CN108326292B - Metal-coated composite powder electroplating process - Google Patents
Metal-coated composite powder electroplating process Download PDFInfo
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- CN108326292B CN108326292B CN201711362737.8A CN201711362737A CN108326292B CN 108326292 B CN108326292 B CN 108326292B CN 201711362737 A CN201711362737 A CN 201711362737A CN 108326292 B CN108326292 B CN 108326292B
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
Abstract
The invention discloses a metal-coated composite powder electroplating process in the technical field of core-shell material production processes, and aims to solve the technical problems of low deposition rate, rough coating, no density and powder agglomeration in the prior art; the process comprises the following steps: firstly, preparing a degreasing agent, degreasing the conductive powder and preparing a plating solution; then injecting the prepared plating solution and the deoiled conductive powder into the outer cavity of the plating bath; then adding powdery plating metal into the inner cavity of the electroplating bath; then starting a circulating pump to circulate the plating solution and starting a power supply for electroplating; finally, filtering out powder, washing with water and passivating. The invention can conveniently and cheaply coat a layer of metal phase outside the conductive powder to form a well-combined core-shell type composite material, and the process has the advantages of high deposition rate, smooth and compact coating.
Description
Technical Field
The invention relates to the technical field of core-shell material production processes, in particular to a metal-coated composite powder electroplating process.
Background
The metal-coated composite powder is a novel multiphase composite powder metallurgy material, has various varieties and unique performance, and is widely used in the fields of national defense industry, mechanical manufacturing, chemical chemistry and the like. The metal-coated composite powder can be roughly classified into three types, namely a metal-carbon material, a metal-ceramic material and a metal-metal material, according to the difference of core-shell structures.
The preparation method of the metal-coated composite powder generally comprises the following steps of ball milling, dipping, sol-gel method, coprecipitation method, chemical plating, electroplating and the like. The ball milling method is simple, the content of metal in the powder is easy to control, but the coated composite powder, especially the superfine powder, is difficult to form and is difficult to mix uniformly; although the sol-gel method can uniformly disperse, the composite powder prepared from the solution is a metal oxide and needs to be reduced at a higher temperature, and the process is complicated, particles are easy to grow up in the reduction process, and fine powder is difficult to prepare; impregnation and coprecipitation methods generally only allow powders with low metal content to be obtained; the chemical plating and electroplating are widely applied, the uniformity of metal coating in the prepared powder is better, but the chemical plating pretreatment process is complex, the plating solution is unstable, the components of the plating solution are complex, and the preparation cost is high. Compared with chemical plating, the electroplating has the advantages of faster deposition speed, good stability of plating solution, low cost, more environmental friendliness, high metal coating rate on the surface of the powder and the like.
However, when the existing electroplating device is used for preparing the metal-coated composite powder, the problems of low deposition rate, rough coating, non-density, powder agglomeration and the like generally exist.
Disclosure of Invention
In view of the above, the present invention provides a metal-coated composite powder electroplating process to solve the technical problems of low deposition rate, rough coating, non-dense coating and powder agglomeration in the prior art.
The technical scheme adopted by the invention is as follows:
a metal-coated composite powder electroplating process is designed, and comprises the following steps:
s1 pretreatment for plating: preparing a degreasing agent, a plating solution and degreasing the conductive powder;
s2 electroplating: injecting the plating solution prepared in the step S1 and the deoiled conductive powder into an outer cavity of the electroplating bath; adding powdery plating metal into an inner cavity of the electroplating bath, wherein the inner cavity of the electroplating bath and an outer cavity of the electroplating bath are separated by a water-permeable ceramic film; then starting a circulating pump to circulate the plating solution between the plating bath outer cavity and the liquid storage tank and starting a power supply to carry out plating;
s3 post-plating treatment: filtering out powder, washing with water and passivating.
Preferably, the plating solution in step S1 is prepared from 0.9-1.3mol/L copper sulfate, silver nitrate or nickel sulfate, 1-12mmol/L sulfuric acid, 5-30mmol/L glacial acetic acid, 0.2-1.5g/L emulsifier OP-10, 15-35g/L glyoxylic acid and water.
Preferably, the plating solution in step S1 is prepared from 1.0-1.2mol/L copper sulfate or nickel sulfate, 4-8mmol/L sulfuric acid, 19-25mmol/L glacial acetic acid, 0.5-0.8g/L emulsifier OP-10, 15-30g/L glyoxylic acid and water.
Preferably, the plating solution in step S1 is prepared from 1.0mol/L silver nitrate, 5mmol/L sulfuric acid, 5mmol/L glacial acetic acid, 0.2g/L emulsifier OP-10, 15g/L glyoxylic acid and water.
Preferably, the plating solution in step S1 is prepared from 1.0mol/L nickel sulfate, 1mmol/L sulfuric acid, 8mmol/L glacial acetic acid, 0.5g/L emulsifier OP-10, 25g/L glyoxylic acid and water.
Preferably, the loading amount of the conductive powder in the step S2 is 10-100 g/L; the current density during electroplating is 10-30A/dm2The electroplating time is 2-3 h.
Preferably, the loading amount of the conductive powder in the step S2 is 50 g/L; the current density during electroplating is 20A/dm2The plating time is 2.5 h.
Preferably, when the metal cation content in the plating solution is insufficient, the inner cavity is replenished with the powdered plating metal.
Preferably, the powdered plating metal is any one of copper, nickel and silver.
Preferably, the conductive powder is any one of graphite powder, coke powder and metal powder.
Compared with the prior art, the invention has the beneficial technical effects that:
1. the invention can conveniently and cheaply coat a layer of metal phase (copper, nickel and silver) outside the conductive powder (graphite powder, coke powder and metal powder) to form a well-combined core-shell type composite material.
2. The invention replaces the anode bar with the powder coating metal, which is beneficial to the supplement of the positive ions in the plating solution, especially in the plating process, when the positive ions of the plating solution are seriously insufficient, the plating is not required to be interrupted and the anode bar is drawn out for replacement, only the powder coating metal is required to be supplemented into the inner cavity, and due to the obstruction of the permeable ceramic film, the coating powder is convenient to recover and cannot enter the liquid storage tank.
3. According to the invention, glyoxylic acid is added into the plating solution, and through the reduction action of the glyoxylic acid, the powder can quickly form metal crystal nuclei on the surface of the powder during electroplating, so that the quick growth and compaction of metal crystals on the surface of the powder are facilitated, and the electrodeposition speed is high, and the plating layer is smooth and compact.
Drawings
FIG. 1 is a schematic structural view of an electroplating apparatus;
FIG. 2 is a schematic view of the electroplating bath structure;
FIG. 3 is a flow chart of the present invention;
the device comprises a plating bath 1, a circulating pump 2, a flow meter 3, a liquid storage tank 4, a power supply 5, an ultrasonic vibrator 6, powdered copper 7, a liquid discharge port 11, a conductive shell 12, a water-permeable ceramic film 13, a liquid inlet 14, an outer cavity 15, an inner cavity 16 and a material supplementing port 17.
Detailed Description
The following examples are intended to illustrate the present invention in detail and should not be construed as limiting the scope of the present invention in any way. The components, structures, mechanisms and the like in the following examples are all conventional commercially available products unless otherwise specified.
Example 1: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of copper-coated graphite powder as an example, as shown in fig. 3, and includes the following specific operation steps:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of graphite powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out the graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the powder when in contact with the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.1mol/L of copper sulfate, 12mmol/L of sulfuric acid, 20mmol/L of glacial acetic acid, 101.5 g/L of emulsifier OP-20 g/L of glyoxylic acid.
Electroplating:
adding the prepared plating solution and the graphite powder after oil removal into an outer cavity of the plating bath, wherein the loading capacity of the graphite powder is 50g/L, adding copper powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 20A/dm2And electroplating for 2 h. In the electroplating process, when the obvious consumption of the copper powder in the inner cavity cannot be seen, the powder-shaped plating metal needs to be supplemented into the inner cavity.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 30min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the washed powder at the temperature of 60 ℃.
Example 2: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of copper-coated graphite powder as an example, as shown in fig. 3, and includes the following specific operation steps:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of graphite powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out the graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the powder when in contact with the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.2mol/L of copper sulfate, 8mmol/L of sulfuric acid, 25mmol/L of glacial acetic acid, 100.8 g/L of emulsifier OP-100, and 26g/L of glyoxylic acid.
Electroplating:
adding the prepared plating solution and the graphite powder after oil removal into an outer cavity of the plating bath, wherein the loading capacity of the graphite powder is 10g/L, adding copper powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, turning on the DC power supply to supply electricityThe flow density is adjusted to 10A/dm2And electroplating for 2 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 25min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the washed powder at the temperature of 60 ℃.
Example 3: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of copper-coated graphite powder as an example, as shown in fig. 3, and includes the following specific operation steps:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of graphite powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out the graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the powder when in contact with the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.0mol/L copper sulfate, 6mmol/L sulfuric acid, 19mmol/L glacial acetic acid, 100.7 g/L emulsifier OP-100, 30g/L glyoxylic acid.
Electroplating:
adding the prepared plating solution and the graphite powder after oil removal into an outer cavity of the plating bath, wherein the loading capacity of the graphite powder is 100g/L, adding copper powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 30A/dm2And electroplating for 3 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 30min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the washed powder at the temperature of 60 ℃.
Example 4: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of copper-coated graphite powder as an example, as shown in fig. 3, and includes the following specific operation steps:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of graphite powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out the graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the powder when in contact with the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.3mol/L of copper sulfate, 8mmol/L of sulfuric acid, 19mmol/L of glacial acetic acid, 100.5 g/L of emulsifier OP-100, and 15g/L of glyoxylic acid.
Electroplating:
adding the prepared plating solution and the deoiled graphite powder into an outer cavity of the plating bath, wherein the loading capacity of the graphite powder is 30g/L, adding copper powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 15A/dm2And electroplating for 2 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 25min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the washed powder at the temperature of 60 ℃.
Example 5: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of copper-coated graphite powder as an example, as shown in fig. 3, and includes the following specific operation steps:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of graphite powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out the graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the powder when in contact with the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 0.9mol/L of copper sulfate, 5mmol/L of sulfuric acid, 20mmol/L of glacial acetic acid, 100.6 g/L of emulsifier OP-100, and 35g/L of glyoxylic acid.
Electroplating:
adding the prepared plating solution and the graphite powder after oil removal into an outer cavity of the plating bath, wherein the loading capacity of the graphite powder is 70g/L, adding copper powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 25A/dm2And electroplating for 3 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 25min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the washed powder at the temperature of 60 ℃.
Example 6: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of copper-coated coke powder as an example, and as shown in fig. 3, the specific operation steps are as follows:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of coke powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the coke powder when contacting the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.1mol/L of copper sulfate, 4mmol/L of sulfuric acid, 30mmol/L of glacial acetic acid, OP-101 g/L of emulsifier and 30g/L of glyoxylic acid.
Electroplating:
adding the prepared plating solution and the deoiled coke powder into an outer cavity of the plating bath, wherein the loading capacity of the coke powder is 80g/L, adding copper powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to circulate the plating solution between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 20A/dm2And electroplating for 2.5 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 30min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the powder at the temperature of 60 ℃.
Example 7: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of copper-coated metal powder as an example, as shown in fig. 3, the specific operation steps are as follows:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of metal powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out the metal powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the metal powder when in contact with the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.2mol/L of copper sulfate, 3mmol/L of sulfuric acid, 10mmol/L of glacial acetic acid, 100.2 g/L of emulsifier OP-100, and 15g/L of glyoxylic acid.
Electroplating:
adding the prepared plating solution and the deoiled metal powder into an outer cavity of the plating bath, wherein the loading capacity of the metal powder is 50g/L, adding copper powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 20A/dm2And electroplating for 2.5 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 30min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the powder at the temperature of 60 ℃.
Example 8: a metal-coated composite powder electroplating process, which is described in this embodiment by taking preparation of nickel-coated coke powder as an example, and as shown in fig. 3, the specific operation steps are as follows:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of coke powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the coke powder when contacting the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.0mol/L of nickel sulfate, 1mmol/L of sulfuric acid, 8mmol/L of glacial acetic acid, 100.5 g/L of emulsifier OP-100, and 25g/L of glyoxylic acid.
Electroplating:
adding the prepared plating solution and the deoiled coke powder into an outer cavity of the plating bath, wherein the loading capacity of the coke powder is 100g/L, adding the nickel powder into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 20A/dm2And electroplating for 2.5 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 30min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the powder at the temperature of 60 ℃.
Example 9: a metal-coated composite powder electroplating process, which is described in this embodiment by taking the preparation of silver-coated graphite powder as an example, as shown in fig. 3, the specific operation steps are as follows:
pre-plating treatment:
oil removal: preparing a degreasing agent containing 150g/L of sodium hydroxide, 30g/L of sodium carbonate, 35g/L of sodium phosphate and water, adding 100g of graphite powder into the degreasing agent, stirring for 30min at the temperature of 60 ℃, filtering out the graphite powder, washing with deionized water, and drying for later use.
Degreasing can reduce the surface tension of the graphite powder when contacting with the plating solution.
Preparing a plating solution: the plating solution is prepared from the following substances in percentage by weight: 1.0mol/L silver nitrate, 5mmol/L glacial acetic acid, 100.2 g/L emulsifier OP-and 15g/L glyoxylic acid.
Electroplating:
adding the prepared plating solution and the graphite powder after oil removal into an outer cavity of the plating bath, wherein the loading capacity of the graphite powder is 100g/L, adding the powdery plating metal into the inner cavity of the plating bath, starting an external circulating pump, and adjusting a flowmeter to enable the plating solution to circulate between the plating bath and a liquid storage tank.
Starting the ultrasonic vibrator, starting the direct current power supply, and adjusting the current density to 20A/dm2And electroplating for 2.5 h.
And (3) post-plating treatment:
and after the electroplating is finished, taking out the metal-coated powder, washing the metal-coated powder by using deionized water, adding the metal-coated powder into a benzotriazole solution for passivation for 30min, then carrying out suction filtration on the passivated powder, washing the powder, and drying the powder at the temperature of 60 ℃.
An electroplating apparatus used in the implementation of embodiments 1 to 9, as shown in fig. 1 to 2, includes a circulation pump 2, a liquid storage tank 4, an electroplating bath 1 and a flow meter 3, wherein a conductive housing 12 (made of stainless steel) is provided outside the electroplating bath 1, a water permeable ceramic film 13 is provided inside the electroplating bath 1 to form an inner cavity 16 and an outer cavity 15 inside the electroplating bath 1, the upper portion of the electroplating bath 1 is cylindrical and is provided with a liquid discharge port 11, the lower portion thereof is conical and is provided with a liquid inlet 14 for the entry and discharge of the electroplating solution, the liquid discharge port 11 is communicated with the top of the liquid storage tank 4, and the liquid inlet 14, the flow meter 3, the circulation pump 2 and; the top of the electroplating bath 1 is also provided with a feeding port 17 for feeding the powder copper 7 into the inner cavity 16.
The device also comprises a power supply 5 (direct current power supply), wherein the negative electrode connecting end of the power supply 5 is electrically connected with the conductive shell 12, the positive electrode connecting end extends into the inner cavity 16 so that the plating solution, the conductive shell 12 and the power supply 5 form a loop, the conductive shell 12 is used as a cathode to reduce metal cations during electroplating, and the powder copper 7 of the inner cavity 16 is used as an anode to precipitate the metal cations during electroplating.
Two pairs of ultrasonic vibrators 6 are symmetrically arranged on the conductive shell 12, and conductive powder particles adhered to the surface of the cathode are returned to the plating solution again through the ultrasonic vibrators, so that excessive deposition of plating metal on the surface of the conductive powder is prevented, and the plating layer is compact and uniform.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A metal-coated composite powder electroplating process is characterized by comprising the following steps:
s1 pretreatment for plating: preparing a degreasing agent, a plating solution and degreasing the conductive powder;
s2 electroplating: injecting the plating solution prepared in the step S1 and the deoiled conductive powder into an outer cavity of the electroplating bath; adding powdery plating metal into an inner cavity of the electroplating bath, wherein the inner cavity of the electroplating bath and an outer cavity of the electroplating bath are separated by a water-permeable ceramic film; then starting a circulating pump to circulate the plating solution between the plating bath outer cavity and the liquid storage tank and starting a power supply to carry out plating;
s3 post-plating treatment: filtering out powder, washing with water and passivating.
2. The electroplating process of claim 1, wherein: the plating solution in the step S1 is prepared by 0.9-1.3mol/L of copper sulfate or silver nitrate or nickel sulfate, 1-12mmol/L of sulfuric acid, 5-30mmol/L of glacial acetic acid, 0.2-1.5g/L of emulsifier OP-10, 15-35g/L of glyoxylic acid and water.
3. The electroplating process according to claim 2, wherein: the plating solution in the step S1 is prepared by 1.0-1.2mol/L of copper sulfate or nickel sulfate, 4-8mmol/L of sulfuric acid, 19-25mmol/L of glacial acetic acid, 0.5-0.8g/L of emulsifier OP-10, 15-30g/L of glyoxylic acid and water.
4. The electroplating process according to claim 2, wherein: in the step S1, the plating solution is prepared from 1.0mol/L silver nitrate, 5mmol/L sulfuric acid, 5mmol/L glacial acetic acid, 0.2g/L emulsifier OP-10, 15g/L glyoxylic acid and water.
5. The electroplating process according to claim 2, wherein: in the step S1, the plating solution is prepared from 1.0mol/L nickel sulfate, 1mmol/L sulfuric acid, 8mmol/L glacial acetic acid, 0.5g/L emulsifier OP-10, 25g/L glyoxylic acid and water.
6. The electroplating process of claim 1, wherein: the loading amount of the conductive powder in the step S2 is 10-100 g/L; the current density during electroplating is 10-30A/dm2The electroplating time is 2-3 h.
7. The electroplating process of claim 1, wherein: the loading amount of the conductive powder in the step S2 is 50 g/L; the current density during electroplating is 20A/dm2The plating time is 2.5 h.
8. The electroplating process of claim 1, wherein: when the metal cation content in the plating solution is insufficient, the inner cavity is supplemented with powdery plating metal.
9. The electroplating process of claim 8, wherein: the powdery plating metal is any one of copper, nickel and silver.
10. The electroplating process of claim 1, wherein: the conductive powder is any one of graphite powder, coke powder and metal powder.
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| CN108070895B (en) * | 2017-12-18 | 2024-02-02 | 开封平煤新型炭材料科技有限公司 | Metal cladding type composite powder electroplating device |
| CN109909496B (en) * | 2019-01-26 | 2021-01-05 | 北京工业大学 | Environment-friendly silver electrochemical coating method for aluminum powder |
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| JP6121090B2 (en) * | 2011-05-10 | 2017-04-26 | 三菱マテリアル株式会社 | Method for producing stannous oxide powder for replenishing Sn component to Sn alloy plating solution and stannous oxide powder produced by the method |
| CN104368808B (en) * | 2014-10-15 | 2017-03-01 | 中国科学院过程工程研究所 | A kind of copper clad molybdenum composite granule of thickness uniform, controllable, preparation method and its usage |
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