CN114799181A - Preparation method of flaky silver powder and application of flaky silver powder in field of conductive paste - Google Patents
Preparation method of flaky silver powder and application of flaky silver powder in field of conductive paste Download PDFInfo
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- CN114799181A CN114799181A CN202110671235.3A CN202110671235A CN114799181A CN 114799181 A CN114799181 A CN 114799181A CN 202110671235 A CN202110671235 A CN 202110671235A CN 114799181 A CN114799181 A CN 114799181A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention relates to the technical field of conductive paste, in particular to a preparation method of flaky silver powder and application of the flaky silver powder in the field of conductive paste. The method specifically comprises the following steps: 1) cleaning the grinding tank by using deionized water, drying in the air, and wetting the inner wall of the grinding tank by using oleic acid; 2) adding silver powder, a dispersing agent and a grinding ball into the grinding tank, and then tightly covering the cover of the grinding tank; 3) placing the grinding tank in a ball mill for ball milling; 4) and (4) after the ball milling is finished, washing the silver powder by deionized water and ethanol, and drying the silver powder to obtain the fine silver powder. The preparation method of the flaky silver powder and the application of the flaky silver powder in the field of conductive paste have the advantages that the silver powder is small in particle size, uniform in dispersion and extremely excellent in conductivity.
Description
Technical Field
The invention relates to the technical field of conductive paste, in particular to a preparation method of flaky silver powder and application of the flaky silver powder in the field of conductive paste.
Background
With the development of society, the sustainable utilization of energy and the concept of green environmental protection are more and more deeply focused. Solar energy has the advantages of being pollution-free and sustainable and enters the sight of people. The crystalline silicon solar cell mainly comprises a silver electrode and an aluminum back field. The silver electrode is used as a main conductive material to play an important role in the photoelectric conversion process of the crystalline silicon solar cell. Research shows that under the condition of the same quality, the flake silver powder has a higher contact area than the spherical silver powder, can coat a larger area, reduces the using amount of the silver powder, reduces the production cost and improves the photoelectric conversion efficiency. However, at present, the flake silver powder in China mainly depends on import, and the development and the application of the crystalline silicon solar cell are severely limited.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a method for preparing a fine silver powder, comprising the steps of:
1) cleaning the grinding tank by using deionized water, drying in the air, and wetting the inner wall of the grinding tank by using oleic acid;
2) adding silver powder, a dispersing agent and a grinding ball into the grinding tank, and then tightly covering the cover of the grinding tank;
3) placing the grinding tank in a ball mill for ball milling;
4) and (4) after the ball milling is finished, washing the silver powder by deionized water and ethanol, and drying the silver powder to obtain the fine silver powder.
Preferably, the silver powder is spherical silver powder, the average particle diameter of the silver powder is 8-15um, and the apparent density is 8-12g/cm 3 。
Preferably, the dispersant comprises at least one of PVP, stearic acid, oleic acid, absolute ethanol, octadecenoic acid.
Preferably, the dispersant is added in an amount of 1.2 to 1.8 wt% based on the total weight of the silver powder.
Preferably, the grinding balls comprise at least one of alumina balls, zirconia balls, stainless steel balls, hard alloy balls, polyurethane-coated iron and agate.
Preferably, the grinding balls have a diameter of 0.1 to 5.0 mm.
Preferably, the mass ratio of the silver powder to the grinding balls is (1-3): (8-15).
Preferably, the rotation speed of the ball milling is 200-300 r/min.
Preferably, the ball milling time is 18-23 h.
The second aspect of the invention provides application of a preparation method of fine silver powder in the field of conductive paste.
Has the advantages that:
the silver powder prepared by ball milling the composite dispersant consisting of PVP, oleic acid and absolute ethyl alcohol and yttrium zirconia ball grinding balls with the diameter of 0.1-5.0mm effectively solves the problems of large surface energy and easy agglomeration in the silver powder preparation process, and the prepared silver powder has small particle size and uniform dispersion and has extremely excellent conductivity and sintering performance when applied to the field of silver conductive paste. Especially when the weight ratio of the PVP to the oleic acid to the absolute ethyl alcohol is (10-15): (1-3): (5-8), the prepared silver powder has the best performance, and is particularly suitable for preparing the back silver paste of the crystalline silicon solar cell.
Detailed Description
In order to solve the problems, the invention provides a preparation method of fine silver powder, which specifically comprises the following steps:
1) cleaning the grinding tank by using deionized water, drying in the air, and wetting the inner wall of the grinding tank by using oleic acid;
2) adding silver powder, a dispersing agent and a grinding ball into the grinding tank, and then tightly covering the cover of the grinding tank;
3) placing the grinding tank in a ball mill for ball milling;
4) and (4) after the ball milling is finished, washing the silver powder by deionized water and ethanol, and drying the silver powder to obtain the fine silver powder.
Preferably, the silver powder is spherical silver powder, the average particle diameter of the silver powder is 8-15um, and the apparent density is 8-12g/cm 3 。
Preferably, the dispersant comprises at least one of PVP, stearic acid, oleic acid, absolute ethanol, octadecenoic acid.
Further preferably, the dispersant comprises PVP, oleic acid and absolute ethyl alcohol. The weight ratio of PVP, oleic acid and absolute ethyl alcohol is (10-15): (1-3): (5-8).
Preferably, the molecular weight of the PVP is 30000-150000, and the viscosity of the PVP at-25 ℃/5% aq is 1.5-8 mPa-s.
Preferably, the dispersant is added in an amount of 1.2 to 1.8 wt% based on the total weight of the silver powder.
Preferably, the grinding balls comprise at least one of alumina balls, zirconia balls, stainless steel balls, hard alloy balls, polyurethane-coated iron and agate.
Preferably, the grinding balls have a diameter of 0.1 to 5.0 mm.
Further preferably, the grinding balls have a diameter of 0.1 to 2.0 mm.
Preferably, the zirconia balls are yttrium zirconia balls.
More preferably, the content of the zirconium oxide in the yttrium zirconium oxide ball is 94-96%, and the content of the yttrium oxide is 4-6%.
Preferably, the yttrium zirconium oxide balls comprise yttrium zirconium oxide balls with the diameter of 0.1-0.3mm, yttrium zirconium oxide balls with the diameter of 0.8-1mm and yttrium zirconium oxide balls with the diameter of 1.8-2.0 mm. The yttrium zirconium oxide balls comprise yttrium zirconium oxide balls with the diameter of 0.1-0.3mm, and the number ratio of the yttrium zirconium oxide balls with the diameter of 0.8-1mm to the yttrium zirconium oxide balls with the diameter of 1.8-2.0mm is (10-15): (3-5): (1-3).
Preferably, the mass ratio of the silver powder to the grinding balls is (1-3): (8-15).
Preferably, the ball mill has a packing factor of 0.2 to 0.35.
Preferably, the rotation speed of the ball milling is 200-300 r/min.
Preferably, the ball milling time is 18-23 h.
Preferably, the washing times of the deionized water are 2-5 times, and the washing times of the absolute ethyl alcohol are 2-5 times.
Preferably, the drying temperature is 55-65 ℃, and the drying time is 10-15 h.
The second aspect of the invention provides application of a preparation method of fine silver powder in the field of conductive paste.
The present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
A preparation method of fine silver powder specifically comprises the following steps:
1) cleaning the grinding tank by using deionized water, drying in the air, and wetting the inner wall of the grinding tank by using oleic acid;
2) adding silver powder, a dispersing agent and a grinding ball into the grinding tank, and then tightly covering the cover of the grinding tank;
3) placing the grinding tank in a ball mill for ball milling;
4) and (4) after the ball milling is finished, washing the silver powder by deionized water and ethanol, and drying the silver powder to obtain the fine silver powder.
The silver powder is spherical silver powder, the average particle diameter of the silver powder is 10um, and the apparent density is 10.49g/cm 3 . Purchased from Hefei Zhonghang nanotechnology development Co., Ltd., brand: ZH-Ag20 um.
The dispersant comprises PVP, oleic acid and absolute ethyl alcohol. The weight ratio of PVP, oleic acid and absolute ethyl alcohol is 13: 1.5: 7.5. the addition amount of the dispersant accounts for 1.5 wt% of the total weight of the silver powder.
The PVP has a molecular weight of 37900, and the viscosity of the PVP at-25 ℃/5% aq is 2.1-2.7 mPa. The PVP has a moisture content of <0.5 wt%. The PVP was purchased from Gobekie corporation under the designation: PVPK 30. The water content of the oleic acid is less than or equal to 0.5 wt%. The oleic acid was purchased from ZiboHaijie chemical Co., Ltd, brand: and Y-8.
The grinding balls are zirconia balls. The zirconia ball is an yttrium zirconia ball. The content of zirconium oxide in the yttrium zirconium oxide ball is 94.7%, and the content of yttrium oxide is 5.2%. The yttrium zirconium oxide balls comprise yttrium zirconium oxide balls with the diameter of 0.2mm, yttrium zirconium oxide balls with the diameter of 1mm and yttrium zirconium oxide balls with the diameter of 2.0 mm. The yttrium zirconia balls comprise yttrium zirconia balls with the diameter of 0.2mm, and the number ratio of the yttrium zirconia balls with the diameter of 1mm to the yttrium zirconia balls with the diameter of 2.0mm is 13: 4: 2. the grinding balls were purchased from Ganzhou encyclopedia ceramics, Inc.
The mass ratio of the silver powder to the grinding balls is 2: 13. the ball mill has a packing coefficient of 0.3. The rotating speed of the ball milling is 250 r/min. The ball milling time is 20 h. The washing times of the deionized water are 3 times, and the washing times of the absolute ethyl alcohol are 3 times. The drying temperature is 60 ℃, and the drying time is 12 h.
Example 2
The specific implementation mode of the preparation method of the fine silver powder is the same as that of example 1, except that the mass ratio of the silver powder to the grinding balls is 1: 8.
example 3
The specific implementation mode of the preparation method of the fine silver powder is the same as that of example 1, except that the yttrium zirconia balls comprise 0.2 mm-diameter yttrium zirconia balls, and the number ratio of the 1 mm-diameter yttrium zirconia balls to the 2.0 mm-diameter yttrium zirconia balls is 10: 3: 1.
example 4
The specific implementation mode of the preparation method of the fine silver powder is the same as that of example 1, except that the ball milling time is 18 hours.
Comparative example 1
The specific implementation mode of the preparation method of the fine silver powder is the same as that of example 1, except that the weight ratio of PVP, oleic acid and absolute ethyl alcohol is 7: 1.5: 7.5.
comparative example 2
The specific implementation mode of the preparation method of the fine silver powder is the same as that of example 1, except that the yttrium zirconia balls comprise yttrium zirconia balls with the diameter of 1 mm.
Comparative example 3
The specific implementation mode of the preparation method of the fine silver powder is the same as that of example 1, except that the addition amount of the dispersing agent accounts for 0.7 wt% of the total weight of the silver powder.
Performance testing
1. And (3) particle size testing: and (3) testing the particle size of the silver powder by using a laser particle sizer, setting 5 parallel samples, and averaging the test results.
2. And (3) conductivity test: and (2) stirring and uniformly mixing 85 parts of silver powder, 5 parts of glass powder and 10 parts of terpineol solution with the mass fraction of 10% to obtain conductive silver paste, and then printing the conductive silver paste on a silicon substrate. Drying at 200 ℃, and sintering at 850 ℃ to obtain the silver film. The test was carried out according to GB/T1747.3-2008.
Table 1 results of performance testing
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art may modify or change the technical content of the above disclosure into equivalent embodiments with equivalent changes, but all those simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the present invention.
Claims (10)
1. The preparation method of the fine silver powder is characterized by comprising the following steps:
1) cleaning the grinding tank by using deionized water, drying in the air, and wetting the inner wall of the grinding tank by using oleic acid;
2) adding silver powder, a dispersing agent and a grinding ball into the grinding tank, and then tightly covering the cover of the grinding tank;
3) placing the grinding tank in a ball mill for ball milling;
4) and (4) after the ball milling is finished, washing the silver powder by deionized water and ethanol, and drying the silver powder to obtain the fine silver powder.
2. The method for producing a fine silver powder according to claim 1, wherein the silver powder is a spherical silver powder, the silver powder has an average particle diameter of 8 to 15 μm and a bulk density of 8 to 12g/cm 3 。
3. The method for preparing fine silver powder according to claim 1, wherein the dispersant comprises at least one of PVP, stearic acid, oleic acid, absolute ethanol, and octadecenoic acid.
4. The method for producing a fine silver powder according to claim 1 or 3, wherein the dispersant is added in an amount of 1.2 to 1.8 wt% based on the total weight of the silver powder.
5. The method for preparing fine silver powder according to claim 1, wherein the milling balls comprise at least one of alumina balls, zirconia balls, stainless steel balls, cemented carbide balls, polyurethane-coated iron, and agate.
6. The method for producing a fine silver powder according to claim 1 or 5, wherein the grinding balls have a diameter of 0.1 to 5.0 mm.
7. The method for producing a fine silver powder according to any one of claims 1 to 6, wherein the ratio by mass of the silver powder to the milling balls is (1-3): (8-15).
8. The method for preparing fine silver powder according to claim 1, wherein the rotation speed of the ball mill is 200-300 r/min.
9. The method for preparing fine silver powder according to claim 1, wherein the ball milling time is 18 to 23 hours.
10. Use of a method for producing a fine silver powder according to any one of claims 1 to 9 in the field of electroconductive pastes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110671235.3A CN114799181A (en) | 2021-06-17 | 2021-06-17 | Preparation method of flaky silver powder and application of flaky silver powder in field of conductive paste |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110671235.3A CN114799181A (en) | 2021-06-17 | 2021-06-17 | Preparation method of flaky silver powder and application of flaky silver powder in field of conductive paste |
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| CN114799181A true CN114799181A (en) | 2022-07-29 |
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| CN202110671235.3A Withdrawn CN114799181A (en) | 2021-06-17 | 2021-06-17 | Preparation method of flaky silver powder and application of flaky silver powder in field of conductive paste |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114939667A (en) * | 2021-06-16 | 2022-08-26 | 河南金渠银通金属材料有限公司 | Preparation method of micron-sized silver powder and application of micron-sized silver powder in filter |
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2021
- 2021-06-17 CN CN202110671235.3A patent/CN114799181A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114939667A (en) * | 2021-06-16 | 2022-08-26 | 河南金渠银通金属材料有限公司 | Preparation method of micron-sized silver powder and application of micron-sized silver powder in filter |
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Application publication date: 20220729 |
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