CN111360246A - Silver-coated copper powder with high coating rate and excellent quality and preparation method thereof - Google Patents
Silver-coated copper powder with high coating rate and excellent quality and preparation method thereof Download PDFInfo
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- CN111360246A CN111360246A CN202010332700.6A CN202010332700A CN111360246A CN 111360246 A CN111360246 A CN 111360246A CN 202010332700 A CN202010332700 A CN 202010332700A CN 111360246 A CN111360246 A CN 111360246A
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- copper powder
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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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
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
- C23C18/44—Coating with noble metals using reducing agents
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- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses silver-coated copper powder with high coating rate and excellent quality and a preparation method thereof, wherein the preparation method of the silver-coated copper powder with excellent conductivity comprises the steps of preparing a main salt solution, preparing a reducing solution, pretreating copper powder, coating silver, washing with water, draining, screening and packaging‑4Omega cm, excellent conductivity and good shielding performance.
Description
Technical Field
The invention relates to the technical field of silver-coated copper powder, in particular to silver-coated copper powder with high coating rate and excellent quality and a preparation method thereof.
Background
With the rapid development of electronics, information and traffic industries, the miniaturization, sheet formation, multilayering and other processes of electronic components are increasingly accelerated, and the demand for electronic paste (conductive paint and conductive adhesive) using metal powder such as silver, gold, platinum, nickel, copper and the like as main functional phases is increasing. The electronic paste is widely applied to electrodes of resistors, capacitors, inductors and the like, shielding coatings for preventing electromagnetic interference and the like. Silver powder is an excellent conductive filler, but is expensive; copper powder is cheap, but is easy to oxidize and has poor stability. If a layer of silver particles is uniformly coated on the surface of the copper powder to obtain the silver-coated copper powder, the excellent conductivity of the copper powder can be maintained, the oxidation resistance stability of the copper powder is improved, and the cost can be reduced. However, the silver wrapping layer in the existing silver-coated copper powder is not wrapped uniformly and completely, so that the existing silver-coated copper powder is poor in conductivity and cannot meet the shielding requirement.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects in the prior art, and provides silver-coated copper powder with high coating rate and excellent quality and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of silver-coated copper powder with high coating rate and excellent quality comprises the following steps:
s1, preparing a main salt solution, adding silver nitrate into distilled water, and obtaining a silver nitrate solution after the silver nitrate is completely dissolved; then slowly adding ammonia water with the concentration of 25.0-28.0 wt% while stirring the silver nitrate solution to enable the silver nitrate solution to be a transparent precipitate-free liquid, then adding sodium hydroxide, and continuously adding the ammonia water until the solution is clear, so that the preparation of the main salt solution is finished; the mass concentration of silver nitrate in the main salt solution is 25.0-45.0 g/L, and the mass concentration of sodium hydroxide is 3.0-5.0 g/L;
s2, preparing a reducing solution, and sequentially adding glucose and tartaric acid into distilled water to prepare the reducing solution; the mass concentration of glucose in the reducing solution is 15.0-25.0 g/L, and the mass concentration of tartaric acid is 1.5-2.5 g/L;
s3, pretreating copper powder, adding the copper powder into a dilute sulfuric acid solution with the concentration of 3.0-10.0 wt% at a constant speed, stirring the mixed solution after adding the copper powder, pickling the copper powder, repeatedly washing the pickled copper powder with deionized water, and drying the copper powder in the shade for later use;
s4, coating with silver, namely putting the copper powder prepared in the step S3 into the reducing solution prepared in the step S2, and stirring for 2-5 min to obtain a mixed solution; adding a main salt solution into the mixed solution, quickly adding the main salt solution, slowly adding the main salt solution when the pH of the mixed solution is 11, and carrying out chemical silver plating to obtain a finished product mixed solution, wherein the whole chemical silver plating reaction adopts a water bath method, the temperature is 55-65 ℃, and the chemical silver plating time is 25-40 min; the mass ratio of the copper powder to the reducing solution to the main salt solution is 1: (15-20): (15-20);
s4, washing with water, draining, washing the powder prepared in the step S4 with deionized water, carrying out solid-liquid separation on the finished product mixed solution obtained in the step S4, filtering to obtain powder, and drying in vacuum to obtain the silver-coated copper powder with high coating rate and excellent quality;
and S5, screening and packaging, wherein after the silver-coated copper powder prepared in the S5 is screened by a vibrating screen, qualified products are packaged to obtain finished products.
In S4, the reaction mechanism of adding the main salt solution quickly and then slowly is as follows: the main salt solution is added at a higher speed when the chemical silver plating reaction is started, the concentration of the main salt is improved, a good alkaline environment is provided for the reduction solution, the reaction rate of silver plating is higher, the chemical balance can be pushed to move to the right, and the conversion rate of silver ions is improved. Because heterogeneous surface nucleation is prior to in-phase nucleation, a large amount of silver particles initially separated out in the reaction can be continuously nucleated and accumulated on the surface of the copper powder to form a coating on the surface of the copper powder, which is beneficial to forming a continuous and uniform coating after the main salt solution is slowly added subsequently. When the pH of the mixed solution is 11, continuously adding the main salt solution at a slow speed, gradually increasing the silver particles on the surface of the copper powder in the deposition process of the silver-coated copper powder coating at the stage, and gradually growing the coating. With the continuous addition of the main salt, the reduced silver particles are continuously deposited on the surface of the copper powder, the silver plating amount is gradually increased, and the silver plating layer grows in an extending mode. The silver coating uniformly and completely wraps the copper powder.
Further, the pickling time of the copper powder in the S3 is 8-15 min, and the pickling temperature is room temperature.
Further, the ratio of the fast addition speed to the slow addition speed in the step S4 is (7-8): 1.
in S3, the copper powder is flake copper powder, spherical copper powder or dendritic copper powder.
The silver-coated copper powder with excellent conductivity is prepared by the preparation method.
The invention has the beneficial effects that: the method has the advantages of reasonable design and simple and convenient operation, the main salt solution is quickly added in the silver coating reaction, then the main salt solution is slowly added, the silver-coated layer uniformly and completely coats the copper powder, and the particle size of the prepared silver-coated copper powder is divided intoThe cloth is concentrated, the wrapping performance is excellent, and the volume resistivity of the silver-coated copper powder is lower than 1.9 × 10-4Omega cm, excellent conductivity, good shielding performance and excellent quality.
Detailed Description
The present invention will now be described in further detail with reference to preferred embodiments.
Example 1
A preparation method of silver-coated copper powder with high coating rate and excellent quality comprises the following steps:
s1, preparing a main salt solution, adding silver nitrate into distilled water, and obtaining a silver nitrate solution after the silver nitrate is completely dissolved; then slowly adding ammonia water with the concentration of 25.0 wt% while stirring the silver nitrate solution to enable the silver nitrate solution to be a transparent precipitate-free liquid, then adding sodium hydroxide, and continuously adding the ammonia water until the solution is clear, thus completing the preparation of the main salt solution; the mass concentration of silver nitrate in the main salt solution is 25.0g/L, and the mass concentration of sodium hydroxide is 3.0 g/L;
s2, preparing a reducing solution, and sequentially adding glucose and tartaric acid into distilled water to prepare the reducing solution; the mass concentration of glucose in the reducing solution is 15.0g/L, and the mass concentration of tartaric acid is 1.5 g/L;
s3, copper powder pretreatment, namely adding flaky copper powder into a dilute sulfuric acid solution with the concentration of 3.0 percent by weight at a constant speed, stirring the mixed solution after adding the flaky copper powder, and carrying out acid pickling on the flaky copper powder for 8 min; then repeatedly washing the flake copper powder after the acid washing by using deionized water, and drying the flake copper powder in the shade for later use;
s4, coating silver, namely putting 6Kg of flake copper powder prepared in the step S3 into the reducing solution prepared in the step S2, wherein 90Kg of the reducing solution is adopted, and stirring for 2min to obtain a mixed solution; adding a main salt solution into the mixed solution, wherein the main salt solution is added at a speed of 25L/min by adopting 90Kg, and when the pH of the mixed solution is 11, the main salt solution is added at a speed of 3L/min for chemical plating to obtain a finished product mixed solution, and the whole chemical plating reaction adopts a water bath method, the temperature is 55 ℃, and the chemical plating time is 25 min;
s4, washing with water, draining, washing the powder prepared in the step S4 with deionized water, carrying out solid-liquid separation on the finished product mixed solution obtained in the step S4, filtering to obtain powder, and drying in vacuum to obtain the silver-coated copper powder with high coating rate and excellent quality;
and S5, screening and packaging, wherein after the silver-coated copper powder prepared in the S5 is screened by a vibrating screen, qualified products are packaged to obtain finished products.
Example 2
The method for preparing the silver-coated copper powder with high coating rate and excellent quality is different from the method in example 1 in that:
s3, copper powder pretreatment, namely adding spherical copper powder into a dilute sulfuric acid solution with the concentration of 6.0 percent by weight at a constant speed, stirring the mixed solution after adding the spherical copper powder, and carrying out acid pickling on the spherical copper powder for 12 min; then, repeatedly washing the spherical copper powder after acid washing by using deionized water, and drying the spherical copper powder in the shade for later use;
s4, coating silver, namely putting 6Kg of spherical copper powder prepared in the step S3 into the reducing solution prepared in the step S2, wherein 120Kg of the reducing solution is adopted, and stirring for 3min to obtain a mixed solution; and adding a main salt solution into the mixed solution, wherein the main salt solution is added at a speed of 28L/min by adopting 100Kg, and when the pH of the mixed solution is 11, the main salt solution is added at a speed of 3.5L/min for chemical plating to obtain a finished product mixed solution, and the whole chemical plating reaction adopts a water bath method, the temperature is 60 ℃, and the chemical plating time is 35 min.
Example 3
The method for preparing the silver-coated copper powder with high coating rate and excellent quality is different from the method in example 1 in that:
s3, copper powder pretreatment, namely adding the dendritic copper powder into a dilute sulfuric acid solution with the concentration of 10.0 wt% at a constant speed, stirring the mixed solution after adding the dendritic copper powder, and carrying out acid washing on the dendritic copper powder for 15 min; then repeatedly washing the acid-washed dendritic copper powder by using deionized water, and drying the dendritic copper powder in the shade for later use;
s4, coating silver, namely putting 6Kg of dendritic copper powder prepared in the step S3 into the reducing solution prepared in the step S2, wherein 100Kg of the reducing solution is adopted, and stirring for 5min to obtain a mixed solution; and adding a main salt solution into the mixed solution, wherein the main salt solution is added at a speed of 35L/min by adopting 120Kg, and when the pH of the mixed solution is 11, the main salt solution is added at a speed of 4L/min for chemical plating to obtain a finished product mixed solution, wherein the whole chemical plating reaction adopts a water bath method, the temperature is 65 ℃, and the chemical plating time is 40 min.
The silver-coated copper powders having high coating rates and excellent qualities prepared in examples 1 to 3 were subjected to performance tests, and the respective performances were measured according to the national standards, and the test results are shown in table 1.
TABLE 1 Performance test results for silver-coated copper powders prepared in examples 1-3
In conclusion, the method has reasonable design and simple and convenient operation, the main salt solution is quickly added in the silver coating reaction and then slowly added, the silver coating layer uniformly and completely coats the copper powder, the particle size distribution of the prepared silver-coated copper powder is concentrated, and the volume resistivity of the silver-coated copper powder is lower than 1.9 × 10-4Omega cm, excellent conductivity, good shielding performance and excellent quality.
While particular embodiments of the present invention have been described in the foregoing specification, various modifications and alterations to the previously described embodiments will become apparent to those skilled in the art from this description without departing from the spirit and scope of the invention.
Claims (5)
1. A preparation method of silver-coated copper powder with high coating rate and excellent quality is characterized by comprising the following steps: comprises the following steps:
s1, preparing a main salt solution, adding silver nitrate into distilled water, and obtaining a silver nitrate solution after the silver nitrate is completely dissolved; then slowly adding ammonia water with the concentration of 25.0-28.0 wt% while stirring the silver nitrate solution to enable the silver nitrate solution to be a transparent precipitate-free liquid, then adding sodium hydroxide, and continuously adding the ammonia water until the solution is clear, so that the preparation of the main salt solution is finished; the mass concentration of silver nitrate in the main salt solution is 25.0-45.0 g/L, and the mass concentration of sodium hydroxide is 3.0-5.0 g/L;
s2, preparing a reducing solution, and sequentially adding glucose and tartaric acid into distilled water to prepare the reducing solution; the mass concentration of glucose in the reducing solution is 15.0-25.0 g/L, and the mass concentration of tartaric acid is 1.5-2.5 g/L;
s3, pretreating copper powder, adding the copper powder into a dilute sulfuric acid solution with the concentration of 3.0-10.0 wt% at a constant speed, stirring the mixed solution after adding the copper powder, pickling the copper powder, repeatedly washing the pickled copper powder with deionized water, and drying the copper powder in the shade for later use;
s4, coating with silver, namely putting the copper powder prepared in the step S3 into the reducing solution prepared in the step S2, and stirring for 2-5 min to obtain a mixed solution; adding a main salt solution into the mixed solution, quickly adding the main salt solution, slowly adding the main salt solution when the pH of the mixed solution is 11, and carrying out chemical silver plating to obtain a finished product mixed solution, wherein the whole chemical silver plating reaction adopts a water bath method, the temperature is 55-65 ℃, and the chemical silver plating time is 25-40 min; the mass ratio of the copper powder to the reducing solution to the main salt solution is 1: (15-20): (15-20);
s4, washing with water, draining, washing the powder prepared in the step S4 with deionized water, carrying out solid-liquid separation on the finished product mixed solution obtained in the step S4, filtering to obtain powder, and drying in vacuum to obtain the silver-coated copper powder with high coating rate and excellent quality;
and S5, screening and packaging, wherein after the silver-coated copper powder prepared in the S5 is screened by a vibrating screen, qualified products are packaged to obtain finished products.
2. The method for producing silver-coated copper powder excellent in electric conductivity according to claim 1, characterized in that: and the pickling time of the copper powder in the S3 is 8-15 min, and the pickling temperature is room temperature.
3. The method for producing a silver-coated copper powder having a high coating rate and excellent quality according to claim 1, characterized in that: and the ratio of the rapid adding speed to the slow adding speed in the S4 is (7-8): 1.
4. the method for producing a silver-coated copper powder having a high coating rate and excellent quality according to claim 1, characterized in that: the copper powder in the S3 is flake copper powder, spherical copper powder or dendritic copper powder.
5. A silver-coated copper powder having a high coating rate and excellent quality, which is produced by the production method according to any one of claims 1 to 4.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112935246A (en) * | 2021-01-27 | 2021-06-11 | 刘勤华 | Integrated device for processing superfine silver-coated copper composite powder material |
| CN112935244A (en) * | 2021-01-27 | 2021-06-11 | 刘勤华 | Silver-coated copper composite powder process for photovoltaic use and replacing pure silver slurry |
| CN115805310A (en) * | 2023-01-17 | 2023-03-17 | 苏州星翰新材料科技有限公司 | Silver-coated copper powder, preparation method, application in silver-coated copper slurry and method for detecting compactness of silver-coated layer in silver-coated copper powder |
| CN116117136A (en) * | 2023-02-16 | 2023-05-16 | 安靖盛(江苏)电子新材料有限公司 | Silver-coated copper powder and application thereof |
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| CN112935244A (en) * | 2021-01-27 | 2021-06-11 | 刘勤华 | Silver-coated copper composite powder process for photovoltaic use and replacing pure silver slurry |
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| CN116117136A (en) * | 2023-02-16 | 2023-05-16 | 安靖盛(江苏)电子新材料有限公司 | Silver-coated copper powder and application thereof |
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Application publication date: 20200703 |