CN114999704A - Auxiliary glass powder additive for silver paste and preparation method thereof - Google Patents
Auxiliary glass powder additive for silver paste and preparation method thereof Download PDFInfo
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- CN114999704A CN114999704A CN202210349286.9A CN202210349286A CN114999704A CN 114999704 A CN114999704 A CN 114999704A CN 202210349286 A CN202210349286 A CN 202210349286A CN 114999704 A CN114999704 A CN 114999704A
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- glass powder
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- 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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/07—Glass compositions containing silica with less than 40% silica by weight containing lead
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/102—Glass compositions containing silica with 40% to 90% silica, by weight containing lead
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- 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
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- 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
- Y02E10/547—Monocrystalline silicon PV cells
Abstract
The invention relates to H01L, in particular to an auxiliary glass powder additive for silver paste and a preparation method thereof, wherein the auxiliary glass powder additive comprises at least one of a glass powder additive I and a glass powder additive II, the glass powder additive can be matched with main glass powder in a sintering process, and the problem that high battery conversion efficiency and high positive silver sintering effect are difficult to realize by single glass powder is solved by using different softening points of different additives and different redox reaction sequences. The inventor also finds that when the two glass powder additives and the main glass powder are used together, the silver powder can be promoted to be densified in the sintering process, meanwhile, the complete corrosion of the front silicon nitride antireflection layer is promoted, the silver crystal is promoted to be separated out by etching the emitter, and a plurality of silver colloids are separated out from the sintered intermediate glass layer so as to realize good ohmic contact, and meanwhile, good adhesive force is provided, so that the high conversion efficiency of the solar cell is obtained.
Description
Technical Field
The invention relates to H01L, in particular to an auxiliary glass powder additive for silver paste and a preparation method thereof.
Background
The mainstream solar cells in the market at present include PERC cells, Al-BSF cells, TOPCon cells, HJT cells, etc., wherein PERC cells are dominant and account for about 90% of crystalline silicon solar cells, and how to further improve the photoelectric conversion efficiency of PERC cells and reduce the cost is always a major goal of photovoltaic development.
In the preparation process of the PERC battery, the last procedure is screen printing of front silver paste, and a front electrode with good ohmic contact is formed by short-time high-temperature sintering. The positive silver paste mainly comprises silver powder for ohmic contact, organic additives such as an organic carrier for realizing good printing performance and the like, and glass powder which is a key preparation raw material for realizing ohmic contact. Although the specific gravity of the glass powder in the front silver paste is small, the glass powder has important influence on corrosion of a front silicon nitride film, precipitation of silver crystal grains, ohmic contact of silver and silicon and the like, so that the conversion efficiency of the battery is obviously influenced.
Therefore, there is a need to develop glass powder more beneficial to the function of silver paste and positive electrode, and there are many kinds of glass powder, such as Te-Si-Pb-Bi system crystal glass powder, Pb-Bi-B-Si system glass powder, Bi-Si-B system glass powder, Bi-B-Ba system lead-free glass powder, etc., but the research on the glass powder is mainly focused on the main glass powder, such as CN106892567A, etc., but one glass powder is difficult to achieve better sintering effect, thereby improving conversion efficiency.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides an auxiliary glass frit additive for silver paste, where the glass frit additive is prepared from at least one of a first glass frit additive and a second glass frit additive:
glass powder additive one, including SiO 2 、Bi 2 O 3 、ZnO、WO 3 、PbO、CuO、TeO 2 ；
Glass powder additives II, including SiO 2 、Bi 2 O 3 、ZnO、WO 3 、PbO、TeO 2 。
As a preferred technical scheme of the invention, the preparation raw materials of the first glass powder additive comprise, by weight: SiO 2 2 25-45％、Bi 2 O 3 15-35％、ZnO 5-15％、WO 3 5-20％、PbO 5-15％、CuO 1-10％、TeO 2 1-10％。
As a preferred technical scheme of the invention, the preparation raw materials of the first glass powder additive comprise, by weight: SiO 2 2 30-40％、Bi 2 O 3 15-30％、ZnO 5-10％、WO 3 5-25％、PbO 5-10％、CuO 1-5％、TeO 2 1-5％。
As a preferred technical scheme of the invention, the preparation raw materials of the first glass powder additive comprise, by weight: SiO 2 2 33-38％、Bi 2 O 3 25-30％、ZnO 5-10％、WO 3 8-15％、PbO 8-10％、CuO 1-5％、TeO 2 1-5％。
The inventors found that by increasing Bi 3+ And Pb 2+ The content of ions with equal polarizability is reduced to lower the melting temperature of the first glass powder additive, so that the first glass powder additive with medium softening point is obtainedAnd the adhesion of silver powder is promoted with the main glass powder after subsequent silver paste printing and sintering, a more compact structure is formed, and the obvious improvement of Rsh is promoted, but the inventor also finds that Pb and the like can be separated out when the silver powder is melted earlier if the softening point is lower, the deposition of Ag crystal grains and ohmic contact are also influenced, so that the problems of increase of Rser, reduction of FF and the like are caused, and the final Eta is influenced.
As a preferred technical scheme, the preparation raw materials of the second glass powder additive comprise the following components in percentage by weight: SiO 2 2 65-85％、TeO 2 5-15％、PbO 5-15％、WO 3 1-15％、Bi 2 O 3 1-15％、ZnO 1-10％。
As a preferred technical scheme of the invention, the preparation raw materials of the second glass powder additive comprise, by weight: SiO 2 2 70-80％、TeO 2 5-10％、PbO 5-15％、WO 3 1-10％、Bi 2 O 3 1-10％、ZnO 1-10％。
As a preferred technical scheme of the invention, the preparation raw materials of the second glass powder additive comprise, by weight: SiO 2 2 70-75％、TeO 2 5-10％、PbO 5-12％、WO 3 3-8％、Bi 2 O 3 2-8％、ZnO 1-4％。
The inventor also found that by adding the second glass powder additive and controlling the high Si 4+ The content of the glass powder is formed into a structure with silicon-oxygen tetrahedron as a main body structure, PbO is used as a structure with a network outer body, and the glass powder with high softening point is obtained, so that in the process of jointly acting with the main body glass powder and silver powder, silver crystal grains are promoted to be deposited at an Ag/Si interface and are in ohmic contact, the penetration to a positive electrode is reduced, but the compactness is reduced, and the Rser is improved, so that the WO is added 3 And TeO 2 And ZnO, the inventor finds that glass powder with higher FF and Rsh can be obtained, increase of Rser is reduced, and silver paste with higher Eta is obtained.
According to a preferable technical scheme of the invention, the weight ratio of the glass powder additive I to the glass powder additive II is (1-2): (1-2).
The inventor finds that when the glass frit additive I and the glass frit additive II act together with the main glass frit, in the printing and sintering process, on one hand, the glass frit additive is utilized to form a small amount of molten state, the main glass frit, the glass frit additive II and the silver powder are connected, the dissolution of the small amount of silver powder is promoted, the separation of Ag and Pb is promoted along with the melting of the main glass frit, silver crystal grains are attached to the main glass frit and the unmelted glass frit additive II, and meanwhile, through a series of complex redox reactions, the post-molten glass frit additive is also beneficial to reducing the influence of the precipitation of Pb and the like on the sintering stability, so that a compact and high-ohmic contact structure is promoted, the improvement of Uoc, Isc, FF and Rsh and the reduction of Rser are promoted, and the battery with high Eta is obtained.
As a preferable technical scheme of the invention, the D50 of the glass powder additive is 1.5-2 um.
In order to improve the performances of wetting and the like, optimize the doping of the glass powder and the like, and also add a small amount of other oxides, as a preferable technical scheme of the invention, the glass powder additive also comprises MgO and Ni 2 At least one of O, BaO and SnO, MgO and Ni 2 At least one of O, BaO and SnO accounts for 0-5% of the glass powder additive by mass, preferably 0-3% of the glass powder additive by mass, and more preferably 0-1.5% of the glass powder additive by mass.
As a preferable technical scheme of the invention, the second glass powder additive also comprises Na 2 O、K 2 O、Li 2 At least one of O, said Na 2 O、K 2 O、Li 2 At least one of O accounts for 0-10% of the glass powder additive, preferably 0-5%, and more preferably 1-2% by mass of the glass powder additive.
The second aspect of the invention provides a preparation method of the auxiliary glass powder additive for silver paste, which comprises the following steps:
preparing a first glass powder additive: heating, sintering, cooling and grinding a preparation raw material of a first glass powder additive to obtain the first glass powder additive;
preparing a glass powder additive II: and heating, sintering, cooling and grinding the preparation raw materials of the second glass powder additive to obtain the second glass powder additive.
As a preferred technical solution of the present invention, the preparation method of the auxiliary glass frit additive for silver paste comprises:
preparing a first glass powder additive: heating the preparation raw material of the first glass powder additive to 1100-1300 ℃, sintering for 0.5-1h, cooling, drying for 2-3h at 100-120 ℃, ball-milling for 0.5-1h, and jet-milling until D50 is 1.5-2um to obtain the first glass powder additive;
preparing a glass powder additive II: heating the preparation raw material of the second glass powder additive to 1100-1300 ℃, sintering for 0.5-1h, cooling, drying at 100-120 ℃ for 2-3h, ball milling for 0.5-1h, and jet milling until D50 is 1.5-2um to obtain the second glass powder additive.
According to a second aspect of the invention, the silver paste comprises, by weight, 0.05-0.3% of the auxiliary glass powder additive for silver paste, 1-3% of Te-Si-Pb-Bi-based crystalline glass powder, 80-90% of silver powder and 5-12% of an organic carrier.
Compared with the prior art, the invention has the following beneficial effects:
the glass powder additive provided by the invention can be matched with the main glass powder in the sintering process, and the problem that high battery conversion efficiency and high positive silver sintering effect are difficult to realize by single glass powder is solved by utilizing the difference of softening points of different additives and different redox reaction sequences. The inventor also finds that when the two glass powder additives and the main glass powder are used together, the silver powder can be promoted to be densified in the sintering process, meanwhile, the complete corrosion of the front silicon nitride antireflection layer is promoted, the silver crystal is promoted to be separated out by etching the emitter, and a plurality of silver colloids are separated out from the sintered intermediate glass layer so as to realize good ohmic contact, and meanwhile, good adhesive force is provided, so that the high conversion efficiency of the solar cell is obtained. The glass powder additive provided by the invention can be well added into original silver paste, is particularly suitable for front silver paste of a p-type PERC crystalline silicon solar cell, does not need to change the printing, sintering and other processes of the original paste, and is simple in preparation method, low in cost and high in yield.
Drawings
FIG. 1 is a spectrum of a crystal glass powder of Te-Si-Pb-Bi system on the market.
Detailed Description
Examples
Comparative example
Comparative example a crystalline glass frit of the Te-Si-Pb-Bi series, which is commercially available, and having a spectral diagram as shown in fig. 1, and a front silver paste including the commercially available glass frit, the front silver paste including, in parts by weight: 2.3 parts of commercial Te-Si-Pb-Bi crystal glass powder, 89 parts of silver powder, 8.7 parts of commercial organic carrier (7.1 parts of resin hydroxyethyl cellulose, 0.3 part of solvent diethylene glycol monobutyl ether acetate, 0.8 part of plasticizer dibutyl phthalate and 0.5 part of dispersant sorbitan monooleate) are uniformly mixed by a V-shaped stirrer and then are put on a three-roll pulp rolling machine for grinding, and the normal silver paste for the solar cell is obtained.
Example 1
This example provides an additive of glass frit, which comprises 36.3 parts by weight of SiO 2 27.2 parts of Bi 2 O 3 8.4 parts of ZnO, 10.9 parts of WO 3 9.8 parts of PbO, 2.7 parts of CuO and 3.9 parts of TeO 2 And 0.8 part of MgO.
The embodiment also provides a preparation method of the first auxiliary glass frit additive, which comprises the following steps:
uniformly mixing the preparation raw materials of the first auxiliary glass powder additive to obtain mixed powder, filling the mixed powder into a crucible, then putting the crucible into a box-type resistance furnace, heating the resistance furnace to 1200 ℃ for constant-temperature melting, preserving heat for 0.8h to obtain uniform molten glass, pouring the molten glass into a stirred stainless steel container filled with deionized water for quenching, putting the obtained glass granules into a 110 ℃ constant-temperature drying box, drying, finely grinding and air-milling to obtain the first auxiliary glass powder additive with D50 of 1.5-2 um.
The embodiment also provides silver paste which comprises 2.2 parts by weight of commercial Te-Si-Pb-Bi system crystal glass powder, 0.1 part by weight of first auxiliary glass powder additive, 89 parts by weight of silver powder and 8.7 parts by weight of conventional organic carrier, wherein the mixture is uniformly mixed by a V-shaped mixer and then is put on a three-roll paste rolling mill for grinding to obtain the positive silver paste for the solar cell.
Example 2
The second auxiliary glass powder additive comprises 72.8 parts by weight of SiO 2 8.0 parts of TeO 2 8.0 parts of PbO and 4.6 parts of WO 3 4.0 parts of Bi 2 O 3 1.1 parts of ZnO and 1.5 parts of Na 2 O。
The second embodiment also provides a method for preparing the auxiliary glass frit additive, which comprises the following steps:
uniformly mixing the preparation raw materials of the first auxiliary glass powder additive to obtain mixed powder, placing the mixed powder into a crucible, placing the crucible into a box-type resistance furnace, heating the resistance furnace to 1300 ℃ for constant-temperature melting, preserving heat for 1h to obtain uniform molten glass, pouring the molten glass into a stirred stainless steel container filled with deionized water for quenching, placing the obtained glass particles into a 100-120 ℃ constant-temperature drying box, drying, finely grinding and air-flow grinding to obtain the first auxiliary glass powder additive with D50 of 1.5-2 um.
The embodiment also provides a silver paste which comprises 2.2 parts by weight of Te-Si-Pb-Bi series crystal glass powder sold on the market, 0.1 part by weight of auxiliary glass powder additive II, 89 parts by weight of silver powder and 8.7 parts by weight of conventional organic carrier, and the mixture is uniformly mixed by a V-shaped mixer and then is put on a three-roll pulp rolling machine for grinding to obtain the positive silver paste for the solar cell.
Example 3
The present example provides an auxiliary glass frit additive, which includes the first glass frit additive provided in example 1 and the second glass frit additive provided in example 2.
The embodiment also provides silver paste which comprises 2.1 parts by weight of commercial Te-Si-Pb-Bi system crystal glass powder, 0.1 part by weight of first auxiliary glass powder additive, 0.1 part by weight of second auxiliary glass powder additive, 89 parts by weight of silver powder and 8.7 parts by weight of conventional organic carrier, wherein the mixture is uniformly mixed by a V-shaped mixer and then is placed on a three-roll pulp grinder to be ground, and thus the positive silver paste for the solar cell is obtained.
Evaluation of Performance
The positive silver pastes in examples and comparative examples were printed on a p-type PERC crystalline silicon solar cell, dried to obtain a film having a thickness of 20 μm, and sintered at a high temperature of 780 ℃ to obtain a solar cell, and an open circuit voltage (Uoc), Isc (short circuit current), Fill Factor (FF), conversion efficiency (Eta), series resistance (Rser), and Rsh were measured as a shunt resistance (Rsh) by a solar simulator, and the results are shown in table 1.
TABLE 1
| Electrical Properties | Uoc(mV) | Isc(A) | FF(％) | Eta(％) | Rser(mΩ) | Rsh(mΩ) |
| Comparative example | 0.6550 | 10.8002 | 79.93 | 20.645 | 0.001082 | 44.5 |
| Example 1 | 0.6582 | 10.6685 | 79.26 | 20.323 | 0.001143 | 186.4 |
| Example 2 | 0.6646 | 10.7701 | 79.57 | 20.800 | 0.002126 | 69.9 |
| Example 3 | 0.6673 | 10.819 | 80.37 | 21.194 | 0.001086 | 54.7 |
According to the test result, the glass powder additive provided by the invention is added into silver paste, so that the effects of the glass powder and the silver powder in the original silver paste can be improved, the corrosion to the front silicon nitride layer is promoted, and the conversion efficiency of the battery is effectively improved.
Claims (10)
1. The auxiliary glass powder additive for the silver paste is characterized in that raw materials for preparing the glass powder additive comprise at least one of a first glass powder additive and a second glass powder additive:
glass powder additive one, including SiO 2 、Bi 2 O 3 、ZnO、WO 3 、PbO、CuO、TeO 2 ；
Glass powder additives II, including SiO 2 、Bi 2 O 3 、ZnO、WO 3 、PbO、TeO 2 。
2. Silver according to claim 1The auxiliary glass powder additive for the paste is characterized in that the preparation raw materials of the first glass powder additive comprise the following components in percentage by weight: SiO 2 2 25-45％、Bi 2 O 3 15-35％、ZnO 5-15％、WO 3 5-20％、PbO 5-15％、CuO 1-10％、TeO 2 1-10％。
3. The auxiliary glass frit additive for silver paste as claimed in claim 2, wherein the first glass frit additive is prepared from the following raw materials in percentage by weight: SiO 2 2 30-40％、Bi 2 O 3 15-30％、ZnO 5-10％、WO 3 5-25％、PbO 5-10％、CuO 1-5％、TeO 2 1-5％。
4. The auxiliary glass frit additive for silver paste as claimed in claim 1, wherein the second glass frit additive is prepared from the following raw materials in percentage by weight: SiO 2 2 65-85％、TeO 2 5-15％、PbO 5-15％、WO 3 1-15％、Bi 2 O 3 1-15％、ZnO 1-10％。
5. The auxiliary glass frit additive for silver paste as set forth in claim 4, wherein the second glass frit additive is prepared from the following raw materials in percentage by weight: SiO 2 2 70-80％、TeO 2 5-10％、PbO 5-15％、WO 3 1-10％、Bi 2 O 3 1-10％、ZnO 1-10％。
6. The auxiliary glass frit additive for silver paste according to claim 2 or 3, wherein the first glass frit additive further comprises MgO and Ni 2 At least one of O, BaO and SnO, MgO and Ni 2 At least one of O, BaO and SnO accounts for 0-5% of the glass powder additive by mass, and preferably 0-3%.
7. The auxiliary glass frit additive for silver paste according to claim 4 or 5, wherein the glass is selected from the group consisting ofThe powder additive also comprises Na 2 O、K 2 O、Li 2 At least one of O, Na 2 O、K 2 O、Li 2 At least one of O accounts for 0-10% of the glass powder additive by mass, and preferably 0-5% of the glass powder additive by mass.
8. The auxiliary glass frit additive for silver paste according to claim 1, wherein the weight ratio of the first glass frit additive to the second glass frit additive is (1-2): (1-2).
9. The preparation method of the auxiliary glass powder additive for silver paste according to any one of claims 1 to 8, characterized by comprising the following steps:
preparing a first glass powder additive: heating, sintering, cooling and grinding a preparation raw material of a first glass powder additive to obtain the first glass powder additive;
preparing a glass powder additive II: and heating, sintering, cooling and grinding the preparation raw materials of the second glass powder additive to obtain the second glass powder additive.
10. A silver paste characterized by comprising, by weight, 0.05 to 0.3% of the auxiliary glass frit additive for silver paste according to any one of claims 1 to 8, 1 to 3% of Te-Si-Pb-Bi-based crystalline glass frit, 80 to 90% of silver powder and 5 to 12% of an organic vehicle.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115504674A (en) * | 2022-09-26 | 2022-12-23 | 浙江晶科新材料有限公司 | Glass powder for N-type solar cell front slurry and preparation method thereof |
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2022
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115504674A (en) * | 2022-09-26 | 2022-12-23 | 浙江晶科新材料有限公司 | Glass powder for N-type solar cell front slurry and preparation method thereof |
| CN115504674B (en) * | 2022-09-26 | 2023-09-05 | 浙江晶科新材料有限公司 | Glass powder for front surface sizing agent of N-type solar cell and preparation method thereof |
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