CN110438541B - Particle-doped composite gradient micro-arc oxidation coating, multistage preparation method and application - Google Patents
Particle-doped composite gradient micro-arc oxidation coating, multistage preparation method and application Download PDFInfo
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Abstract
The invention relates to a particle-doped composite gradient micro-arc oxidation coating, a multistage preparation method and application. The preparation method utilizes micro-arc oxidation technology to prepare a composite coating doped with heterogeneous particles on the metal surface in the electrolyte containing micro-particles, the particle content of the outer surface layer of the coating is higher than that of the core part, and the composite particles present the characteristic of gradient distribution in the micro-arc oxidation coating. The preparation method is to realize that the target coating decomposes the micro-arc oxidation process step by step, and the target coating is subjected to a series of stages of particle pre-adsorption, rapid coating growth, particle main adsorption, particle capture and compounding, coating roughness finishing and coating self-sealing hole in sequence, and the stubble pressing is carried out, so that the preparation of the high-quality composite coating with high density, low roughness and particle gradient distribution is finally realized. The invention can be compounded with high-hardness particles, self-lubricating particles, conductive particles, bioactive particles and the like according to the functional requirements of the target coating, and is applied to the field of surface treatment of metal materials.
Description
Technical Field
The invention belongs to the field of material surface treatment, and particularly relates to a particle-doped composite gradient micro-arc oxidation coating, a multistage preparation method and application.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Surface coating technology has long been a common means of modifying materials to impart or enhance properties not otherwise provided by the material. In recent years, micro-arc oxidation (MAO) technology has attracted great attention as a newly developed surface treatment technology, and can grow a ceramic film layer mainly comprising matrix metal oxide on the surface of valve metals such as aluminum, magnesium, titanium, zirconium and the like under the action of instantaneous high temperature and high pressure generated by arc discharge, and the film layer has the characteristics of high impedance, electrical insulation and the like, can greatly enhance the corrosion resistance of the alloy, and has a very good application prospect.
However, with the development of technological innovation and industrial process, integration and multi-functionalization of products are required more and more, and in order to achieve the purpose, a product workpiece is required to have multi-aspect functional expression. How to conveniently and reliably realize multiple functions of products is a trend of market development.
Although the micro-arc oxidation technology can enable light alloys such as magnesium, aluminum, titanium and the like to have better corrosion resistance, under certain practical conditions, the materials are required to have good corrosion resistance and special functions such as wear resistance, self-lubrication, electrical conductivity, electromagnetic shielding, catalytic activity, biological activity and the like which meet the specific service environment of the materials. According to market demands, the micro-arc oxidation technology is utilized to prepare the composite functional coating, which is a future development trend.
By utilizing the micro-arc oxidation technology, the multi-functionalization of the micro-arc oxidation coating can be realized by compounding heterogeneous particles such as high-hardness particles, self-lubricating particles, conductive particles, catalytic active particles, bioactive particles and the like in the coating. Research reports that ZrO is oxidized by micro-arc2、Al2O3、SiO2、SiC、TiN、MoS2、TiO2HA, Ag and other particles are compounded into the micro-arc oxidation film layer, so that the film layer can have the characteristics of wear resistance, self-lubrication, photocatalysis, biological activity, antibacterial property and the like besides the corrosion resistance. However, conventionally, heterogeneous particles in these composite coatings are characterized by being uniformly dispersed. In the actual use process of the material, more attention is paid to the surface characteristics of the material, for example, the wear resistance of the surface layer of the material is firstly improved to improve the wear resistance of the material, and the material is improvedThe catalytic properties are also of primary importance to improve the catalytic properties of the surface layer. The traditional uniformly doped composite coating cannot consider the actual use requirement of materials, thereby limiting the improvement of the performance of the composite coating.
In the past, when the micro-arc oxidation coating is prepared, researchers usually control parameters such as pulse voltage, frequency, duty ratio and the like to regulate the growth rate and the structure of the coating, which is a common technique for those skilled in the art, but the inventors found that: the method is essentially characterized in that the speed and the form of a newly generated oxidation product are controlled by regulating the magnitude of single-pulse discharge energy, and a high-quality composite coating with high density, low roughness and particle gradient distribution is difficult to prepare.
In addition, a set of multi-step combined process is obtained by combining magnetron sputtering, anodic oxidation, electrodeposition and other technologies with a micro-arc oxidation technology in parallel, but the preparation process is complicated, the equipment investment is large, and the practicability is not strong.
Disclosure of Invention
In order to overcome the problems, the invention provides a particle-doped composite gradient micro-arc oxidation coating, a multistage preparation method and application. The preparation method comprises the steps of decomposing the micro-arc oxidation process step by step, sequentially carrying out a series of steps of particle pre-adsorption, coating rapid growth, particle main adsorption, particle capture and compounding, coating roughness finishing and coating self-sealing hole, and carrying out stubble pressing, thereby finally obtaining the high-quality composite coating with high density, low roughness and particle gradient distribution.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a particle-doped composite gradient micro-arc oxidation coating comprises the following components in sequence from inside to outside: the particle pre-adsorption composite layer, the rapid growth layer, the high-content particle main adsorption composite layer and the surface finishing layer, wherein the particle content of the outer surface layer of the coating is higher than that of the core layer.
In the invention, the phrase "the particle content of the outer surface layer of the coating is higher than that of the core" means that: the highest particle content is mainly concentrated in the high-content particle main adsorption composite layer. In general, the relationship between the particle content is: the high-content particle main adsorption composite layer is larger than the particle pre-adsorption composite layer is larger than the rapid growth layer.
In the present invention, the fine particles mean: one or more types of heterogeneous particles added into the electrolyte and capable of endowing the micro-arc oxidation film layer with characteristics of wear resistance, self-lubrication, photocatalysis, biological activity, antibacterial property and the like can be adopted in some embodiments: ZrO (ZrO)2、Al2O3、SiO2、SiC、TiN、MoS2、TiO2HA or Ag.
The research of the invention finds that: the energy size, the continuous state and the positive and negative polarities of the single pulse are matched through targeted setting, so that the migration, trapping, compounding and vector movement of exogenous heterogeneous particles can be controlled. Based on the method, the micro-arc oxidation film layer is designed and prepared in a grading manner in the micro-arc oxidation process category, so that the particles are subjected to a series of stages of pre-adsorption, rapid coating growth, main particle adsorption, particle capture and compounding, coating roughness finishing and self-sealing of the coating, and stubble pressing is carried out, and finally the high-quality composite coating with high density, low roughness and particle gradient distribution is obtained.
In some embodiments, the sum of the thicknesses of the particle pre-adsorption composite layer, the rapid growth layer, the high-content particle main adsorption composite layer and the surface finishing layer is 20-100 μm, wherein the thickness of the rapid growth layer is not less than 50%, the thickness of the high-content particle main adsorption composite layer is 10-30%, the prepared coating has good compactness and roughness, and the function expression of the composite particles is enhanced.
The invention also provides a multistage preparation method of the particle-doped composite gradient micro-arc oxidation coating, which comprises the following steps:
the first step is as follows: placing the pretreated sample in an electrolyte containing micro-particles, and forming a loop system by taking the sample to be treated as an anode and stainless steel as a cathode;
the second step is that: preparation of a particle pre-adsorption composite layer: promoting the adsorption of particles on the surface of the sample, forming a dielectric layer and exciting spark discharge;
the third step: preparing a rapid growth layer: the micro-arc oxidation layer is enabled to grow rapidly to reach the preset thickness;
the fourth step: preparing a high-content particle main adsorption composite layer: promoting the adsorption of the particles on the surface of the coating, and enabling the particles adsorbed on the surface of the coating to be captured and compounded into the coating by the generated high-heat melt;
the fifth step: preparation of surface finish layer: the protruding tips on the surface of the coating and the particles which are not captured and compounded into the coating are weakened, the large discharge holes are sealed, and the micro-arc oxidation layer slowly grows.
The invention designs and prepares the composite gradient coating with heterogeneous particles presenting the gradient distribution characteristic, so that the heterogeneous particles are more intensively distributed on the surface layer of the material, the functional expression of the composite particles can be furthest enhanced, and the effect of good steel on the cutting edge is realized.
In some embodiments, the particle pre-adsorption composite layer is prepared under the following conditions: application of a positive pulse current, low voltage: 20-80V, high duty cycle: 70-90%, low frequency: 10-60 Hz, application time: 5-10 s. The adsorption of particles on the surface of the sample is promoted, a dielectric layer is quickly formed, and spark discharge is excited.
In some embodiments, the conditions for preparing the fast-growth layer are: application of a positive pulse current, high voltage: 300-600V, medium duty ratio: 15-50%, medium frequency: 200-800 Hz, application time: 180-600 s. The micro-arc oxidation layer is rapidly grown by utilizing continuous high-energy output to reach the preset thickness.
In some embodiments, the high content particle primary adsorption composite layer is prepared under the following conditions:
a. applying positive pulse current to the loop system, wherein the application process is as follows: 180-280V, high duty cycle: 70-90%, low frequency: 10-60 Hz, application time: 5-10 s; promoting the adsorption of the particles on the surface of the coating so as to improve the content of the particles in the outer surface layer of the composite coating.
b. Applying positive pulse current to the loop system, wherein the application process is high voltage: 300-600V, medium duty ratio: 15-50%, medium frequency: 200-800 Hz, application time: 20-40 s; so that the particles adsorbed on the surface of the coating are captured and compounded into the coating by the generated high-heat melt.
c. And (c) circularly performing the steps a and b, wherein the circulation times are 1-4.
In some embodiments, the surface finish layer is prepared under the conditions:
s1: applying negative pulse current to the loop system, medium and high voltage: 200-350V, low duty cycle: 3-10%, high frequency: 700-1500 Hz, application time: 0.5-5 s; by outputting high-frequency negative pulse micro energy, the protruding tips on the surface of the coating and particles which are not captured and compounded into the coating are weakened, and the roughness of the surface of the coating is reduced.
S2: applying positive pulse current to the loop system, wherein the application process is high voltage: 300-600V, medium-low duty ratio: 8-15%, medium-high frequency: 600-1000 Hz, application time: 15-20 s; the micro-arc oxidation layer slowly grows through output of slightly low energy, so that larger discharge holes are sealed, the density of the coating is improved, and the surface roughness of the coating is reduced.
S3: and (5) circularly performing the steps S1 and S2, wherein the number of the circulation is 1-6.
In some embodiments, the electrolyte has a composition of: 15-18 g/L of sodium hexametaphosphate, 5-8 g/L of sodium silicate, 3-5 g/L of sodium fluoride and 4-6 g/L of silicon dioxide particles;
in some embodiments, the electrolyte comprises 3-5 g/L sodium hexametaphosphate, 8-10 g/L potassium fluoride dihydrate, 5-8 g/L sodium hydroxide, 10-12 ml/L ethylene glycol, and 5-8 g/L nano-hydroxyapatite particles.
The invention also provides a particle-doped composite gradient micro-arc oxidation coating prepared by any one of the methods.
The invention also provides application of the particle-doped composite gradient micro-arc oxidation coating in the fields of military industry, aerospace, aviation, automobiles, textiles or machinery.
The invention has the beneficial effects that:
(1) the particle-doped composite gradient micro-arc oxidation coating not only realizes the basic functions of the micro-arc oxidation coating, but also can be compounded with high-hardness particles, self-lubricating particles, conductive particles, bioactive particles and the like according to the special function requirements of a target coating so as to prepare composite functional coatings such as a wear-resistant coating, an antifriction coating, a conductive coating, a bioactive coating and the like.
(2) The particle-doped composite gradient micro-arc oxidation coating is characterized in that the content of particles on the outer surface layer of the coating is higher than that of the core, the composite particles are in gradient distribution in the micro-arc oxidation coating, and the function expression of the composite particles can be enhanced to the maximum extent by designing the gradient distribution of the composite particles.
(3) According to the multistage preparation method of the particle-doped composite gradient micro-arc oxidation coating, the micro-arc oxidation process is decomposed step by step, and the micro-arc oxidation process is subjected to a series of stages of particle pre-adsorption, coating rapid growth, particle main adsorption, particle capture and compounding, coating roughness finishing and coating self-sealing hole sealing, stubble pressing and stubble progressive progression are performed, each stage is slow and ordered, the purpose is clear, the internal logic is correlated, and finally the preparation of the high-quality composite coating with high density (more than or equal to 90%), low roughness (Ra is less than or equal to 0.3 mu m) and particle gradient distribution can be realized.
(4) The method has the advantages of simple operation method, low cost, universality and easy large-scale production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a schematic structural diagram of a particle-doped composite gradient micro-arc oxidation coating prepared in embodiment 1 of the present invention.
The material comprises an alloy matrix 1, a particle pre-adsorption composite layer 2, a rapid growth layer 3, a high-content particle main adsorption composite layer 4 and a surface finishing layer 5.
FIG. 2 is a surface microtopography of the micro-arc oxidized composite gradient coating prepared in example 1.
FIG. 3 is a surface microtopography of the micro-arc oxidized coating prepared in comparative example 1.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, 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 invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As introduced in the background art, the problem that heterogeneous particles in the existing composite coating are uniformly dispersed, and the improvement of the performance of the coating is limited is solved. Therefore, the invention provides a particle-doped composite gradient micro-arc oxidation coating and a multistage preparation method, and the preparation method comprises the following steps:
(1) polishing, cleaning and airing a sample to be processed, placing the sample to be processed into an electrolyte containing micro-particles, constructing a loop system by taking the sample to be processed as an anode and stainless steel as a cathode, and performing micro-arc oxidation preparation;
(2) applying positive pulse current to the loop system, wherein the application process is low voltage: 20-80V, high duty cycle: 70-90%, low frequency: 10-60 Hz, application time: 5-10 s;
(3) applying positive pulse current to the loop system, wherein the application process is high voltage: 300-600V, medium duty ratio: 15-50%, medium frequency: 200-800 Hz, application time: 180-600 s;
(4) applying positive pulse current to the loop system, wherein the application process is as follows: 180-280V, high duty cycle: 70-90%, low frequency: 10-60 Hz, application time: 5-10 s;
(5) applying positive pulse current to the loop system, wherein the application process is high voltage: 300-600V, medium duty ratio: 15-50%, medium frequency: 200-800 Hz, application time: 20-40 s;
(6) circularly performing the steps (4) and (5), wherein the circulation frequency is 1-4;
(7) applying negative pulse current to the loop system, wherein the application process is medium-high voltage: 200-350V, low duty cycle: 3-10%, high frequency: 700-1500 Hz, application time: 0.5-5 s;
(8) applying positive pulse current to the loop system, wherein the application process is high voltage: 300-600V, medium-low duty ratio: 8-15%, medium-high frequency: 600-1000 Hz, application time: 15-20 s;
(9) and (5) circularly performing the steps (7) and (8) for 1-6 times.
(10) And taking out the treated sample and cleaning.
The step (2) is to promote the adsorption of particles on the surface of the sample, quickly form a dielectric layer and excite spark discharge.
Wherein, the step (3) aims to utilize continuous high-energy output to enable the micro-arc oxidation layer to grow rapidly to reach the preset thickness.
Wherein, the purpose of the step (4) is to promote the adsorption of the particles on the surface of the coating so as to increase the content of the particles in the outer surface layer of the composite coating.
Wherein, the purpose of the step (5) is to make the particles adsorbed on the surface of the coating trapped and compounded into the coating by the generated high-heat melt.
And (4) outputting high-frequency negative pulse micro energy to weaken the protrusion of the tip of the coating surface and particles which are not captured and compounded into the coating, and reducing the roughness of the coating surface.
Wherein, the purpose of the step (8) is to enable the micro-arc oxidation layer to slowly grow through output of slightly lower energy so as to seal larger discharge holes, improve the density of the coating and reduce the surface roughness of the coating.
The technical solution of the present invention will be described below with specific examples.
Example 1
Preparing an electrolyte, wherein the electrolyte comprises the following components: 15g/L of sodium hexametaphosphate, 5g/L of sodium silicate, 3g/L of sodium fluoride and 4g/L of silicon dioxide particles. The treatment is carried out according to the following steps:
(1) polishing, cleaning and airing a 6061 aluminum alloy sample to be treated, placing the 6061 aluminum alloy sample into the electrolyte, constructing a loop system by taking the sample to be treated as an anode and stainless steel as a cathode, and performing micro-arc oxidation preparation;
(2) applying positive pulse current to the loop system, wherein the application process is low voltage: 60V, high duty cycle: 80%, low frequency: 40Hz, application time: 10 s;
(3) applying positive pulse current to the loop system, wherein the application process is high voltage: 500V, medium duty cycle: 25%, medium frequency: 550Hz, application time: 500 s;
(4) applying positive pulse current to the loop system, wherein the application process is as follows: 250V, high duty cycle: 80%, low frequency: 40Hz, application time: 8 s;
(5) applying positive pulse current to the loop system, wherein the application process is high voltage: 520V, medium duty ratio: 25%, medium frequency: 550Hz, application time: 30 s;
(6) circularly performing the steps (4) and (5), wherein the circulation times are 2;
(7) applying negative pulse current to the loop system, wherein the application process is medium-high voltage: 300V, low duty cycle: 8%, high frequency: 1200Hz, application time: 3 s;
(8) applying positive pulse current to the loop system, wherein the application process is high voltage: 520V, medium and low duty cycle: 10%, medium-high frequency: 800Hz, application time: 20 s;
(9) and (5) circularly performing the steps (7) and (8) for 3 times.
(10) And taking out the treated sample and cleaning.
The surface layer of the treated sample is observed by a scanning electron microscope, the surface microscopic topography picture of the treated sample is shown in an attached drawing 2, the surface discharge holes on the surface of the sample are fewer, no large holes exist, no obvious protrusions exist, the surface is smooth and flat, the apparent density of the surface layer is 95 +/-2%, the surface roughness Ra is 0.203 mu m, and the coating hole sealing and finishing effects are excellent. The embodiment realizes the preparation of the silicon dioxide particle doped composite gradient micro-arc oxidation coating on the surface of the aluminum alloy.
Example 2
Preparing an electrolyte, wherein the electrolyte comprises the following components: 3g/L of sodium hexametaphosphate, 8g/L of potassium fluoride dihydrate, 5g/L of sodium hydroxide, 10ml/L of ethylene glycol and 5g/L of nano-hydroxyapatite particles. The treatment is carried out according to the following steps:
(1) polishing, cleaning and airing a pure magnesium sample to be treated, placing the pure magnesium sample into the electrolyte, constructing a loop system by using the sample to be treated as an anode and stainless steel as a cathode, and performing micro-arc oxidation preparation;
(2) applying positive pulse current to the loop system, wherein the application process is low voltage: 50V, high duty cycle: 70%, low frequency: 40Hz, application time: 8 s;
(3) applying positive pulse current to the loop system, wherein the application process is high voltage: 360V, medium duty cycle: 20%, medium frequency: 600Hz, application time: 360 s;
(4) applying positive pulse current to the loop system, wherein the application process is as follows: 200V, high duty cycle: 70%, low frequency: 40Hz, application time: 6 s;
(5) applying positive pulse current to the loop system, wherein the application process is high voltage: 380V, medium duty ratio: 20%, medium frequency: 600Hz, application time: 25 s;
(6) circularly performing the steps (4) and (5), wherein the circulation times are 3;
(7) applying negative pulse current to the loop system, wherein the application process is medium-high voltage: 220V, low duty cycle: 5%, high frequency: 1000Hz, application time: 3 s;
(8) applying positive pulse current to the loop system, wherein the application process is high voltage: 380V, medium-low duty ratio: 10%, medium-high frequency: 650Hz, application time: 15 s;
(9) and (5) circularly performing the steps (7) and (8) for 4 times.
(10) And taking out the treated sample and cleaning.
The observation of a scanning electron microscope shows that the surface of a sample has fewer discharge holes, no large holes and no obvious bulges, the surface is smooth and flat, the apparent density of the surface layer is 95 +/-2%, the surface roughness Ra is 0.285 mu m, and the sealing and finishing effects of the coating are excellent. The embodiment realizes the preparation of the magnesium alloy surface nano hydroxyapatite particle doped composite gradient micro arc oxidation coating.
Comparative example 1
An electrolyte was prepared, and the composition of the electrolyte was the same as in example 1. The treatment is carried out according to the following steps:
(1) polishing, cleaning and airing a 6061 aluminum alloy sample to be treated, placing the 6061 aluminum alloy sample into the electrolyte, constructing a loop system by taking the sample to be treated as an anode and stainless steel as a cathode, and performing micro-arc oxidation preparation;
(2) applying positive pulse current to the loop system, wherein the application process is as follows: 300V, duty ratio: 25%, frequency: 300Hz, application time: 40 s;
(3) applying positive pulse current to the loop system, wherein the application process is as follows: 550V, duty ratio: 25%, frequency: 550Hz, application time: 600 s;
(4) and taking out the treated sample and cleaning.
The surface layer of the treated sample is observed by a scanning electron microscope, the surface microscopic topography picture is shown in figure 3, and it can be observed that discharge holes are densely distributed on the surface of the sample, obvious oxide bulges can be seen, the apparent density of the surface layer is 60 +/-3%, and the surface roughness Ra is 1.472 mu m.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (4)
1. A particle-doped composite gradient micro-arc oxidation coating is characterized in that the coating sequentially comprises the following components from inside to outside: the particle pre-adsorption composite layer, the rapid growth layer, the high-content particle main adsorption composite layer and the surface finishing layer are arranged on the surface of the coating, and the particle content of the outer surface layer of the coating is higher than that of the core part of the coating;
the sum of the thicknesses of the coatings is 20-100 mu m, wherein the thickness of the rapid growth layer is not less than 50%, and the thickness of the high-content particle main adsorption composite layer is 10-30%;
the preparation method comprises the following steps:
the first step is as follows: placing the pretreated sample in an electrolyte containing micro-particles, and forming a loop system by taking the sample to be treated as an anode and stainless steel as a cathode;
the second step is that: preparation of a particle pre-adsorption composite layer: promoting the adsorption of particles on the surface of the sample, forming a dielectric layer and exciting spark discharge;
the third step: preparing a rapid growth layer: the micro-arc oxidation layer is enabled to grow rapidly to reach the preset thickness;
the fourth step: preparing a high-content particle main adsorption composite layer: promoting the adsorption of the particles on the surface of the coating, and enabling the particles adsorbed on the surface of the coating to be captured and compounded into the coating by the generated high-heat melt;
the fifth step: preparation of surface finish layer: weakening the tip bulge on the surface of the coating and particles which are not captured and compounded into the coating, sealing larger discharge holes and enabling the micro-arc oxidation layer to slowly grow;
the preparation conditions of the particle pre-adsorption composite layer are as follows: application of a positive pulse current, low voltage: 20-80V, high duty cycle: 70-90%, low frequency: 10-60 Hz, application time: 5-10 s;
the preparation conditions of the rapid growth layer are as follows: application of a positive pulse current, high voltage: 300-600V, medium duty ratio: 15-50%, medium frequency: 200-800 Hz, application time: 180-600 s;
the preparation conditions of the high-content particle main adsorption composite layer are as follows:
a. applying positive pulse current to the loop system, wherein the application process is as follows: 180-280V, high duty cycle: 70-90%, low frequency: 10-60 Hz, application time: 5-10 s;
b. applying positive pulse current to the loop system, wherein the application process is high voltage: 300-600V, medium duty ratio: 15-50%, medium frequency: 200-800 Hz, application time: 20-40 s;
c. circularly performing the step a and the step b, wherein the circulation times are 1-4;
the preparation conditions of the surface finishing layer are as follows:
s1: applying negative pulse current to the loop system, medium and high voltage: 200-350V, low duty cycle: 3-10%, high frequency: 700-1500 Hz, application time: 0.5-5 s;
s2: applying positive pulse current to the loop system, wherein the application process is high voltage: 300-600V, medium-low duty ratio: 8-15%, medium-high frequency: 600-1000 Hz, application time: 15-20 s;
s3: and (5) circularly performing the steps S1 and S2, wherein the number of the circulation is 1-6.
2. The particle-doped composite gradient micro-arc oxidation coating according to claim 1, wherein the electrolyte comprises: 15-18 g/L sodium hexametaphosphate, 5-8 g/L sodium silicate, 3-5 g/L sodium fluoride and 4-6 g/L silicon dioxide particles.
3. The particle-doped composite gradient micro-arc oxidation coating according to claim 1, wherein the electrolyte comprises: 3-5 g/L of sodium hexametaphosphate, 8-10 g/L of potassium fluoride dihydrate, 5-8 g/L of sodium hydroxide, 10-12 ml/L of ethylene glycol and 5-8 g/L of nano hydroxyapatite particles.
4. Use of the particle-doped composite gradient micro-arc oxidation coating according to any one of claims 1 to 3 in the fields of military industry, aerospace and automobile, textile or machinery.
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