CN115798786B - High-adhesion back surface field aluminum conductive paste for crystalline silicon solar cell and preparation method thereof - Google Patents
High-adhesion back surface field aluminum conductive paste for crystalline silicon solar cell and preparation method thereof Download PDFInfo
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- CN115798786B CN115798786B CN202211685370.4A CN202211685370A CN115798786B CN 115798786 B CN115798786 B CN 115798786B CN 202211685370 A CN202211685370 A CN 202211685370A CN 115798786 B CN115798786 B CN 115798786B
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 229910021419 crystalline silicon Inorganic materials 0.000 title claims abstract description 34
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 60
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229920005989 resin Polymers 0.000 claims abstract description 39
- 239000011347 resin Substances 0.000 claims abstract description 39
- 229910052709 silver Inorganic materials 0.000 claims abstract description 31
- 239000004332 silver Substances 0.000 claims abstract description 31
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 14
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 14
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 14
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 14
- 239000011734 sodium Substances 0.000 claims abstract description 14
- NVKSMKFBUGBIGE-UHFFFAOYSA-N 2-(tetradecoxymethyl)oxirane Chemical compound CCCCCCCCCCCCCCOCC1CO1 NVKSMKFBUGBIGE-UHFFFAOYSA-N 0.000 claims abstract description 13
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 13
- 239000007822 coupling agent Substances 0.000 claims abstract description 13
- 150000001282 organosilanes Chemical class 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000011521 glass Substances 0.000 claims abstract description 10
- 150000002688 maleic acid derivatives Chemical class 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 60
- 238000002156 mixing Methods 0.000 claims description 49
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- -1 epoxy itaconic acid ester Chemical class 0.000 claims description 24
- 239000003822 epoxy resin Substances 0.000 claims description 24
- 229920000647 polyepoxide Polymers 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 24
- 239000002904 solvent Substances 0.000 claims description 24
- 239000000725 suspension Substances 0.000 claims description 24
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 18
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 18
- 238000001291 vacuum drying Methods 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 12
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 12
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 12
- 239000012295 chemical reaction liquid Substances 0.000 claims description 12
- 239000011231 conductive filler Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000008103 glucose Substances 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 12
- 239000003112 inhibitor Substances 0.000 claims description 12
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical group COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 12
- 238000006116 polymerization reaction Methods 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 12
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 6
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 239000012298 atmosphere Substances 0.000 abstract description 2
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002002 slurry Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Classifications
-
- 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
- Conductive Materials (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention discloses a high-adhesion back surface field aluminum conductive paste for a crystalline silicon solar cell and a preparation method thereof, and relates to the technical field of solar cell processing, wherein the conductive paste is prepared from the following components: aluminum powder, silver-coated aluminum powder, silver powder, tributyl phosphate, modified maleic acid resin, ethyl cellulose, tetradecyl glycidyl ether, N-acyl amino acid sodium, an organosilane coupling agent and glass powder; the high-adhesion back surface field aluminum conductive paste for preparing the crystalline silicon solar cell has excellent performance, can remarkably improve and improve the photoelectric conversion efficiency of the crystalline silicon solar cell, and can effectively play a role in oxidation protection on aluminum powder by introducing tributyl phosphate to generate a reducing atmosphere during combustion, so that the aluminum powder cannot be oxidized to form aluminum oxide, and the electrochemical performance of the aluminum powder is ensured.
Description
Technical Field
The invention belongs to the field of solar cell processing, and particularly relates to high-adhesion back surface field aluminum conductive paste for a crystalline silicon solar cell and a preparation method thereof.
Background
With the growing shortage of global energy, solar energy is widely valued in all countries of the world with the unique advantages of no pollution, large market space and the like. The crystalline silicon solar cell photovoltaic power generation has the advantages of safety, reliability, no noise, low failure rate and the like, and meanwhile, the excellent environmental protection performance, abundant resources and renewable performance are popular among countries in the world, so that the crystalline silicon solar cell photovoltaic power generation becomes an economic resuscitating engine and a low-carbon environment-friendly representation. The common crystalline silicon solar cell is composed of a back electrode, a back field, a P-type layer formed by semiconductor materials, an N-type layer, a P-N junction, an antireflection film, a front gate electrode and the like. When sunlight irradiates the surface of the solar cell, the antireflection film and the suede structure can effectively reduce light reflection loss on the surface of the cell. After absorbing solar energy, the semiconductor structure in the solar cell excites and generates electron and hole pairs, the electron and hole pairs are separated by a self-built electric field of a P-N junction in the semiconductor, the electrons flow into an N region, the holes flow into a P region, and if the positive electrode and the negative electrode of the crystalline silicon solar cell are connected with an external load, photo-generated current flows in an external circuit.
In the preparation of crystalline silicon solar cells, the front and back sides of the cells need to be metallized (Metallization). The metallization of the front (light-facing) surface of the cell is typically performed by screen printing a conductive metal paste onto the surface of the passivation film in a desired pattern, and then etching and penetrating the passivation film by high temperature sintering and thereby making electrical contact with the emitter electrode to form a conductive structure (or electrode) in the form of a conductive metal contact.
The invention belongs to the field of new materials of solar cells, and particularly relates to a crystalline silicon solar cell back surface field lead-free aluminum conductive paste and a preparation method thereof. The crystalline silicon solar cell back surface field lead-free aluminum conductive paste is mainly prepared by mixing the following raw materials in percentage by mass: 70-80% of aluminum powder, 1-10% of glass powder and 15-25% of organic binder. The aluminum conductive paste has the advantages of no lead or cadmium, no aluminum beads or aluminum bubbles after being sintered, good Back Surface Field (BSF) can be formed, and the aluminum conductive paste can bear the sintering temperature of 830 ℃, has more defects in the prior art, has poor conductive performance and limits the application of the aluminum conductive paste.
Accordingly, there is a need for further improvements in the art.
Disclosure of Invention
The invention aims to provide a high-adhesion back surface field aluminum conductive paste for a crystalline silicon solar cell, which solves the defects in the prior art.
The technical scheme adopted by the invention is as follows:
The high-adhesion back surface field aluminum conductive paste for the crystalline silicon solar cell is prepared from the following components in parts by weight: 20-25 parts of aluminum powder, 4-5 parts of silver coated aluminum powder, 3-5 parts of silver powder, 18-25 parts of tributyl phosphate, 12-16 parts of modified maleic acid resin, 6-8 parts of ethyl cellulose, 2-6 parts of tetradecyl glycidyl ether, 1-3 parts of N-acyl amino acid sodium, 1.3-1.5 parts of organosilane coupling agent and 30-40 parts of glass powder.
As a further technical scheme: the preparation method of the silver-coated aluminum powder comprises the following steps:
(1) Adding aluminum powder into a dispersing agent to prepare a solution;
(2) Adding hydrochloric acid into the solution, stirring and reacting for 10min, filtering, washing with water to neutrality, and drying to obtain activated aluminum powder;
(3) Mixing silver nitrate, glucose and water, and stirring for 40 min to obtain a reaction solution;
(4) Adding activated aluminum powder into deionized water, and uniformly stirring to obtain aluminum powder suspension;
(5) And adding the prepared reaction liquid into aluminum powder suspension, stirring at room temperature for reaction for 30 min, separating by adopting a centrifugal machine, filtering, washing with water to be neutral, and drying in a drying oven to obtain the silver-coated aluminum powder.
As a further technical scheme: the mixing mass ratio of the aluminum powder to the dispersing agent is 1:20;
the dispersing agent is ethanol solution;
the mass fraction of the ethanol solution is 10%.
As a further technical scheme: the concentration of the hydrochloric acid is 0.5 mol/L;
The mixing mass ratio of the hydrochloric acid to the solution is 1:10;
the mixing mass ratio of the silver nitrate to the glucose to the water is 3:1:15;
The mass fraction of the aluminum powder suspension is 12.5%;
The mixing mass ratio of the reaction liquid to the aluminum powder suspension is 1:3.
As a further technical scheme: the preparation method of the modified maleic acid resin comprises the following steps:
adding itaconic acid, epoxy resin and solvent into a reaction kettle according to a proportion, heating and stirring, heating the temperature to 75 ℃ at a heating rate of 5 ℃/s, then adding a catalyst and a polymerization inhibitor, continuously heating to 90 ℃, keeping the temperature and stirring for reaction for 1 hour, ending the reaction, and performing reduced pressure distillation to recover the solvent to obtain the epoxy itaconic acid ester;
Sequentially adding the obtained epoxy itaconic acid ester, maleic resin and rosin into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, heating to melt, stirring for 30min at a rotating speed of 500 r/min, naturally cooling to room temperature, performing vacuum drying treatment, and finally crushing and sieving to obtain the modified maleic resin.
As a further technical scheme: the epoxy resin adopts glycidol amine epoxy resin.
As a further technical scheme: the mixing mass ratio of the itaconic acid to the epoxy resin to the solvent is 8:3:15;
The solvent is isopropanol.
As a further technical scheme: the catalyst is dibenzoyl peroxide;
The polymerization inhibitor is 4-hydroxyanisole;
the mixing mass ratio of the itaconic acid to the dibenzoyl peroxide to the 4-hydroxyanisole is 12:1:2.
As a further technical scheme: the mixing mass ratio of the epoxy itaconic acid ester to the maleic resin to the rosin is 4:18:1;
The inert gas is nitrogen;
The vacuum drying temperature is 55 ℃;
the vacuum drying time was 4 hours.
The preparation method of the high-adhesion back surface field aluminum conductive paste of the crystalline silicon solar cell comprises the following steps:
(1) Sequentially adding aluminum powder, silver-coated aluminum powder and silver powder into a stirrer to uniformly stir to obtain a metal conductive filler;
(2) Sequentially adding tributyl phosphate, modified maleic resin, ethylcellulose, tetradecyl glycidyl ether, N-acyl amino acid sodium and an organosilane coupling agent into a stirrer, stirring uniformly, then adding a metal conductive filler, adjusting the temperature to 112 ℃, preserving heat, stirring for 30min, naturally cooling to room temperature to obtain the modified tributyl phosphate, and finally smelting in a muffle furnace at 1200 ℃ for 1 hour to obtain the modified tributyl phosphate.
According to the invention, the aluminum powder, the silver coated aluminum powder and the silver powder are mixed, so that the recombination rate of carriers can be reduced, the current and the open-circuit voltage of the battery are improved, the formation of a back surface field P+ layer is facilitated, and the photoelectric conversion efficiency of the battery is improved.
The softening point of the glass powder can be adjusted by introducing ethyl cellulose and N-acyl sodium amino acid, so that the slurry is easier to sinter into smooth coverage surface, and the warping degree of the silicon wafer after the conductive slurry is sintered is more suitable, and the application performance of the conductive slurry is improved. The modification treatment of the maleic resin can be beneficial to the formation of a back surface field layer, and the rheological property and thixotropic property of the slurry are improved, so that the adhesive force is greatly improved.
The beneficial effects are that:
The high-adhesion back surface field aluminum conductive paste for preparing the crystalline silicon solar cell has excellent performance, can remarkably improve and improve the photoelectric conversion efficiency of the crystalline silicon solar cell, and can effectively play a role in oxidation protection on aluminum powder by introducing tributyl phosphate to generate a reducing atmosphere during combustion, so that the aluminum powder cannot be oxidized to form aluminum oxide, and the electrochemical performance of the aluminum powder is ensured. Through carrying out the cooperation collocation with aluminium powder, silver cladding aluminium powder, silver powder, can make to have good ohmic contact between electrode and the silicon, and then improved the photoelectric conversion efficiency of crystalline silicon solar cell by a wide margin to with the introduction of silver cladding aluminium powder, can also improve the adhesion between rete to the base member.
Drawings
FIG. 1 is a graph comparing the effect of different parts by weight of silver-coated aluminum powder on photoelectric conversion efficiency;
fig. 2 is a graph comparing the effect of different amounts of aluminum powder added on photoelectric conversion efficiency.
Detailed Description
Example 1
The high-adhesion back surface field aluminum conductive paste for the crystalline silicon solar cell is prepared from the following components in parts by weight: 20 parts of aluminum powder, 4 parts of silver-coated aluminum powder, 3 parts of silver powder, 18 parts of tributyl phosphate, 12 parts of modified maleic resin, 6 parts of ethyl cellulose, 2 parts of tetradecyl glycidyl ether, 1 part of N-acyl amino acid sodium, 1.3 parts of organosilane coupling agent and 30 parts of glass powder.
The preparation method of the silver-coated aluminum powder comprises the following steps:
(1) Adding aluminum powder into a dispersing agent to prepare a solution;
(2) Adding hydrochloric acid into the solution, stirring and reacting for 10min, filtering, washing with water to neutrality, and drying to obtain activated aluminum powder;
(3) Mixing silver nitrate, glucose and water, and stirring for 40 min to obtain a reaction solution;
(4) Adding activated aluminum powder into deionized water, and uniformly stirring to obtain aluminum powder suspension;
(5) And adding the prepared reaction liquid into aluminum powder suspension, stirring at room temperature for reaction for 30 min, separating by adopting a centrifugal machine, filtering, washing with water to be neutral, and drying in a drying oven to obtain the silver-coated aluminum powder.
The mixing mass ratio of the aluminum powder to the dispersing agent is 1:20;
the dispersing agent is ethanol solution;
the mass fraction of the ethanol solution is 10%.
The concentration of the hydrochloric acid is 0.5 mol/L;
The mixing mass ratio of the hydrochloric acid to the solution is 1:10;
the mixing mass ratio of the silver nitrate to the glucose to the water is 3:1:15;
The mass fraction of the aluminum powder suspension is 12.5%;
The mixing mass ratio of the reaction liquid to the aluminum powder suspension is 1:3.
The preparation method of the modified maleic acid resin comprises the following steps:
adding itaconic acid, epoxy resin and solvent into a reaction kettle according to a proportion, heating and stirring, heating the temperature to 75 ℃ at a heating rate of 5 ℃/s, then adding a catalyst and a polymerization inhibitor, continuously heating to 90 ℃, keeping the temperature and stirring for reaction for 1 hour, ending the reaction, and performing reduced pressure distillation to recover the solvent to obtain the epoxy itaconic acid ester;
Sequentially adding the obtained epoxy itaconic acid ester, maleic resin and rosin into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, heating to melt, stirring for 30min at a rotating speed of 500 r/min, naturally cooling to room temperature, performing vacuum drying treatment, and finally crushing and sieving to obtain the modified maleic resin.
The epoxy resin adopts glycidol amine epoxy resin.
The mixing mass ratio of the itaconic acid to the epoxy resin to the solvent is 8:3:15;
The solvent is isopropanol.
The catalyst is dibenzoyl peroxide;
The polymerization inhibitor is 4-hydroxyanisole;
the mixing mass ratio of the itaconic acid to the dibenzoyl peroxide to the 4-hydroxyanisole is 12:1:2.
The mixing mass ratio of the epoxy itaconic acid ester to the maleic resin to the rosin is 4:18:1;
The inert gas is nitrogen;
The vacuum drying temperature is 55 ℃;
the vacuum drying time was 4 hours.
The preparation method of the high-adhesion back surface field aluminum conductive paste of the crystalline silicon solar cell comprises the following steps:
(1) Sequentially adding aluminum powder, silver-coated aluminum powder and silver powder into a stirrer to uniformly stir to obtain a metal conductive filler;
(2) Sequentially adding tributyl phosphate, modified maleic resin, ethylcellulose, tetradecyl glycidyl ether, N-acyl amino acid sodium and an organosilane coupling agent into a stirrer, stirring uniformly, then adding a metal conductive filler, adjusting the temperature to 112 ℃, preserving heat, stirring for 30min, naturally cooling to room temperature to obtain the modified tributyl phosphate, and finally smelting in a muffle furnace at 1200 ℃ for 1 hour to obtain the modified tributyl phosphate.
Example 2
The high-adhesion back surface field aluminum conductive paste for the crystalline silicon solar cell is prepared from the following components in parts by weight: 22 parts of aluminum powder, 4.5 parts of silver-coated aluminum powder, 4 parts of silver powder, 20 parts of tributyl phosphate, 15 parts of modified maleic resin, 7 parts of ethyl cellulose, 3 parts of tetradecyl glycidyl ether, 2 parts of N-acyl amino acid sodium, 1.4 parts of organosilane coupling agent and 35 parts of glass powder.
The preparation method of the silver-coated aluminum powder comprises the following steps:
(1) Adding aluminum powder into a dispersing agent to prepare a solution;
(2) Adding hydrochloric acid into the solution, stirring and reacting for 10min, filtering, washing with water to neutrality, and drying to obtain activated aluminum powder;
(3) Mixing silver nitrate, glucose and water, and stirring for 40 min to obtain a reaction solution;
(4) Adding activated aluminum powder into deionized water, and uniformly stirring to obtain aluminum powder suspension;
(5) And adding the prepared reaction liquid into aluminum powder suspension, stirring at room temperature for reaction for 30 min, separating by adopting a centrifugal machine, filtering, washing with water to be neutral, and drying in a drying oven to obtain the silver-coated aluminum powder.
The mixing mass ratio of the aluminum powder to the dispersing agent is 1:20;
the dispersing agent is ethanol solution;
the mass fraction of the ethanol solution is 10%.
The concentration of the hydrochloric acid is 0.5 mol/L;
The mixing mass ratio of the hydrochloric acid to the solution is 1:10;
the mixing mass ratio of the silver nitrate to the glucose to the water is 3:1:15;
The mass fraction of the aluminum powder suspension is 12.5%;
The mixing mass ratio of the reaction liquid to the aluminum powder suspension is 1:3.
The preparation method of the modified maleic acid resin comprises the following steps:
adding itaconic acid, epoxy resin and solvent into a reaction kettle according to a proportion, heating and stirring, heating the temperature to 75 ℃ at a heating rate of 5 ℃/s, then adding a catalyst and a polymerization inhibitor, continuously heating to 90 ℃, keeping the temperature and stirring for reaction for 1 hour, ending the reaction, and performing reduced pressure distillation to recover the solvent to obtain the epoxy itaconic acid ester;
Sequentially adding the obtained epoxy itaconic acid ester, maleic resin and rosin into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, heating to melt, stirring for 30min at a rotating speed of 500 r/min, naturally cooling to room temperature, performing vacuum drying treatment, and finally crushing and sieving to obtain the modified maleic resin.
The epoxy resin adopts glycidol amine epoxy resin.
The mixing mass ratio of the itaconic acid to the epoxy resin to the solvent is 8:3:15;
The solvent is isopropanol.
The catalyst is dibenzoyl peroxide;
The polymerization inhibitor is 4-hydroxyanisole;
the mixing mass ratio of the itaconic acid to the dibenzoyl peroxide to the 4-hydroxyanisole is 12:1:2.
The mixing mass ratio of the epoxy itaconic acid ester to the maleic resin to the rosin is 4:18:1;
The inert gas is nitrogen;
The vacuum drying temperature is 55 ℃;
the vacuum drying time was 4 hours.
The preparation method of the high-adhesion back surface field aluminum conductive paste of the crystalline silicon solar cell comprises the following steps:
(1) Sequentially adding aluminum powder, silver-coated aluminum powder and silver powder into a stirrer to uniformly stir to obtain a metal conductive filler;
(2) Sequentially adding tributyl phosphate, modified maleic resin, ethylcellulose, tetradecyl glycidyl ether, N-acyl amino acid sodium and an organosilane coupling agent into a stirrer, stirring uniformly, then adding a metal conductive filler, adjusting the temperature to 112 ℃, preserving heat, stirring for 30min, naturally cooling to room temperature to obtain the modified tributyl phosphate, and finally smelting in a muffle furnace at 1200 ℃ for 1 hour to obtain the modified tributyl phosphate.
Example 3
The high-adhesion back surface field aluminum conductive paste for the crystalline silicon solar cell is prepared from the following components in parts by weight: 24 parts of aluminum powder, 4.5 parts of silver-coated aluminum powder, 4 parts of silver powder, 22 parts of tributyl phosphate, 15 parts of modified maleic resin, 7 parts of ethyl cellulose, 5 parts of tetradecyl glycidyl ether, 2 parts of N-acyl amino acid sodium, 1.4 parts of organosilane coupling agent and 35 parts of glass powder.
The preparation method of the silver-coated aluminum powder comprises the following steps:
(1) Adding aluminum powder into a dispersing agent to prepare a solution;
(2) Adding hydrochloric acid into the solution, stirring and reacting for 10min, filtering, washing with water to neutrality, and drying to obtain activated aluminum powder;
(3) Mixing silver nitrate, glucose and water, and stirring for 40 min to obtain a reaction solution;
(4) Adding activated aluminum powder into deionized water, and uniformly stirring to obtain aluminum powder suspension;
(5) And adding the prepared reaction liquid into aluminum powder suspension, stirring at room temperature for reaction for 30 min, separating by adopting a centrifugal machine, filtering, washing with water to be neutral, and drying in a drying oven to obtain the silver-coated aluminum powder.
The mixing mass ratio of the aluminum powder to the dispersing agent is 1:20;
the dispersing agent is ethanol solution;
the mass fraction of the ethanol solution is 10%.
The concentration of the hydrochloric acid is 0.5 mol/L;
The mixing mass ratio of the hydrochloric acid to the solution is 1:10;
the mixing mass ratio of the silver nitrate to the glucose to the water is 3:1:15;
The mass fraction of the aluminum powder suspension is 12.5%;
The mixing mass ratio of the reaction liquid to the aluminum powder suspension is 1:3.
The preparation method of the modified maleic acid resin comprises the following steps:
adding itaconic acid, epoxy resin and solvent into a reaction kettle according to a proportion, heating and stirring, heating the temperature to 75 ℃ at a heating rate of 5 ℃/s, then adding a catalyst and a polymerization inhibitor, continuously heating to 90 ℃, keeping the temperature and stirring for reaction for 1 hour, ending the reaction, and performing reduced pressure distillation to recover the solvent to obtain the epoxy itaconic acid ester;
Sequentially adding the obtained epoxy itaconic acid ester, maleic resin and rosin into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, heating to melt, stirring for 30min at a rotating speed of 500 r/min, naturally cooling to room temperature, performing vacuum drying treatment, and finally crushing and sieving to obtain the modified maleic resin.
The epoxy resin adopts glycidol amine epoxy resin.
The mixing mass ratio of the itaconic acid to the epoxy resin to the solvent is 8:3:15;
The solvent is isopropanol.
The catalyst is dibenzoyl peroxide;
The polymerization inhibitor is 4-hydroxyanisole;
the mixing mass ratio of the itaconic acid to the dibenzoyl peroxide to the 4-hydroxyanisole is 12:1:2.
The mixing mass ratio of the epoxy itaconic acid ester to the maleic resin to the rosin is 4:18:1;
The inert gas is nitrogen;
The vacuum drying temperature is 55 ℃;
the vacuum drying time was 4 hours.
The preparation method of the high-adhesion back surface field aluminum conductive paste of the crystalline silicon solar cell comprises the following steps:
(1) Sequentially adding aluminum powder, silver-coated aluminum powder and silver powder into a stirrer to uniformly stir to obtain a metal conductive filler;
(2) Sequentially adding tributyl phosphate, modified maleic resin, ethylcellulose, tetradecyl glycidyl ether, N-acyl amino acid sodium and an organosilane coupling agent into a stirrer, stirring uniformly, then adding a metal conductive filler, adjusting the temperature to 112 ℃, preserving heat, stirring for 30min, naturally cooling to room temperature to obtain the modified tributyl phosphate, and finally smelting in a muffle furnace at 1200 ℃ for 1 hour to obtain the modified tributyl phosphate.
Example 4
The high-adhesion back surface field aluminum conductive paste for the crystalline silicon solar cell is prepared from the following components in parts by weight: 25 parts of aluminum powder, 5 parts of silver-coated aluminum powder, 5 parts of silver powder, 25 parts of tributyl phosphate, 16 parts of modified maleic resin, 8 parts of ethyl cellulose, 6 parts of tetradecyl glycidyl ether, 3 parts of sodium N-acyl amino acid, 1.5 parts of organosilane coupling agent and 40 parts of glass powder.
The preparation method of the silver-coated aluminum powder comprises the following steps:
(1) Adding aluminum powder into a dispersing agent to prepare a solution;
(2) Adding hydrochloric acid into the solution, stirring and reacting for 10min, filtering, washing with water to neutrality, and drying to obtain activated aluminum powder;
(3) Mixing silver nitrate, glucose and water, and stirring for 40 min to obtain a reaction solution;
(4) Adding activated aluminum powder into deionized water, and uniformly stirring to obtain aluminum powder suspension;
(5) And adding the prepared reaction liquid into aluminum powder suspension, stirring at room temperature for reaction for 30 min, separating by adopting a centrifugal machine, filtering, washing with water to be neutral, and drying in a drying oven to obtain the silver-coated aluminum powder.
The mixing mass ratio of the aluminum powder to the dispersing agent is 1:20;
the dispersing agent is ethanol solution;
the mass fraction of the ethanol solution is 10%.
The concentration of the hydrochloric acid is 0.5 mol/L;
The mixing mass ratio of the hydrochloric acid to the solution is 1:10;
the mixing mass ratio of the silver nitrate to the glucose to the water is 3:1:15;
The mass fraction of the aluminum powder suspension is 12.5%;
The mixing mass ratio of the reaction liquid to the aluminum powder suspension is 1:3.
The preparation method of the modified maleic acid resin comprises the following steps:
adding itaconic acid, epoxy resin and solvent into a reaction kettle according to a proportion, heating and stirring, heating the temperature to 75 ℃ at a heating rate of 5 ℃/s, then adding a catalyst and a polymerization inhibitor, continuously heating to 90 ℃, keeping the temperature and stirring for reaction for 1 hour, ending the reaction, and performing reduced pressure distillation to recover the solvent to obtain the epoxy itaconic acid ester;
Sequentially adding the obtained epoxy itaconic acid ester, maleic resin and rosin into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, heating to melt, stirring for 30min at a rotating speed of 500 r/min, naturally cooling to room temperature, performing vacuum drying treatment, and finally crushing and sieving to obtain the modified maleic resin.
The epoxy resin adopts glycidol amine epoxy resin.
The mixing mass ratio of the itaconic acid to the epoxy resin to the solvent is 8:3:15;
The solvent is isopropanol.
The catalyst is dibenzoyl peroxide;
The polymerization inhibitor is 4-hydroxyanisole;
the mixing mass ratio of the itaconic acid to the dibenzoyl peroxide to the 4-hydroxyanisole is 12:1:2.
The mixing mass ratio of the epoxy itaconic acid ester to the maleic resin to the rosin is 4:18:1;
The inert gas is nitrogen;
The vacuum drying temperature is 55 ℃;
the vacuum drying time was 4 hours.
The preparation method of the high-adhesion back surface field aluminum conductive paste of the crystalline silicon solar cell comprises the following steps:
(1) Sequentially adding aluminum powder, silver-coated aluminum powder and silver powder into a stirrer to uniformly stir to obtain a metal conductive filler;
(2) Sequentially adding tributyl phosphate, modified maleic resin, ethylcellulose, tetradecyl glycidyl ether, N-acyl amino acid sodium and an organosilane coupling agent into a stirrer, stirring uniformly, then adding a metal conductive filler, adjusting the temperature to 112 ℃, preserving heat, stirring for 30min, naturally cooling to room temperature, and finally smelting in a muffle furnace at 1200 ℃ for 1 hour to obtain the modified tributyl phosphate.
Comparative example 1: the difference from example 1 is that the maleic resin was not modified;
comparative example 2: the difference from example 1 is that no silver-coated aluminum powder was added;
Experiment
Performance testing of the conductive slurries of examples and comparative examples:
adhesion detection (see national standard GB 1720-1979 (1989)):
TABLE 1
| Adhesion/N | |
| Example 1 | 32.4 |
| Example 2 | 33.3 |
| Example 3 | 32.8 |
| Example 4 | 32.1 |
| Comparative example 1 | 25.4 |
As can be seen from table 1, the conductive paste prepared according to the present invention has excellent adhesion.
The photoelectric conversion efficiency of the solar cell adopting the conductive paste of the examples and the comparative examples is detected, and the industry standard is referred to: photocell measurement method part 3: photoelectric conversion efficiency, performing:
TABLE 2
| Photoelectric conversion efficiency% | |
| Example 1 | 16.2 |
| Example 2 | 17.3 |
| Example 3 | 17.1 |
| Example 4 | 16.6 |
| Comparative example 1 | 10.4 |
| Comparative example 2 | 14.3 |
As can be seen from table 2, the photoelectric conversion efficiency of the solar cell can be further improved by using the conductive paste of the present invention.
The viscosity performance of the conductive paste is detected:
TABLE 3 Table 3
| Viscosity Pa.s | |
| Example 1 | 32.3 |
| Example 2 | 31.8 |
| Example 3 | 32.0 |
| Example 4 | 32.4 |
As can be seen from table 3, the conductive paste prepared according to the present invention has a suitable viscosity for use in a subsequent solar cell.
After the conductive paste of the embodiment and the comparative example is applied to the back surface field of the solar cell, detecting and observing the appearance by using a vernier caliper;
TABLE 4 Table 4
As can be seen from table 4, the conductive paste prepared by the invention has smooth appearance and strong adhesive force when used in the back surface field of the crystalline silicon solar cell.
Based on the sample of example 1, the effect of different parts by weight of silver-coated aluminum powder on photoelectric conversion efficiency was compared as shown in fig. 1.
Based on the sample of example 1, the effect of different amounts of aluminum powder added on photoelectric conversion efficiency was compared, as shown in fig. 2.
The foregoing description of the preferred embodiments of the invention should not be taken as limiting the scope of the invention, which is defined by the appended claims, but rather by the description of the preferred embodiments, all changes and modifications that come within the meaning and range of equivalency of the claims are intended to be embraced therein.
Claims (6)
1. The high-adhesion back surface field aluminum conductive paste for the crystalline silicon solar cell is characterized in that: the composition is prepared from the following components in parts by weight: 20-25 parts of aluminum powder, 4-5 parts of silver coated aluminum powder, 3-5 parts of silver powder, 18-25 parts of tributyl phosphate, 12-16 parts of modified maleic acid resin, 6-8 parts of ethyl cellulose, 2-6 parts of tetradecyl glycidyl ether, 1-3 parts of N-acyl amino acid sodium, 1.3-1.5 parts of organosilane coupling agent and 30-40 parts of glass powder; the preparation method of the modified maleic acid resin comprises the following steps:
adding itaconic acid, epoxy resin and solvent into a reaction kettle according to a proportion, heating and stirring, heating to 75 ℃ at a heating rate of 5 ℃/s, then adding a catalyst and a polymerization inhibitor, continuously heating to 90 ℃, keeping the temperature and stirring for reaction for 1 hour, ending the reaction, and carrying out reduced pressure distillation to recover the solvent to obtain the epoxy itaconic acid ester;
Sequentially adding the obtained epoxy itaconic acid ester, maleic resin and rosin into a reaction kettle, introducing inert gas into the reaction kettle, discharging air in the reaction kettle, heating to melt, stirring at a rotating speed of 500r/min for 30min, naturally cooling to room temperature, carrying out vacuum drying treatment, and finally crushing and sieving to obtain modified maleic resin; the epoxy resin adopts glycidol amine epoxy resin; the mixing mass ratio of the itaconic acid to the epoxy resin to the solvent is 8:3:15;
The solvent is isopropanol;
the mixing mass ratio of the epoxy itaconic acid ester to the maleic resin to the rosin is 4:18:1;
The inert gas is nitrogen;
The vacuum drying temperature is 55 ℃;
the vacuum drying time was 4 hours.
2. The high adhesion back surface field aluminum conductive paste for crystalline silicon solar cells according to claim 1, wherein: the preparation method of the silver-coated aluminum powder comprises the following steps:
(1) Adding aluminum powder into a dispersing agent to prepare a solution;
(2) Adding hydrochloric acid into the solution, stirring and reacting for 10min, filtering, washing with water to be neutral, and drying to obtain activated aluminum powder;
(3) Mixing silver nitrate, glucose and water, and stirring for 40min to obtain a reaction solution;
(4) Adding activated aluminum powder into deionized water, and uniformly stirring to obtain aluminum powder suspension;
(5) And adding the prepared reaction liquid into aluminum powder suspension, stirring at room temperature for reaction for 30min, separating by adopting a centrifugal machine, filtering, washing with water to be neutral, and drying in a drying oven to obtain the silver-coated aluminum powder.
3. The high adhesion back surface field aluminum conductive paste for crystalline silicon solar cells according to claim 2, wherein: the mixing mass ratio of the aluminum powder to the dispersing agent is 1:20;
the dispersing agent is ethanol solution;
The mass fraction of the ethanol solution is 10%.
4. The high adhesion back surface field aluminum conductive paste for crystalline silicon solar cells according to claim 2, wherein: the concentration of the hydrochloric acid is 0.5mol/L;
The mixing mass ratio of the hydrochloric acid to the solution is 1:10;
the mixing mass ratio of the silver nitrate to the glucose to the water is 3:1:15;
The mass fraction of the aluminum powder suspension is 12.5%;
The mixing mass ratio of the reaction liquid to the aluminum powder suspension is 1:3.
5. The high adhesion back surface field aluminum conductive paste for crystalline silicon solar cells according to claim 1, wherein: the catalyst is dibenzoyl peroxide;
The polymerization inhibitor is 4-hydroxyanisole;
the mixing mass ratio of the itaconic acid to the dibenzoyl peroxide to the 4-hydroxyanisole is 12:1:2.
6. The method for preparing the high-adhesion back surface field aluminum conductive paste for the crystalline silicon solar cell, which is disclosed in claim 1, is characterized in that: the method comprises the following steps:
(1) Sequentially adding aluminum powder, silver-coated aluminum powder and silver powder into a stirrer to uniformly stir to obtain a metal conductive filler;
(2) Sequentially adding tributyl phosphate, modified maleic resin, ethylcellulose, tetradecyl glycidyl ether, N-acyl amino acid sodium, an organosilane coupling agent and glass powder into a stirrer, stirring uniformly, then adding a metal conductive filler, regulating the temperature to 112 ℃, preserving heat and stirring for 30min, then naturally cooling to room temperature, and finally smelting in a muffle furnace at 1200 ℃ for 1 hour to obtain the modified tributyl phosphate.
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| CN103514974A (en) * | 2012-06-22 | 2014-01-15 | 日本油漆株式会社 | Electroconductive aluminium-dispersed paste, manufacturing method of solar cell and solar cell |
| CN105814093A (en) * | 2013-12-16 | 2016-07-27 | 日立化成株式会社 | Resin paste composition and semiconductor device |
| CN114360760A (en) * | 2021-12-31 | 2022-04-15 | 广东南海启明光大科技有限公司 | Conductive powder, thick-film silver-aluminum paste, and preparation method and application thereof |
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| KR101133466B1 (en) * | 2008-09-08 | 2012-04-09 | 주식회사 에프피 | Low temperature dryable conductive paste composite for solar cell and printing method using the same |
| WO2012033303A2 (en) * | 2010-09-08 | 2012-03-15 | Dongjin Semichem Co., Ltd. | Zno-based glass frit composition and aluminum paste composition for back contacts of solar cell using the same |
| CN102314958A (en) * | 2011-08-31 | 2012-01-11 | 乐凯胶片股份有限公司 | Conductive aluminum paste used for crystalline-silicon solar-battery back electrode and preparation method thereof |
| WO2014146306A1 (en) * | 2013-03-22 | 2014-09-25 | 深圳首创光伏有限公司 | Conductive slurry of positive electrode of solar cell and preparing method thereof |
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| CN103514974A (en) * | 2012-06-22 | 2014-01-15 | 日本油漆株式会社 | Electroconductive aluminium-dispersed paste, manufacturing method of solar cell and solar cell |
| CN105814093A (en) * | 2013-12-16 | 2016-07-27 | 日立化成株式会社 | Resin paste composition and semiconductor device |
| CN114360760A (en) * | 2021-12-31 | 2022-04-15 | 广东南海启明光大科技有限公司 | Conductive powder, thick-film silver-aluminum paste, and preparation method and application thereof |
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