CN110983393A - Silver-niobium carbide composite coating and preparation method thereof - Google Patents
Silver-niobium carbide composite coating and preparation method thereof Download PDFInfo
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- CN110983393A CN110983393A CN201911380386.2A CN201911380386A CN110983393A CN 110983393 A CN110983393 A CN 110983393A CN 201911380386 A CN201911380386 A CN 201911380386A CN 110983393 A CN110983393 A CN 110983393A
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/64—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of silver
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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
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
Abstract
The application belongs to the technical field of composite electroplating coatings, and particularly relates to a silver-niobium carbide composite coating and a preparation method thereof. The application provides a preparation method of a silver-niobium carbide composite coating, which comprises the following steps: step 1, using NbCl5Taking Nb and carbon black as reactants, carrying out heating reaction on the reactants and chloride salt, and then washing to obtain nano niobium carbide powder; step 2, mixing the nano niobium carbide powder with a plating solution to obtain an electroplating solution, wherein the plating solution comprises a water-soluble silver-containing compound, succinimide, potassium pyrophosphate, a dispersant and an acid-base regulator; and 3, electroplating the base material in the electroplating solution to obtain the silver-niobium carbide composite coating. The application provides a silver-niobium carbide composite coating and a preparation method thereof, which can effectively solve the problem of the existing silver coatingCannot simultaneously have the technical defects of wear resistance, corrosion resistance, electrical conductivity and thermal conductivity.
Description
Technical Field
The application belongs to the technical field of composite coatings, and particularly relates to a silver-niobium carbide composite coating and a preparation method thereof.
Background
The isolation switch device is most prone to generate heat during field operation, which not only causes the reduction of the through-current capacity of the device, but also causes greater harm to the operation safety of the power grid if the device cannot be processed in time. The heating defect is mainly caused by that the silver coating on the surface of the moving contact and the static contact of the isolating switch is abraded due to the increase of the switching-on and switching-off times of the switch, even copper is polished and leaked, and then the contact resistance on the surface of the contact is increased, and the electric quantity loss is increased. In addition, the silver-plated layer contact is also easy to corrode in the service process, and particularly, the silver-plated layer contact is easy to corrode in an industrial sulfur-containing atmosphere environment to form a silver sulfide film with poor conductivity, so that the conductivity of the contact is poor.
Modification treatment of the silver plating layer is a simple and effective method for improving the wear resistance and the corrosion resistance of the silver plating layer, but the existing modification treatment cannot enable the silver plating layer to have the wear resistance, the corrosion resistance, the conductivity and the heat conductivity at the same time.
Disclosure of Invention
In view of the above, the present application provides a silver-niobium carbide composite plating layer and a preparation method thereof, which can effectively solve the technical defect that the existing silver plating layer cannot simultaneously have wear resistance, corrosion resistance, electrical conductivity and thermal conductivity.
The application provides a preparation method of a silver-niobium carbide composite coating, which comprises the following steps:
step 1, using NbCl5Taking Nb and carbon black as reactants, carrying out heating reaction on the reactants and chloride salt, and then washing to obtain nano niobium carbide powder;
step 2, mixing the nano niobium carbide powder with a plating solution to obtain an electroplating solution, wherein the plating solution comprises a water-soluble silver-containing compound, succinimide, potassium pyrophosphate, a dispersant and an acid-base regulator;
and 3, electroplating the base material in the electroplating solution to obtain the silver-niobium carbide composite coating.
Preferably, the particle size of the nano niobium carbide powder is 10-500 nm.
Preferably, the particle size of the nano niobium carbide powder is 20-200 nm.
Preferably, the microhardness of the nano niobium carbide powder>23.5 GPa; the resistivity of the nano niobium carbide powder is 35 mu omega cm; the theoretical density of the nano niobium carbide powder is 7.821g/cm3。
Preferably, the silver-niobium carbide composite plating layer has a thickness of 10 to 30 μm.
Preferably, in step 1, (the NbCl)5+ said Nb) to said carbon black in a molar ratio of 1: 1; the NbCl5The molar ratio to said Nb is greater than 1/8.
Preferably, in step 1, the chloride salt is selected from sodium chloride or/and potassium chloride, and the mass ratio of the reactant to the chloride salt is 1/7.
Wherein the reactant is NbCl5A mixture of Nb and carbon black.
Preferably, in the step 1, the reaction temperature is 800-950 ℃; the reaction time is 0.5-5 hours.
More preferably, in step 1, the reaction temperature is 900 ℃; the reaction time was 0.5 hour.
Preferably, in the step 2, the concentration of the water-soluble silver-containing compound is 20-60 g/L; the concentration of the succinimide is 80-140 g/L; the concentration of the potassium pyrophosphate is 80-140 g/L; the concentration of the dispersing agent is 0.1-1.2 g/L; the concentration of the nano niobium carbide powder is 1-10 g/L.
More preferably, the water soluble silver containing compound is selected from silver nitrate.
Preferably, in the step 2, the acid-base regulator is HNO with the mass fraction of 10%3Solution and 35g/L NaOH solution; the pH value of the electroplating solution is 8.5-10.5.
Preferably, in step 3, the electroplating method comprises: taking a base material of an oxygen-free copper sheet as a cathode and a graphite plate as an anode; placing the base material in the electroplating solution for electroplating, wherein the current density of the electroplating is 10-40 mA ∙ cm-2And the temperature of the electroplating solution is 20-60 ℃.
Specifically, the electroplating method comprises the following steps:
(1) in the electroplating process, a cathode adopts a high-purity oxygen-free copper sheet as an electroplating substrate, and an anode adopts a high-purity graphite plate;
(2) placing the oxygen-free copper sheet into an electroplating solution, and stirring the electroplating solution by using a constant-temperature heating magnetic stirrer, wherein the current density is 10-40 mA ∙ cm-2And the temperature is 20-60 ℃, so that the electroplated part deposited with the silver-niobium carbide layer is obtained;
(3) and washing the electroplated part by deionized water, and then air-drying to obtain the electroplated part with the silver-niobium carbide composite coating deposited on the surface.
More preferably, the mixture is stirred by a magnetic stirrer, and the rotor speed is 500-2000 r ∙ min-1Preferably 800 to 1200r ∙ min-1。
Wherein the thickness of the silver-niobium carbide composite coating obtained after 20-60 minutes of electroplating deposition is 10-30 μm.
Preferably, the preparation method of the oxygen-free copper sheet substrate comprises the following steps: and (3) polishing, deoiling, cleaning and pickling the copper sheet in sequence to obtain the oxygen-free copper sheet base material.
Specifically, the preparation method of the oxygen-free copper sheet substrate comprises the following steps:
firstly, sequentially and uniformly polishing copper sheets by using No. 240-1000 abrasive paper under an aqueous condition until the surfaces of the copper sheets are smooth and flat;
secondly, respectively soaking the copper sheet obtained in the first step in deionized water, acetone and absolute ethyl alcohol, and ultrasonically cleaning for 5min, and soaking the copper sheet in absolute ethyl alcohol to be used as a base material for later use;
thirdly, taking out the base material before electroplating, and washing the base material by using deionized water;
and fourthly, putting the cleaned base material obtained in the third step into an acid washing solution to be soaked for 30-60 s, and then cleaning the base material with deionized water to obtain the oxygen-free copper sheet.
The application creatively takes NbCl5Nb and carbon black are reactants to prepare nano niobium carbide powder in high-temperature molten chloride salt, and the dispersion-distributed high-hardness wear-resistant particles (niobium carbide) are introduced into the silver-niobium carbide composite coatingThe hardness of the silver-niobium carbide composite coating and the niobium carbide serving as wear-resistant particles can well resist sliding wear, so that the overall wear resistance of the material is improved. Niobium carbide has excellent chemical stability, high conductivity (resistivity 35. omega. cm) and high hardness (harder than corundum, microhardness)>23.5Gpa, hardness greater than 130 HV). Therefore, the silver-niobium carbide composite coating with good wear resistance and corrosion resistance is obtained by modifying the silver coating with the nano niobium carbide particles.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a surface Scanning Electron Microscope (SEM) morphology of a silver-niobium carbide composite coating in example 4 of the present invention;
FIG. 2 is a scanning electron micrograph showing a cross section of a silver-niobium carbide composite plating layer in example 4 of the present invention;
FIG. 3 is an elemental line scan of a cross section of a silver-niobium carbide composite plating layer in example 4 of the present invention.
Detailed Description
The application provides a silver-niobium carbide composite coating and a preparation method thereof, which are used for solving the technical defect that the existing silver coating cannot simultaneously have wear resistance, corrosion resistance, electric conductivity and heat conductivity.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The raw materials used in the following examples are all commercially available or self-made.
Examples 1 to 3
The preparation method of the nano niobium carbide powder of the embodiment 1-3 comprises the following steps:
addition as per Table 1In a molar ratio of NbCl5And taking Nb and carbon black as a reaction mixture 1, taking a mixture of sodium chloride and potassium chloride as a reaction mixture 2, mixing the reaction mixture 1 and the reaction mixture 2 (the mass ratio of the reaction mixture 1 to the reaction mixture 2 is 1/7), heating to 900 ℃, preserving heat for 2 hours, cooling a molten mass after the reaction is finished, washing with deionized water to remove salt, and filtering to obtain nano niobium carbide powder, wherein the nano niobium carbide powder is marked as a product 1-3.
Comparative examples 1 to 4
The products of comparative examples 1-4 were prepared as follows:
in the molar ratio of NbCl added in Table 15And taking Nb and carbon black as a reaction mixture 1, taking a mixture of sodium chloride and potassium chloride as a reaction mixture 2, mixing the reaction mixture 1 and the reaction mixture 2 (the mass ratio of the reaction mixture 1 to the reaction mixture 2 is 1/7), heating to 900 ℃, preserving heat for 2 hours, cooling a molten mass after the reaction is finished, washing with deionized water to remove salt, and filtering to obtain a product 4-7.
TABLE 1
Example 4
The substrate is a high-purity oxygen-free copper sheet, and is firstly polished to 1000# by using sand paper, then is respectively cleaned for 5min by using deionized water, absolute ethyl alcohol and acetone in ultrasonic, and is soaked in the absolute ethyl alcohol for standby. The formula of the electroplating solution is as follows: 40g/L of water-soluble silver-containing compound silver nitrate, 85g/L of succinimide, 70g/L of potassium pyrophosphate and 0.65 g.L-1And a dispersing agent, wherein deionized water is used for dissolving chemicals to prepare a solution, and the pH value of the plating solution is adjusted to 9.5. Adding 1.8 g.L into the prepared plating solution-1The nano niobium carbide powder of example 1 was magnetically stirred for 2.5 hours. Taking a mechanically polished and cleaned high-purity graphite plate as an anode and a copper sheet substrate as a cathode, and before electroplating, taking the copper sheet substrate as a cathodeSoaking the alloy in a dilute sulfuric acid solution with the mass fraction of 10% for 45s, washing the alloy with deionized water to remove surface oxides, then carrying out composite electroplating operation, and controlling process parameters in a constant current mode: the current density is 35.0mA ∙ cm-2The electrodeposition temperature is 30 ℃, the electrodeposition time is 0.5 hour, and the rotating speed of a magnetic stirrer rotor is 1000r ∙ min-1. And repeatedly washing the electroplated part by using deionized water after electroplating, and drying by blowing to obtain the electroplated part deposited with the silver-niobium carbide composite coating.
The silver-niobium carbide composite coating obtained in the present example was subjected to surface micro-morphology and composition analysis, and the results are shown in fig. 1 to 3. FIG. 1 is a surface Scanning Electron Microscope (SEM) morphology of a silver-niobium carbide composite coating in example 4 of the present invention; FIG. 2 is a scanning electron micrograph showing a cross section of a silver-niobium carbide composite plating layer in example 4 of the present invention; FIG. 3 is an elemental line scan of a cross section of a silver-niobium carbide composite plating layer in example 4 of the present invention. In fig. 1, the dark color region is a niobium carbide aggregation region, and the bright color region is a silver matrix, and it can be seen that the coating layer prepared on the surface of the copper matrix is a silver-niobium carbide composite coating layer in which nano niobium carbide is dispersedly distributed in the silver matrix. Fig. 2 illustrates that the silver-based plating layer of the silver-niobium carbide composite plating layer of the examples of the present application is surface dense and well bonded to the copper substrate. Meanwhile, the coating cross section is subjected to line scanning component analysis by using an X-ray energy scattering spectrum (EDS), the distribution of the cross section components is shown in figure 3, and the content of niobium carbide in the silver-based coating is 0.8 at.%, and the balance is silver. The hardness of the plating was also measured, and the HV hardness value was 136.
Example 5
In this example, similar to example 4, 1.8 g.L was added to the prepared plating solution-1The current density of the nano niobium carbide powder of example 1 was 30mA ∙ cm-2The silver-niobium carbide composite plating layer was prepared, the content of niobium carbide in the silver-niobium carbide composite plating layer was 0.5 at.%, the balance was silver, the HV hardness of the plating layer was 131, and the surface and cross-sectional morphology of the plating layer were similar to those of example 4.
Example 6
This example was carried out in a similar manner to example 4, except that 3 was added to the prepared plating solution.5g·L-1The current density of the nano niobium carbide powder of example 1 was 30mA ∙ cm-2The silver-niobium carbide composite plating layer was prepared, the content of niobium carbide in the silver-niobium carbide composite plating layer was 1.1 at.%, the balance was silver, the HV hardness of the plating layer was 139, and the surface and cross-sectional morphology of the plating layer were similar to those of example 4.
Example 7
In this example, similar operation to that of example 4 was carried out, and the prepared plating solution was divided into 7 parts on average, and 1.8 g.L was added to each part of the plating solution-11-7 of the product, and the current density of the product is 30mA ∙ cm-2And preparing the silver-niobium carbide composite coating (marked as products 1-7), wherein the products 1-7 correspond to the products 1-7 one by one (namely the product 1 is prepared into the product 1, and so on). The texture of the product is detected to be 1-7, and the texture of the product is 1-3 and is harder than the texture of the product to be 4-7. As can be seen, the hardness of the products 1-3 prepared in examples 1-3 is significantly higher than the hardness of the products 4-7 prepared in comparative examples 1-4.
Example 8
The product 1 obtained in example 1, a conventional silver-plated product (commercial product), a graphite silver composite-plated product (commercial product), and a copper substrate were subjected to performance tests, and the results are shown in table 2.
TABLE 2
| Average coefficient of friction/COF | Contact resistance (m.OMEGA.. cndot.cm)2) | Hardness (HV) | |
| Product 1 | 0.6392 | 0.068 | 139 |
| Silver coating | 0.3784 | 0.059 | 85 |
| Graphite silver composite coating | 0.2496 | 0.082 | 90.5 |
| Copper (Cu) | 0.3123 | 0.071 | 98 |
The hardness and the wear resistance of the 1Ag-NbC composite coating of the product prepared by the method are far higher than those of other coatings, and the conductivity of the coating is similar to that of a silver-plated coating.
The foregoing is only a preferred embodiment of the present application and it should be noted that those skilled in the art can make several improvements and modifications without departing from the principle of the present application, and these improvements and modifications should also be considered as the protection scope of the present application.
Claims (10)
1. The preparation method of the silver-niobium carbide composite coating is characterized by comprising the following steps of:
step 1, using NbCl5Taking Nb and carbon black as reactants, carrying out heating reaction on the reactants and chloride salt, and then washing to obtain nano niobium carbide powder;
step 2, mixing the nano niobium carbide powder with a plating solution to obtain an electroplating solution, wherein the plating solution comprises a water-soluble silver-containing compound, succinimide, potassium pyrophosphate, a dispersant and an acid-base regulator;
and 3, electroplating the base material in the electroplating solution to obtain the silver-niobium carbide composite coating.
2. The preparation method according to claim 1, wherein the nano niobium carbide powder has a particle size of 10 to 500 nm.
3. The method according to claim 1, wherein the nano niobium carbide powder has microhardness>23.5 GPa; the resistivity of the nano niobium carbide powder is 35 mu omega cm; the theoretical density of the nano niobium carbide powder is 7.821g/cm3。
4. The production method according to claim 1, wherein the silver-niobium carbide composite plating layer has a thickness of 10 to 30 μm.
5. The method of claim 1, wherein in step 1, (the NbCl)5+ said Nb) to said carbon black in a molar ratio of 1: 1; the NbCl5The molar ratio to said Nb is greater than 1/8.
6. The method according to claim 1, wherein in step 1, the chloride salt is selected from sodium chloride and/or potassium chloride, and the mass ratio of the reactant to the chloride salt is 1/7.
7. The method according to claim 1, wherein the reaction temperature in step 1 is 800 to 950 ℃; the reaction time is 0.5-5 hours.
8. The method according to claim 1, wherein in step 2, the concentration of the water-soluble silver-containing compound in step 2 is 20 to 60 g/L; the concentration of the succinimide is 80-140 g/L; the concentration of the potassium pyrophosphate is 80-140 g/L; the concentration of the dispersing agent is 0.1-1.2 g/L; the concentration of the nano niobium carbide powder is 1-10 g/L.
9. The preparation method according to claim 1, wherein in the step 2, the acid-base regulator is HNO with a mass fraction of 10%3Solutions and 35g/LNaOH solution; the pH value of the electroplating solution is 8.5-10.5.
10. The method according to claim 9, wherein in step 3, the electroplating method comprises: taking a base material of an oxygen-free copper sheet as a cathode and a graphite plate as an anode; placing the base material in the electroplating solution for electroplating, wherein the current density of the electroplating is 10-40 mA ∙ cm-2And the temperature of the electroplating solution is 20-60 ℃.
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| CN111424303A (en) * | 2020-05-19 | 2020-07-17 | 暨南大学 | SiC nano-silver composite electrodeposition coating and preparation method and application thereof |
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