CN113106521B - Ni-W-ZrC microcrystal coating, plating solution and preparation method thereof - Google Patents

Ni-W-ZrC microcrystal coating, plating solution and preparation method thereof Download PDF

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CN113106521B
CN113106521B CN202110397996.4A CN202110397996A CN113106521B CN 113106521 B CN113106521 B CN 113106521B CN 202110397996 A CN202110397996 A CN 202110397996A CN 113106521 B CN113106521 B CN 113106521B
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zrc
coating
microcrystal
solution
plating
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CN113106521A (en
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何毅
李虹杰
施太和
范毅
何腾
田秋成
刘大红
张慧俐
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Tianjin Jingcheng Weiye Machine Manufacturing Co ltd
Southwest Petroleum University
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Tianjin Jingcheng Weiye Machine Manufacturing Co ltd
Southwest Petroleum University
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/562Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02TCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T50/00Aeronautics or air transport
    • Y02T50/60Efficient propulsion technologies, e.g. for aircraft

Abstract

The invention discloses a Ni-W-ZrC microcrystal plating layer, plating solution and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a nickel-tungsten electroplating solution, adding zirconium carbide micro powder and a conductive agent into the nickel-tungsten electroplating solution, and then adjusting the pH value of the solution to 5-10 by using a pH regulator to obtain Ni-W-ZrC microcrystal plating solution; and (3) pretreating a sample to be electroplated, then soaking the pretreated sample into the Ni-W-ZrC microcrystal plating solution, and then electroplating to obtain the Ni-W-ZrC microcrystal plating layer. According to the invention, zirconium carbide micropowder is used as a strengthening material of the coating and a nucleation accelerator in the plating solution, disordered deposition of nickel-tungsten alloy can be effectively inhibited, the grain size is refined, so that the Ni-W-ZrC microcrystalline coating with a microcrystalline structure is finally obtained, the surface property of the coating is optimized, and the hydrophobic property of the coating is improved, so that the corrosion resistance of the coating is improved; in addition, the existence of the microcrystal can weaken tensile stress and tensile stress generated in the electroplating process, improve the adhesive force of the plating layer and the matrix, reduce the formation of microcracks and other electroplating defects and enhance the toughness of the plating layer.

Description

Ni-W-ZrC microcrystal coating, plating solution and preparation method thereof
Technical Field
The invention relates to the technical field of electroplating, in particular to a Ni-W-ZrC microcrystal plating layer, a plating solution and a preparation method thereof.
Background
In the existing various corrosion prevention methods, the surface treatment of materials by electroplating is a simple and effective means. Among them, the electroplated Ni-W alloy coating has attracted much attention in the field of oil and gas field application because of its excellent corrosion resistance, wear resistance, high hardness, and the like. However, in practical application, the Ni-W alloy coating is easy to generate micro cracks due to the high hardness of the Ni-W alloy, and the coating is easy to fail. In addition, the hydrophobic property of the existing Ni-W alloy coating is not enough, and if the hydrophobic property is enhanced, the corrosion resistance of the coating can be further improved.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a Ni-W-ZrC microcrystal plating layer, a plating solution and a preparation method thereof.
The technical scheme of the invention is as follows:
on the one hand, the Ni-W-ZrC microcrystal coating is provided, the coating is of a micro-nano crystal structure, and the coating comprises Ni elements, W elements, Zr elements and C elements.
Preferably, the particle size of the plating layer is 500nm to 10 μm.
Preferably, the content of each element is as follows by mass percent: 80-92% of Ni, 5-15% of W, 2-9% of C and 1-3% of Zr.
On the other hand, the Ni-W-ZrC microcrystal plating solution comprises the following components: the micro-crystal plating solution comprises a nickel-tungsten electroplating solution, zirconium carbide micro powder, a conductive agent and a pH regulator, wherein the pH of the micro-crystal plating solution is 5-10.
Preferably, the nickel tungsten plating solution is a sulfate type or a sulfamate type.
Preferably, the particle size of the zirconium carbide fine powder is 10 to 100 nm.
Preferably, the conductive agent is sodium bromide or sodium fluoride.
Preferably, the pH of the microcrystal plating solution is 6-7.5.
Preferably, the microcrystal plating solution also comprises a stress remover and/or a surfactant.
On the other hand, the preparation method of the Ni-W-ZrC microcrystal coating comprises the following steps: preparing a nickel-tungsten electroplating solution, adding zirconium carbide micro powder and a conductive agent into the nickel-tungsten electroplating solution, and then adjusting the pH value of the solution to 5-10 by using a pH regulator to obtain Ni-W-ZrC microcrystal plating solution; and (3) pretreating a sample to be electroplated, then soaking the pretreated sample into the Ni-W-ZrC microcrystal plating solution, and then electroplating to obtain the Ni-W-ZrC microcrystal plating layer.
The invention has the beneficial effects that:
ZrC micro powder is added into the existing nickel-tungsten electroplating solution system to serve as a nucleation accelerator of the plating solution and a dispersion strengthening reinforcing phase of the plating layer. By adding ZrC micro powder, the number of microcracks on the surface of the coating is obviously reduced, the surface integrity of the coating is improved, and in addition, the hydrophobicity of the coating is also improved. The hardness, wear resistance, corrosion resistance and other properties of the plating layer are greatly improved through the dispersion strengthening effect of ZrC. In addition, due to the addition of the ZrC particles, the grain size of the plating layer is refined, and the toughness of the plating layer is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention 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, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic flow chart of a Ni-W-ZrC microcrystal coating preparation method of the invention;
FIG. 2 is a schematic drawing of the scanning electron microscope results of the coatings of example 1 and comparative example 1;
FIG. 3 is a graph showing the results of X-ray diffraction and grain size distribution of the plating layers of examples 1 and 3 and comparative example 1;
FIG. 4 is a graph showing the result of the energy spectrum analysis of the plating layer of example 1;
FIG. 5 is a graph showing the results of cross-sectional analysis of the plating layer of example 1;
FIG. 6 is a graph showing the results of X-ray photoelectron spectroscopy analysis of the plated layer of example 1;
FIG. 7 is a graph showing the results of microhardness of the coatings of examples 1, 3 and comparative example 1;
FIG. 8 is a graph showing the results of the friction test of the plating layers of example 1 and comparative example 1;
FIG. 9 is a graph showing the results of the water contact angle test for the plating layers of examples 1, 3 and comparative example 1;
FIG. 10 is a graph showing the results of an atomic force microscope test of the plating layer of example 1;
fig. 11 is a graph showing the results of electrochemical tests of the plating layers of examples 1, 3 and comparative example 1.
Detailed Description
The invention is further illustrated with reference to the following figures and examples. It should be noted that, in the present application, the embodiments and the technical features of the embodiments may be combined with each other without conflict. It is noted that, unless otherwise indicated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The use of the terms "comprising" or "including" and the like in the present disclosure is intended to mean that the elements or items listed before the term cover the elements or items listed after the term and their equivalents, but not to exclude other elements or items.
On one hand, the invention provides a Ni-W-ZrC microcrystal coating, which is in a micro-nano crystal structure, the particle size of the coating is 500nm-10 mu m, and the coating comprises the following elements in percentage by mass: 80-92% of Ni element, 5-15% of W element, 1-3% of Zr element, and 2-9% of C element.
On the other hand, the invention also provides a Ni-W-ZrC microcrystal plating solution which comprises the following components: the micro-crystal plating solution comprises a nickel-tungsten electroplating solution, zirconium carbide micro powder, a conductive agent and a pH regulator, wherein the pH of the micro-crystal plating solution is 5-10, and optionally, the pH of the micro-crystal plating solution is 6-7.5.
The nickel-tungsten electroplating solution is the prior art and comprises main components such as nickel salt, tungstate, a complexing agent and the like, and the nickel-tungsten electroplating solution is divided into an aminosulfonate type and a sulfate type according to the type of the nickel salt; the nickel-tungsten electroplating solution may be classified into a citric acid type, a tartaric acid type, a malic acid type, a gluconic acid type, a saccharine type, a glycolic acid type, and the like, according to the kind of the complexing agent.
In a specific embodiment, the nickel-tungsten electroplating solution is a sulfate type, and optionally, the microcrystalline plating solution comprises 2-50g/L of nickel sulfate, 5-50g/L of sodium tungstate, 10-200g/L of trisodium citrate, 0.1-20g/L of zirconium carbide micropowder and 10-50g/L, pH of conductive agent regulator, and 10-100 g/L. In another specific embodiment, the nickel-tungsten electroplating solution is of sulfamate type, and optionally, the microcrystalline plating solution comprises 2-50g/L of nickel sulfamate, 5-50g/L of sodium tungstate, 0.1-20g/L of zirconium carbide micropowder, and 10-50g/L, pH of conductive agent regulator, and 10-100g/L of conductive agent regulator.
It should be noted that the pH adjusting agent for adjusting the pH value of the electroplating solution is the prior art, and may be specifically selected according to the type of the nickel-tungsten electroplating solution or the complexing agent adopted by the nickel-tungsten electroplating solution. For example, in the above embodiment, when the nickel-tungsten electroplating solution is a sulfate type and the complexing agent is trisodium citrate, ammonium chloride and citric acid can be used as the corresponding pH adjusting agents; when the nickel-tungsten electroplating solution is of a sulfamate type, the nickel source nickel sulfamate is a complexing agent of the nickel-tungsten electroplating solution, other complexing agents are not needed, the corresponding pH regulator cannot select citric acid, and other pH regulators in the prior art, such as ammonium chloride and hydrochloric acid, can be selected.
In a specific embodiment, the particle size of the zirconium carbide micro powder is 10-100 nm. Optionally, the particle size of the zirconium carbide micro powder is 30-60 nm. The zirconium carbide micro powder with too fine grain diameter can easily cause the agglomeration of zirconium carbide materials, influence the coating effect and is high in price. The zirconium carbide micro powder with too large grain diameter can cause the zirconium carbide particles to be incapable of stably suspending in the plating solution, thereby affecting the performance of the plating layer.
In a specific embodiment, the conductive agent is sodium bromide or sodium fluoride. It should be noted that the kind of the conductive agent in the present embodiment is not a limitation to the present invention, and other conductive agents in the plating solution in the prior art are also applicable to the present invention.
In a specific embodiment, the microcrystalline plating solution further comprises a stress relief agent and/or a surfactant. Optionally, the stress relief agent is saccharin or saccharin sodium; the surfactant is any one of an anionic surfactant (such as sodium dodecyl sulfate), a cationic surfactant (such as cetyl trimethyl ammonium bromide) and a nonionic surfactant (such as polyethylene glycol). It should be noted that the stress relieving agent and the surfactant are prior art, the kind of the examples of the stress relieving agent and the surfactant is not limited to the present invention, and other stress relieving agents and other surfactants that can be used in the electroplating solution are also suitable for the present invention.
On the other hand, as shown in fig. 1, the invention also provides a preparation method of the Ni-W-ZrC microcrystal plating layer, which comprises the following steps: preparing a nickel-tungsten electroplating solution, adding zirconium carbide micro powder and a conductive agent into the nickel-tungsten electroplating solution, and then adjusting the pH value of the solution to 5-10 by using a pH regulator to obtain Ni-W-ZrC microcrystal plating solution; and (3) pretreating a sample to be electroplated, then soaking the pretreated sample into the Ni-W-ZrC microcrystal plating solution, and then electroplating to obtain the Ni-W-ZrC microcrystal plating layer.
In a specific embodiment, the pretreatment of the sample to be electroplated comprises degreasing, derusting and acid washing activation of the sample to be electroplated.
In a specific embodiment, the temperature of the electroplating treatment is 50-80 ℃ and the current density is 1-10A/dm2. Optionally, the temperature is 65-75 ℃, and the current density is 4-6A/dm2. The deposition speed of the Ni-W-ZrC microcrystal coating can be controlled within the range of 15-30 mu m/h by controlling the pH value, the temperature and the current density.
It should be noted that the Ni-W-ZrC microcrystalline coating of the present invention can be prepared by other coating preparation methods in the prior art besides the preparation method of the above embodiment.
Example 1
The Ni-W-ZrC microcrystal coating is prepared by the following steps: weighing 15g/L of nickel sulfate, 40g/L of sodium tungstate, 150g/L of trisodium citrate, 2g/L of zirconium carbide micropowder, 20g/L of sodium bromide, 0.1g/L of sodium dodecyl sulfate and 1g/L of saccharin, adding a proper amount of water, heating, stirring and dissolving the reagents, and preparing 1L of solution (the pH value of the solution is adjusted to 7.5 by using 20g/L of ammonium chloride in the preparation process). The plating solution temperature was set at 75 deg.C, using a graphite plate or titanium mesh as an anode (length 50mm, width 50mm, thickness 2cm), and a pure iron sheet or carbon steel coupon as a cathode (length 50mm, width 50mm, thickness 2 cm). At 5A/dm2Electroplating for 1 hour to obtain the Ni-W-ZrC microcrystal coating.
Comparative example 1
An Ni-W coating is prepared by the following steps: weighing 15g/L of nickel sulfate, 40g/L of sodium tungstate, 150g/L of trisodium citrate, 20g/L of sodium bromide, 0.1g/L of sodium dodecyl sulfate and 1g/L of saccharin, adding a proper amount of water, heating, stirring and dissolving the reagents, and preparing 1L of solution (wherein the pH value of the solution is adjusted to 7.5 by using 20g/L of ammonium chloride in the preparation process). The plating solution temperature was set at 75 deg.C, using a graphite plate or titanium mesh as an anode (length 50mm, width 50mm, thickness 2cm), and a pure iron sheet or carbon steel coupon as a cathode (length 50mm, width 50mm, thickness 2 cm). At 5A/dm2Electroplating for 1 hour to obtain the Ni-W plating layer.
Example 2
The Ni-W-ZrC microcrystal coating is prepared by the following steps: weighing 30g/L nickel sulfamate, 30g/L sodium tungstate, 5g/L zirconium carbide micropowder, 20g/L sodium fluoride, 0.2g/L sodium dodecyl sulfate and 2g/L saccharin sodium powder, adding a proper amount of water, heating, stirring and dissolving the reagents, and preparing 1L solution (in the preparation process, adjusting the pH of the solution to 5.5 by using 10g/L hydrochloric acid). The plating solution temperature was set at 75 ℃ and a graphite plate or a titanium mesh was used as an anode (50 mm. times.50 mm. times.2 cm) and a pure iron piece or a carbon steel test piece was used as a cathode (50 mm. times.50 mm. times.2 cm). At 10A/dm2Electroplating for 1 hour to obtain the Ni-W-ZrC microcrystal coating.
Comparative example 2
An Ni-W coating is prepared by the following steps: weighing 30g/L nickel sulfamate, 30g/L sodium tungstate, 20g/L sodium fluoride, 0.2g/L sodium dodecyl sulfate and 2g/L saccharin sodium, adding a proper amount of water, heating, stirring and dissolving the reagents, and preparing 1L of solution (in the preparation process, the pH value of the solution is adjusted to 5.5 by using 10g/L hydrochloric acid). The plating solution temperature was set at 75 deg.C, using a graphite plate or titanium mesh as an anode (length 50mm, width 50mm, thickness 2cm), and a pure iron sheet or carbon steel coupon as a cathode (length 50mm, width 50mm, thickness 2 cm). At 10A/dm2Electroplating for 1 hour to obtain a Ni-W coating.
Example 3
In this example, 4 kinds of Ni-W-ZrC microcrystal coatings with different zirconium carbide contents were prepared, and the Ni-W-ZrC microcrystal coatings are different from those in example 1 in that the contents of zirconium carbide micro powder in this example are 0.4g/L, 1g/L, 4g/L and 6g/L respectively.
Test example
1) The microscopic morphology of the Ni-W-ZrC microcrystalline plating layer prepared in example 1 and the Ni-W plating layer prepared in comparative example 1 was observed by a scanning electron microscope, and the results are shown in fig. 2, in which fig. 2(a) is a schematic view of the microscopic morphology of the Ni-W plating layer, and fig. 2(B) is a schematic view of the microscopic morphology of the Ni-W-ZrC microcrystalline plating layer. As can be seen from FIG. 2, the Ni-W-ZrC microcrystal coating is relatively flat, while the surface of the conventional Ni-W coating is filled with microcracks and large crystal cells and is extremely uneven.
2) Phase analysis and grain size analysis were performed on the plating layers of example 1, comparative example 1, and example 3, and the results of X-ray diffraction and grain size distribution are shown in fig. 3, in which fig. 3(a) is a graph showing the results of X-ray diffraction, and fig. 3(B) is a graph showing the results of grain size distribution. As can be seen from FIG. 3, the grain size of the Ni-W plating layer was about 30 nm. With the addition of the zirconium carbide micro powder, the grain size of the coating is remarkably reduced, and is minimum at 2g/L and 14 nm; the reduction of the grain size can improve the mechanical property and the corrosion resistance of the plating layer.
3) The result of performing energy spectrum analysis on the Ni-W-ZrC microcrystalline coating prepared in example 1 is shown in fig. 4, where fig. 4(a) is a schematic diagram of a scanning result of an energy spectrum plane obtained by superimposing four elements, i.e., Ni, W, C, and Zr, fig. 4(B) is a schematic diagram of a scanning result of an energy spectrum plane obtained by scanning Ni element, fig. 4(C) is a schematic diagram of a scanning result of an energy spectrum plane obtained by scanning W element, fig. 4(D) is a schematic diagram of a scanning result of an energy spectrum plane obtained by scanning C element, fig. 4(E) is a schematic diagram of a scanning result of an energy spectrum plane obtained by scanning Zr element, fig. 4(F) is a schematic diagram of a corresponding scanning electron microscope, and fig. 4(G) is a schematic diagram of an analysis result of an element content obtained by scanning an energy spectrum plane. As can be seen from FIG. 4, the Ni-W-ZrC microcrystal plating elements are uniformly distributed in the whole.
4) The Ni-W-ZrC microcrystal plating prepared in example 1 was subjected to cross-sectional analysis, and the results are shown in fig. 5, in which fig. 5(a) is a plan view of a selected plating sample, fig. 5(B) is a cross-sectional view of the selected plating sample, and fig. 5(C) is a schematic diagram showing the results of elemental composition analysis of the selected plating sample. As can be seen from FIG. 5, the Ni-W-ZrC microcrystalline plating layer of this example was about 24 μm thick. The Ni-W-ZrC microcrystalline coating layer obtained in example 2 was also analyzed in cross section, and the thickness of the Ni-W-ZrC microcrystalline coating layer was about 28 μm.
5) The result of X-ray photoelectron spectroscopy analysis of the Ni-W-ZrC microcrystal plating layer prepared in example 1 is shown in fig. 6, in which fig. 6(a) is a schematic diagram of the analysis result of Ni element, fig. 6(B) is a schematic diagram of the analysis result of W element, fig. 6(C) is a schematic diagram of the analysis result of C element, and fig. 6(D) is a schematic diagram of the analysis result of Zr element. As can be seen from fig. 6, the contents of several elements are significant, and the deposition on the coating is successful.
6) Microhardness tests were performed on the plating layers of example 1, comparative example 1, and example 3, and the test results are shown in fig. 7. As can be seen from FIG. 7, compared with the pure nickel-tungsten coating, after ZrC with different contents is added, the microhardness of the coating is greatly improved, the improvement is most obvious at 2g/L, and the difference between the two can reach about 300 HV.
7) The coatings of example 1 and comparative example 1 were subjected to a rubbing test, and the test results are shown in fig. 8, in which fig. 8(a) is a rubbing test chart of the Ni-W coating of comparative example 1, fig. 8(B) is a rubbing test chart of the Ni-W-ZrC microcrystal coating of example 1, fig. 8(C) is a three-dimensional profile reconstruction chart of the rubbing scratch of the Ni-W coating of comparative example 1, and fig. 8(D) is a three-dimensional profile reconstruction chart of the rubbing scratch of the Ni-W-ZrC microcrystal coating of example 1. As can be seen from FIG. 8, the wear resistance of the Ni-W-ZrC microcrystal plating layer is greatly improved compared with the wear resistance of the conventional Ni-W plating layer.
8) The plating layers of example 1, comparative example 1, and example 3 were subjected to a water contact angle test, and the test results are shown in fig. 9. As can be seen from FIG. 9, the hydrophobic property of the Ni-W-ZrC microcrystal coating is greatly improved compared with that of the conventional Ni-W coating.
9) The Ni-W-ZrC crystallite plating of example 1 was observed by atomic force microscopy, and the test results are shown in fig. 10, where fig. 10(a) is a 3D image and fig. 10(B) is a 2D image. As can be seen from FIG. 10, the Ni-W-ZrC microcrystal coating has low apparent roughness which is less than 100nm, and the coating is smooth.
10) The plating layers of example 1, comparative example 1, and example 3 were electrochemically tested, and the test results are shown in fig. 11, in which fig. 11(a) is a graph showing the polarization curve test results, fig. 11(B) is an impedance-nyquist plot, fig. 11(C) is an impedance-baud plot, and fig. 11(D) is an impedance-baud phase plot. As can be seen from fig. 11, compared with the pure nickel-tungsten coating, after ZrC with different contents is added, the corrosion potentials of the coating are all shifted to the positive direction, the corrosion current is reduced, and the impedance value is increased; the corrosion resistance of the plating is obviously improved by adding ZrC.
The invention is based on the nickel-tungsten electroplating solution system, zirconium carbide micropowder is added into the nickel-tungsten electroplating solution system, a hydrated double electric layer is formed through the electrostatic action on the surface of the zirconium carbide micropowder, surrounding ions are attracted, and the zirconium carbide micropowder is deposited on the surface of a cathode under the action of an electric field, and simultaneously, the deposition provides a nucleation site for the nickel-tungsten electrodeposition; through the large-scale deposition of the zirconium carbide micro powder, the disordered deposition of the nickel-tungsten alloy can be effectively inhibited, the grain size is refined, and finally the Ni-W-ZrC microcrystal coating with a microcrystal structure is obtained.
The existence of the microcrystal can weaken the tensile stress and tensile stress generated in the electroplating process, improve the adhesive force of the coating and the matrix, reduce the formation of microcracks and other electroplating defects and enhance the toughness of the coating. Meanwhile, due to the ordered deposition of the zirconium carbide particles, the surface property of the coating can be optimized, so that the Ni-W-ZrC microcrystal coating is more hydrophobic than a pure nickel-tungsten coating, and the corrosion resistance of the coating is further improved.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. The Ni-W-ZrC microcrystal coating is characterized by being of a micro-nano crystal structure and composed of a nickel-tungsten coating and a ZrC dispersion strengthening reinforcing phase, wherein the coating comprises 80-92% of Ni element, 5-15% of W element, 1-3% of Zr element and 2-9% of C element in percentage by mass.
2. The Ni-W-ZrC microcrystalline coating of claim 1 wherein the coating has a grain size of 500nm to 10 μm.
3. The Ni-W-ZrC microcrystal plating solution is characterized by comprising the following components: the micro-crystal plating solution comprises a nickel-tungsten electroplating solution, zirconium carbide micro powder, a conductive agent and a pH regulator, wherein the pH of the micro-crystal plating solution is 5-10.
4. The Ni-W-ZrC crystallite plating solution according to claim 3, characterized in that the nickel tungsten plating solution is of the sulphate type or sulphamate type.
5. The Ni-W-ZrC microcrystal plating solution according to claim 3, wherein the zirconia fine powder has a particle size of 10 to 100 nm.
6. The Ni-W-ZrC crystallite plating bath according to claim 3, characterized in that the conductive agent is sodium bromide or sodium fluoride.
7. The Ni-W-ZrC crystallite plating bath according to claim 3, characterized in that the pH of the crystallite plating bath is 6-7.5.
8. The Ni-W-ZrC crystallite plating bath according to any one of claims 3 to 7, characterized in that it further comprises a stress relief agent and/or a surfactant.
9. A preparation method of a Ni-W-ZrC microcrystal coating is characterized by comprising the following steps: preparing a nickel-tungsten electroplating solution, adding zirconium carbide micro powder and a conductive agent into the nickel-tungsten electroplating solution, and then adjusting the pH value of the solution to 5-10 by using a pH regulator to obtain Ni-W-ZrC microcrystal plating solution; and (3) pretreating a sample to be electroplated, then soaking the pretreated sample into the Ni-W-ZrC microcrystal plating solution, and then electroplating to obtain the Ni-W-ZrC microcrystal plating layer.
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