adhesion promoter, and putting the mixture into a centrifugal dispersion machine for dispersion at the rotating speed of 800-1000r/min for 1-3min to obtain a mixed carrier A;
in the steps S4 and S5, the temperature is controlled to be less than 20 ℃ during stirring.
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| JP2006049106A (en) * | 2004-08-05 | 2006-02-16 | Mitsui Mining & Smelting Co Ltd | Silver paste |
| CN110335724A (en) * | 2019-07-25 | 2019-10-15 | 西安宏星电子浆料科技股份有限公司 | A kind of preparation method suitable for hetero-junctions high performance solar batteries silver paste |
| CN111508637A (en) * | 2020-04-28 | 2020-08-07 | 无锡晶睿光电新材料有限公司 | Silver paste with high conductivity at 80 ℃ and preparation method thereof |
| CN113192689A (en) * | 2021-04-07 | 2021-07-30 | 湖南诺尔得材料科技有限公司 | Preparation method and application of silver powder dispersion |
| CN113345623A (en) * | 2021-06-09 | 2021-09-03 | 佛山市瑞纳新材科技有限公司 | HJT battery low-temperature curing silver paste for fine printing and preparation method thereof |
| CN114464371A (en) * | 2022-01-26 | 2022-05-10 | 西南科技大学 | Preparation method of low-temperature conductive silver paste containing nano silver powder for solar cell |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006049106A (en) * | 2004-08-05 | 2006-02-16 | Mitsui Mining & Smelting Co Ltd | Silver paste |
| CN110335724A (en) * | 2019-07-25 | 2019-10-15 | 西安宏星电子浆料科技股份有限公司 | A kind of preparation method suitable for hetero-junctions high performance solar batteries silver paste |
| CN111508637A (en) * | 2020-04-28 | 2020-08-07 | 无锡晶睿光电新材料有限公司 | Silver paste with high conductivity at 80 ℃ and preparation method thereof |
| CN113192689A (en) * | 2021-04-07 | 2021-07-30 | 湖南诺尔得材料科技有限公司 | Preparation method and application of silver powder dispersion |
| CN113345623A (en) * | 2021-06-09 | 2021-09-03 | 佛山市瑞纳新材科技有限公司 | HJT battery low-temperature curing silver paste for fine printing and preparation method thereof |
| CN114464371A (en) * | 2022-01-26 | 2022-05-10 | 西南科技大学 | Preparation method of low-temperature conductive silver paste containing nano silver powder for solar cell |
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