CN110504044B - Conductive silver paste and preparation method thereof - Google Patents
Conductive silver paste and preparation method thereof Download PDFInfo
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- CN110504044B CN110504044B CN201910887310.2A CN201910887310A CN110504044B CN 110504044 B CN110504044 B CN 110504044B CN 201910887310 A CN201910887310 A CN 201910887310A CN 110504044 B CN110504044 B CN 110504044B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 52
- ZFOZVQLOBQUTQQ-UHFFFAOYSA-N Tributyl citrate Chemical compound CCCCOC(=O)CC(O)(C(=O)OCCCC)CC(=O)OCCCC ZFOZVQLOBQUTQQ-UHFFFAOYSA-N 0.000 claims abstract description 36
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 22
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 22
- 239000001856 Ethyl cellulose Substances 0.000 claims abstract description 18
- 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 18
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims abstract description 18
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920001249 ethyl cellulose Polymers 0.000 claims abstract description 18
- 235000019325 ethyl cellulose Nutrition 0.000 claims abstract description 18
- 239000011521 glass Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 229940116411 terpineol Drugs 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 16
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000012153 distilled water Substances 0.000 claims description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000012046 mixed solvent Substances 0.000 claims description 14
- 239000011148 porous material Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 4
- 229910052709 silver Inorganic materials 0.000 abstract description 4
- 239000004332 silver Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 239000002002 slurry Substances 0.000 description 8
- 239000000523 sample Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000003556 assay Methods 0.000 description 5
- 239000000306 component Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Images
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
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
Abstract
The invention provides conductive silver paste and a preparation method thereof, and belongs to the technical field of metal materials. The conductive silver paste consists of flaky porous silver powder, glass powder, ethyl cellulose, terpineol and tributyl citrate. The conductive silver paste is prepared by the following specific steps: pouring the ammonium thiocyanate aqueous solution into the silver nitrate aqueous solution at one time, stirring for 30min, filtering, washing and drying the product, and adding a sodium borohydride aqueous solution to obtain X-type flaky porous silver powder; and then mixing and stirring the X-type flaky porous silver powder, the glass powder, the ethyl cellulose, the terpineol and the tributyl citrate, and adjusting the proportion of the materials to obtain the silver paste. The preparation process of the flaky porous silver powder and the silver paste compounding process do not need high temperature and high pressure, and the preparation method is suitable for large-scale production. Because the flaky porous silver powder is rich in holes, the conductive silver paste can show excellent conductivity even if the content of the silver powder is low after sintering and forming, and the conductive silver paste has the advantage of low cost.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to conductive silver paste and a preparation method thereof.
Background
With the vigorous development of the electronic information era, the electronic paste industry has a huge development space of Yanwanchun and the like, the preparation of low-temperature sintering nano-copper soldering paste and the connection performance analysis thereof, and the soldering bulletin 39(6) and 72-76. As one of widely used electronic pastes, conductive silver paste has become one of the base materials of various electronic components.
As is well known, silver powder, as a core component of conductive silver paste, plays a crucial role in the preparation process, performance and market value of conductive silver paste. Silver powder with different shapes has great influence on the performance of the slurry. The flake silver powder occupies a large proportion in the synthesis of the slurry due to the good two-dimensional structure of the flake silver powder. However, due to the compactness of the surface, the penetration threshold is large, so that a large proportion of silver powder (with a mass fraction of about 70-80%) Liuwann seal and the like needs to be added in the synthesis of later-stage slurry, and a high-performance conductive adhesive and a preparation method thereof, CN 101781540A', can enable the prepared slurry to present ideal conductivity after being cured or sintered, thereby greatly increasing the cost of the product.
Porous materials have a high specific surface area, with outstanding lightweight, adsorptive properties "YY Xia, et al," Nanoporous gold film: catalyzing and activating as a catalytic maker, Dalton trains, 2015,44, 11929-. The flake porous silver powder is used as a conductive component, so that the later-stage slurry can be endowed with good conductivity. Meanwhile, the conductive paste has light weight and can absorb a large amount of non-conductive components in the inner cavity, so that the conductive paste is beneficial to preparing low-cost conductive paste. However, the current flaky porous silver powder is lack of a large-scale preparation method, so that the research on the slurry is not deep enough. Therefore, a novel synthesis method of the flaky porous silver powder capable of being scaled is developed, and the preparation of the conductive paste taking the flaky porous silver micro-nano structure as the conductive component is developed, so that the preparation method has important significance for obtaining the low-cost conductive paste.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the conductive silver paste and the preparation method thereof, so that the high-conductivity silver paste with low cost is obtained, and meanwhile, the preparation process is simple and the large-scale production is easy.
The invention is realized by the following technical scheme.
The invention relates to conductive silver paste which is composed of flaky porous silver powder, glass powder, ethyl cellulose, terpineol and tributyl citrate; the flaky porous silver powder is similar to English letters X in appearance, 25-30 mu m in length and 5-7 mu m in width, is rich in multiple pores on the surface, and has the pore diameter of 180-220 nm.
The invention also provides a preparation method of the conductive silver paste, which comprises the following specific steps:
1. pouring the ammonium thiocyanate aqueous solution into the silver nitrate aqueous solution at one time according to the volume ratio of (1-15):1 at room temperature, stirring for 30min, filtering the product, washing with a large amount of water, and drying in vacuum at 40 ℃ to obtain the product A. The molar concentration of the ammonium thiocyanate aqueous solution is (0.3-0.9) M, and the molar concentration of the silver nitrate aqueous solution is (0.05-0.1) M.
2. And re-dispersing the product A in distilled water, adding a sodium borohydride aqueous solution, reacting for 10min, filtering to obtain insoluble substances, washing with distilled water and ethanol, and drying in vacuum at 40 ℃ to obtain the X-shaped flaky porous silver powder. The mass ratio of the product A to distilled water is 1:10, the mass fraction of the sodium borohydride aqueous solution is 10%, and the volume ratio of the product A to the sodium borohydride aqueous solution is 1: 10.
3. Mixing and stirring the flaky porous silver powder similar to the X shape and the glass powder under the solid condition to obtain a product B. The mass ratio of the X-shaped flaky porous silver powder to the glass powder is 16: 1.
4. And dissolving ethyl cellulose in a mixed solvent of terpineol and tributyl citrate at 90 ℃ to obtain a solution C. The mass fraction of the ethyl cellulose in the solution C is 4%, and the volume ratio of the terpineol to the tributyl citrate in the mixed solvent is 1: 10.
5. And (3) mixing the product B and the solution C for 1h at room temperature by using a three-roller machine to obtain the viscous conductive silver paste. The mass ratio of the product B to the solution C in the conductive silver paste is 17 (8-11).
Compared with the prior art, the invention has the following technical effects:
1. the preparation process of the flake porous silver powder does not need high temperature and high pressure, does not need an organic solvent, and has good product porosity; meanwhile, the method has the advantages of simple process, convenient synthesis and easy large-scale production.
2. The invention prepares the flaky porous silver powder similar to the X shape. Because the flaky porous silver powder is rich in holes, the conductive silver paste can show excellent conductivity even if the content of the silver powder is low after sintering and forming, and the conductive silver paste has the advantage of low cost.
3. When the mass fraction of the flaky porous silver powder is lower in the conductive silver paste prepared by taking the flaky porous silver powder as a conductive component (<65%), excellent conductivity (8X 10) can be obtained after sintering4～1.2×105S/cm) (sintering conditions: sintering at 700 deg.C in air for 4 min; conductivity test conditions: standard four-probe measurement), it can be seen that the method has the advantages of remarkably low cost and high conductivity.
Drawings
FIG. 1 is a typical scanning electron micrograph of a sheet-like porous silver powder obtained in example 1 of the present invention;
as shown in the figure, the flake-like porous silver powder of the present invention has an appearance similar to English letter X, a length of about 25 to 30 μm, a width of about 5 to 7 μm, a surface rich in pores, and a pore diameter of about 200 nm.
FIG. 2 is a photograph of the electroconductive paste obtained in example 1 of the present invention after sintering;
as shown in the figure, after the conductive paste is sintered, the surface is smooth and slightly yellowish, and the conductive paste is strongly adhered to the surface of a substrate.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to the examples.
Example 1
1. Pouring the ammonium thiocyanate aqueous solution into the silver nitrate aqueous solution at one time at room temperature according to the volume ratio of 1:1, stirring for 30min, filtering the product, washing with a large amount of water, and drying in vacuum at 40 ℃ to obtain a product A. The molar concentration of the ammonium thiocyanate aqueous solution is 0.3M, and the molar concentration of the silver nitrate aqueous solution is 0.05M.
2. And re-dispersing the product A in distilled water, adding a sodium borohydride aqueous solution, reacting for 10min, filtering to obtain insoluble substances, washing with distilled water and ethanol, and drying in vacuum at 40 ℃ to obtain the X-shaped flaky porous silver powder. The mass ratio of the product A to distilled water is 1:10, the mass fraction of the sodium borohydride aqueous solution is 10%, and the volume ratio of the product A to the sodium borohydride aqueous solution is 1: 10.
3. Mixing and stirring the flaky porous silver powder similar to the X shape and the glass powder under the solid condition to obtain a product B. The mass ratio of the X-shaped flaky porous silver powder to the glass powder is 16: 1.
4. And dissolving ethyl cellulose in a mixed solvent of terpineol and tributyl citrate at 90 ℃ to obtain a solution C. The mass fraction of the ethyl cellulose in the solution C is 4%, and the volume ratio of the terpineol to the tributyl citrate in the mixed solvent is 1: 10.
5. And (3) mixing the product B and the solution C for 1h at room temperature by using a three-roller machine to obtain the viscous conductive silver paste. The mass ratio of the product B to the solution C in the conductive silver paste is 17:8.
The conductive paste can obtain the conductive paste with excellent conductivity (1.2 multiplied by 10) after being sintered5S/cm) (sintering conditions: sintering at 700 deg.C in air for 4 min; conductivity test conditions: standard four probe assay).
Example 2
1. Pouring the ammonium thiocyanate aqueous solution into the silver nitrate aqueous solution at one time at room temperature according to the volume ratio of 15:1, stirring for 30min, filtering the product, washing with a large amount of water, and drying in vacuum at 40 ℃ to obtain a product A. The molar concentration of the ammonium thiocyanate aqueous solution is 0.9M, and the molar concentration of the silver nitrate aqueous solution is 0.1M.
2. And re-dispersing the product A in distilled water, adding a sodium borohydride aqueous solution, reacting for 10min, filtering to obtain insoluble substances, washing with distilled water and ethanol, and drying in vacuum at 40 ℃ to obtain the X-shaped flaky porous silver powder. The mass ratio of the product A to distilled water is 1:10, the mass fraction of the sodium borohydride aqueous solution is 10%, and the volume ratio of the product A to the sodium borohydride aqueous solution is 1: 10.
3. Mixing and stirring the flaky porous silver powder similar to the X shape and the glass powder under the solid condition to obtain a product B. The mass ratio of the X-shaped flaky porous silver powder to the glass powder is 16: 1.
4. And dissolving ethyl cellulose in a mixed solvent of terpineol and tributyl citrate at 90 ℃ to obtain a solution C. The mass fraction of the ethyl cellulose in the solution C is 4%, and the volume ratio of the terpineol to the tributyl citrate in the mixed solvent is 1: 10.
5. And (3) mixing the product B and the solution C for 1h at room temperature by using a three-roller machine to obtain the viscous conductive slurry. The mass ratio of the product B to the solution C in the conductive silver paste is 17: 11.
After the conductive paste is sintered, the conductive paste with excellent conductivity (8 multiplied by 10) can be obtained4S/cm) (sintering conditions: sintering at 700 deg.C in air for 4 min; conductivity test conditions: standard four probe assay).
Example 3
1. Pouring the ammonium thiocyanate aqueous solution into the silver nitrate aqueous solution at one time at room temperature according to the volume ratio of 5:1, stirring for 30min, filtering the product, washing with a large amount of water, and drying in vacuum at 40 ℃ to obtain a product A. The molar concentration of the ammonium thiocyanate aqueous solution is 0.7M, and the molar concentration of the silver nitrate aqueous solution is 0.08M.
2. And re-dispersing the product A in distilled water, adding a sodium borohydride aqueous solution, reacting for 10min, filtering to obtain insoluble substances, washing with distilled water and ethanol, and drying in vacuum at 40 ℃ to obtain the X-shaped flaky porous silver powder. The mass ratio of the product A to distilled water is 1:10, the mass fraction of the sodium borohydride aqueous solution is 10%, and the volume ratio of the product A to the sodium borohydride aqueous solution is 1: 10.
3. Mixing and stirring the flaky porous silver powder similar to the X shape and the glass powder under the solid condition to obtain a product B. The mass ratio of the X-shaped flaky porous silver powder to the glass powder is 16: 1.
4. And dissolving ethyl cellulose in a mixed solvent of terpineol and tributyl citrate at 90 ℃ to obtain a solution C. The mass fraction of the ethyl cellulose in the solution C is 4%, and the volume ratio of the terpineol to the tributyl citrate in the mixed solvent is 1: 10.
5. And (3) mixing the product B and the solution C for 1h at room temperature by using a three-roller machine to obtain the viscous conductive slurry. The mass ratio of the product B to the solution C in the conductive silver paste is 17: 9.
The conductive paste can be obtained after sinteringHas excellent conductivity (1.1 × 10)5S/cm) (sintering conditions: sintering at 700 deg.C in air for 4 min; conductivity test conditions: standard four probe assay).
Example 4
1. Pouring the ammonium thiocyanate aqueous solution into the silver nitrate aqueous solution at one time at room temperature according to the volume ratio of 3:1, stirring for 30min, filtering the product, washing with a large amount of water, and drying in vacuum at 40 ℃ to obtain a product A. The molar concentration of the ammonium thiocyanate aqueous solution is 0.6M, and the molar concentration of the silver nitrate aqueous solution is 0.08M.
2. And re-dispersing the product A in distilled water, adding a sodium borohydride aqueous solution, reacting for 10min, filtering to obtain insoluble substances, washing with distilled water and ethanol, and drying in vacuum at 40 ℃ to obtain the X-shaped flaky porous silver powder. The mass ratio of the product A to distilled water is 1:10, the mass fraction of the sodium borohydride aqueous solution is 10%, and the volume ratio of the product A to the sodium borohydride aqueous solution is 1: 10.
3. Mixing and stirring the flaky porous silver powder similar to the X shape and the glass powder under the solid condition to obtain a product B. The mass ratio of the X-shaped flaky porous silver powder to the glass powder is 16: 1.
4. And dissolving ethyl cellulose in a mixed solvent of terpineol and tributyl citrate at 90 ℃ to obtain a solution C. The mass fraction of the ethyl cellulose in the solution C is 4%, and the volume ratio of the terpineol to the tributyl citrate in the mixed solvent is 1: 10.
5. And (3) mixing the product B and the solution C for 1h at room temperature by using a three-roller machine to obtain the viscous conductive silver paste. The mass ratio of the product B to the solution C in the conductive silver paste is 17: 10.
After the conductive paste is sintered, the conductive paste with excellent conductivity (9 multiplied by 10) can be obtained4S/cm) (sintering conditions: sintering at 700 deg.C in air for 4 min; conductivity test conditions: standard four probe assay).
Example 5
1. Pouring the ammonium thiocyanate aqueous solution into the silver nitrate aqueous solution at one time at room temperature according to the volume ratio of 12:1, stirring for 30min, filtering the product, washing with a large amount of water, and drying in vacuum at 40 ℃ to obtain a product A. The molar concentration of the ammonium thiocyanate aqueous solution is 0.75M, and the molar concentration of the silver nitrate aqueous solution is 0.08M.
2. And re-dispersing the product A in distilled water, adding a sodium borohydride aqueous solution, reacting for 10min, filtering to obtain insoluble substances, washing with distilled water and ethanol, and drying in vacuum at 40 ℃ to obtain the X-shaped flaky porous silver powder. The mass ratio of the product A to distilled water is 1:10, the mass fraction of the sodium borohydride aqueous solution is 10%, and the volume ratio of the product A to the sodium borohydride aqueous solution is 1: 10.
3. Mixing and stirring the flaky porous silver powder similar to the X shape and the glass powder under the solid condition to obtain a product B. The mass ratio of the X-shaped flaky porous silver powder to the glass powder is 16: 1.
4. And dissolving ethyl cellulose in a mixed solvent of terpineol and tributyl citrate at 90 ℃ to obtain a solution C. The mass fraction of the ethyl cellulose in the solution C is 4%, and the volume ratio of the terpineol to the tributyl citrate in the mixed solvent is 1: 10.
5. And (3) mixing the product B and the solution C for 1h at room temperature by using a three-roller machine to obtain the viscous conductive silver paste. The mass ratio of the product B to the solution C in the conductive silver paste is 17: 8.5.
The conductive paste can obtain the conductive paste with excellent conductivity (1.12 multiplied by 10) after being sintered4S/cm) (sintering conditions: sintering at 700 deg.C in air for 4 min; conductivity test conditions: standard four probe assay).
Claims (1)
1. The conductive silver paste is characterized by comprising flaky porous silver powder, glass powder, ethyl cellulose, terpineol and tributyl citrate;
the flaky porous silver powder is similar to English letters X in appearance, 25-30 mu m in length and 5-7 mu m in width, is rich in multiple pores on the surface, and has the pore diameter of 180-220 nm;
the preparation method of the conductive silver paste comprises the following steps:
(1) pouring an ammonium thiocyanate aqueous solution into a silver nitrate aqueous solution at one time according to the volume ratio of (1-15):1 at room temperature, stirring for 30min, filtering, washing a large amount of water, and drying in vacuum at 40 ℃ to obtain a product A;
the molar concentration of the ammonium thiocyanate aqueous solution is 0.3-0.9M, and the molar concentration of the silver nitrate aqueous solution is 0.05-0.1M;
(2) re-dispersing the product A in distilled water, adding a sodium borohydride aqueous solution, reacting for 10min, filtering to obtain insoluble substances, washing with distilled water and ethanol, and vacuum-drying at 40 ℃ to obtain the flaky porous silver powder;
the mass ratio of the product A to distilled water is 1:10, the mass fraction of the sodium borohydride aqueous solution is 10%, and the volume ratio of the product A to the sodium borohydride aqueous solution is 1: 10;
(3) mixing and stirring the flaky porous silver powder obtained in the step (2) and glass powder under a solid condition to obtain a product B;
the mass ratio of the flaky porous silver powder to the glass powder is 16: 1;
(4) dissolving ethyl cellulose in a mixed solvent of terpineol and tributyl citrate at 90 ℃ to obtain a solution C;
the mass fraction of the ethyl cellulose in the solution C is 4%, and the volume ratio of the terpineol to the tributyl citrate in the mixed solvent is 1: 10;
(5) mixing the product B and the solution C for 1h at room temperature by a three-roller machine to obtain viscous conductive silver paste;
the mass ratio of the product B to the solution C in the conductive silver paste is 17 (8-11).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104470656A (en) * | 2012-07-18 | 2015-03-25 | 福田金属箔粉工业株式会社 | Ultrathin flake-type silver powder and manufacturing method therefor |
| CN105913897A (en) * | 2016-06-01 | 2016-08-31 | 江苏泓源光电科技股份有限公司 | Crystalline silicon solar cell silver paste with low silver content and preparation method thereof |
| CN107068240A (en) * | 2017-02-20 | 2017-08-18 | 江苏瑞德新能源科技有限公司 | A kind of back silver paste |
| CN107545941A (en) * | 2016-06-23 | 2018-01-05 | 扬中市润宇电力设备有限公司 | A kind of method for preparing solar cell front side silver paste slurry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP5945480B2 (en) * | 2012-09-07 | 2016-07-05 | ナミックス株式会社 | Silver paste composition and method for producing the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104470656A (en) * | 2012-07-18 | 2015-03-25 | 福田金属箔粉工业株式会社 | Ultrathin flake-type silver powder and manufacturing method therefor |
| CN105913897A (en) * | 2016-06-01 | 2016-08-31 | 江苏泓源光电科技股份有限公司 | Crystalline silicon solar cell silver paste with low silver content and preparation method thereof |
| CN107545941A (en) * | 2016-06-23 | 2018-01-05 | 扬中市润宇电力设备有限公司 | A kind of method for preparing solar cell front side silver paste slurry |
| CN107068240A (en) * | 2017-02-20 | 2017-08-18 | 江苏瑞德新能源科技有限公司 | A kind of back silver paste |
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