CN108642544B - Method for preparing oxide film on surface of magnesium alloy by utilizing micro-arc oxidation - Google Patents

Method for preparing oxide film on surface of magnesium alloy by utilizing micro-arc oxidation Download PDF

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CN108642544B
CN108642544B CN201810531110.9A CN201810531110A CN108642544B CN 108642544 B CN108642544 B CN 108642544B CN 201810531110 A CN201810531110 A CN 201810531110A CN 108642544 B CN108642544 B CN 108642544B
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magnesium alloy
micro
arc oxidation
oxide film
electrolyte
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CN108642544A (en
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朱宏喜
任凤章
李全安
陈君
夏梁彬
谢云丁
朱亚聪
姚丽馨
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Henan University of Science and Technology
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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
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/30—Anodisation of magnesium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/024—Anodisation under pulsed or modulated current or potential
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/026—Anodisation with spark discharge

Abstract

A method for preparing oxide film on magnesium alloy surface by micro-arc oxidation comprises placing magnesium alloy in alkaline electrolysis apparatusIn the electrolytic bath of the liquid, magnesium alloy is used as an electrolytic anode, the electrolytic bath is used as an electrolytic cathode, voltage is applied to cause plasma discharge on the magnesium alloy, micro-arc oxidation is utilized to form an oxide film on the surface of the magnesium alloy, and the alkaline electrolyte comprises 8-12 g/L, Na NaOH2SiO310—15g/L、KF 6—8g/L、H2O22-3 mL/L, 6-8 mL/L of glycerol, 1-2 g/L of ethylene diamine tetramethylene phosphonic acid sodium and the balance of water; in the process of micro-arc oxidation, zeolite powder and gamma-alumina nano micro powder are sequentially added into the electrolyte, and then the micro-arc oxidation reaction is continued until the preparation of the oxide film is finished. The reaction process of micro-arc oxidation is influenced by the comprehensive action of a plurality of components, the number of micropores on the surface layer of the oxidation film is reduced, the compactness of the oxidation film is fundamentally improved, and the corrosion resistance is enhanced.

Description

Method for preparing oxide film on surface of magnesium alloy by utilizing micro-arc oxidation
Technical Field
The invention relates to a processing method of magnesium alloy, in particular to a method for preparing an oxide film on the surface of magnesium alloy by utilizing micro-arc oxidation.
Background
The magnesium and the magnesium alloy have the characteristics of small density, high specific strength and specific stiffness, good casting, welding, damping, shock absorption, cutting processing and dimensional stability and the like, are the metal structure materials with the most potential of light weight, environmental protection and performance optimization development, and are also one of the metal materials with the most application prospect in the twenty-first century. Since magnesium is an active metal, magnesium and magnesium alloys are very susceptible to corrosion during application, and the poor corrosion resistance severely limits the application of magnesium and magnesium alloys in various fields, the surface modification of magnesium and magnesium alloys becomes a research hotspot in recent years.
Micro-arc oxidation is a surface treatment technology for generating ceramic films on the surfaces of metals such as magnesium, aluminum, titanium and the like in situ, and ceramic oxide films are formed on the surfaces of the metals such as magnesium, aluminum, titanium and the like in situ by the combined action of thermochemistry, plasma chemistry and electrochemistry by adopting higher energy density. The formed film has the characteristics of good corrosion resistance, high wear resistance, good combination with a matrix and the like, and can greatly improve the corrosion resistance of metal. Since the properties of the ceramic membrane prepared by micro-arc oxidation, such as surface appearance, components, structure and corrosion resistance, are mainly determined by the composition of the electrolyte, the matrix material and electrical parameters, an oxide membrane with certain properties can be obtained by adjusting the above influence factors.
The electrolytes used for the magnesium alloy micro-arc oxidation treatment are roughly classified into acidic and alkaline electrolytes. The acidic electrolyte generally pollutes the environment, is easy to corrode products, and is rarely used. Weakly alkaline electrolytes have been the subject of major research. According to different main film forming elements, the electrolyte mainly comprises a phosphate system, a silicate system, an aluminate system and a composite electrolyte system. The phosphate is limited in practical use because it is harmful to human bodies and the environment to various degrees. The silicate system has higher film forming rate, and the obtained film has excellent hardness and wear resistance, but the corrosion resistance is slightly poorer than that of a phosphate system. The wear resistance of the film obtained by the aluminate system is better, the binding force between the film and the substrate is relatively better, but the film forming speed and the corrosion resistance are poorer.
However, no matter which electrolyte is adopted, due to the micro-arc oxidation mechanism, in the process of generating the oxide film, the oxide film generated at the initial stage is continuously broken down, the instantaneous high temperature causes the interface of the film layer and the solution to generate a large amount of water vapor, and meanwhile, the surface layer of the high-temperature melt is directly contacted with the solution and is solidified before the inner layer, so that the escape channel of the internal gas is closed, the escaped gas cannot escape until the next breakdown of the oxide film, and holes are formed. Therefore, the oxide film formed by micro-arc oxidation of the magnesium alloy generally comprises an inner dense layer and an outer loose layer. The loose layer on the outer side of the micro-arc oxidation film can lead corrosive media to enter the magnesium alloy matrix through the pores due to the pores formed by micro-discharge, and can increase the corrosion to the compact layer on the inner side of the oxidation film and the magnesium alloy matrix under the action of a long time.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and provide a method for preparing an oxide film on the surface of a magnesium alloy by utilizing micro-arc oxidation, which can reduce micropores on the oxide film and improve the compactness and the corrosion resistance of the oxide film.
The technical scheme adopted by the invention for solving the technical problems is as follows: a method for preparing an oxide film on the surface of magnesium alloy by utilizing micro-arc oxidation comprises the steps of placing the magnesium alloy in an electrolytic tank filled with alkaline electrolyte, taking the magnesium alloy as an electrolytic anode and the electrolytic tank as an electrolytic cathode, applying voltage to enable the magnesium alloy to generate plasma discharge, and forming the oxide film on the surface of the magnesium alloy by utilizing micro-arc oxidation, wherein the alkaline electrolyte comprises 8-12 g/L, Na NaOH2SiO310—15g/L、KF 6—8g/L、H2O22-3 mL/L, 6-8 mL/L of glycerol, 1-2 g/L of ethylene diamine tetramethylene phosphonic acid sodium and the balance of water; in the process of micro-arc oxidation, zeolite powder and gamma-alumina nano micro powder are sequentially added into the electrolyte, and then the micro-arc oxidation reaction is continued until the preparation of the oxide film is finished.
After voltage is applied and micro-arc oxidation reaction is started for 5-10 minutes, firstly adding zeolite powder into the electrolyte, continuing the reaction for 5-10 minutes, then adding gamma-alumina nano micro powder into the electrolyte, and continuing the reaction for 5-10 minutes to form an oxide film on the surface of the magnesium alloy.
The addition amount of the zeolite powder is 0.5-1% of the weight of the electrolyte, and the addition amount of the gamma-alumina nano micro powder is 1-2% of the weight of the electrolyte.
Applying voltage to the electrolytic anode and the electrolytic cathode by adopting a pulse power supply, wherein the current density is 5mA/cm2～40mA/cm2The frequency range is 100 Hz-500 Hz, and the duty ratio is 10% -30%.
In the process of micro-arc oxidation, the temperature in the electrolytic bath is controlled to be 30-40 ℃.
Before the magnesium alloy is put into an electrolytic bath, the surface of the magnesium alloy is cleaned by alkaline solution or sodium gluconate and then cleaned by water.
The invention has the beneficial effects that: the tip discharge can be well inhibited by adding the glycerol into the electrolyte, so that the micro-arc oxidation process is stabilized, and the micropores of an oxidation film are reduced; KF can increase the conductivity of the electrolyte and the density of the film layer, reduce the voltage, reduce the aperture and the surface roughness of the film layer and enhance the surface hardness and the wear resistance of the film; the ethylene diamine tetramethylene sodium phosphonate can be uniformly dispersed in the electrolyte, promotes the combination of metal elements in the magnesium alloy and film forming elements in the electrolyte in the micro-arc oxidation process, regulates the generation rate of an oxide film and reduces pores in the oxide film. The reaction process of micro-arc oxidation is influenced by the comprehensive action of several components, and the number of micropores on the surface layer of the oxide film is reduced.
Furthermore, in the micro-arc oxidation process, zeolite powder is added into the electrolyte to inhibit the formation and growth of holes and microcracks in the oxide film in the micro-arc oxidation process; the added gamma-alumina nanometer micro powder can increase the conductivity of the solution, and can be deposited on the micropores and the surface of the film layer due to good dispersibility, so that the appearance of the film layer is improved, the surface is smoother, the compactness of the oxide film is fundamentally improved, and the corrosion resistance is enhanced.
Drawings
FIG. 1 is a graph of corrosion rate of magnesium alloy samples in salt spray experiments as a function of corrosion time.
FIG. 2 is a SEM photograph of the surface of a magnesium alloy sample of a control group.
FIG. 3 is a SEM photograph of the surface of a magnesium alloy sample in example 1.
FIG. 4 is a SEM photograph of the surface of a magnesium alloy sample in example 2.
Detailed Description
The technical scheme of the invention is clearly and completely described below with reference to the accompanying drawings and the detailed description. The specific contents listed in the following examples are not limited to the technical features necessary for solving the technical problems to be solved by the technical solutions described in the claims. Meanwhile, the list is that the embodiment is only a part of the present invention, and not all embodiments.
Before micro-arc oxidation, pretreatment can be carried out, the surface of the magnesium alloy is cleaned by alkaline solution or sodium gluconate to remove oil, and then the magnesium alloy is cleaned by water. After pretreatment, the magnesium alloy is firstly placed in an electrolytic tank filled with alkaline electrolyte, the magnesium alloy is used as an electrolytic anode, and the electrolytic tank is used as an electrolytic cathode. The electrolytic bath can be made of stainless steel, and the micro-arc oxidation can be powered by a direct current power supply, an alternating current power supply or a pulse power supply. The invention preferably adopts a pulse power supply, the frequency range is 100 Hz-500 Hz, and the duty ratio is 10% -30%. Applying voltage to the electrolytic anode and the electrolytic cathode to generate plasma discharge on the magnesium alloy, wherein the current density is 5mA/cm2～40mA/cm2. Forming an oxide film on the surface of the magnesium alloy in a micro-arc oxidation mode, and controlling the temperature in the electrolytic bath to be 30-40 ℃ in the process.
The component of the alkaline electrolyte used for the micro-arc oxidation of the invention is preferably NaOH 8-12 g/L, Na2SiO310—15g/L、KF 6—8g/L、H2O2(30%) 2-3 mL/L, glycerine 6-8 mL/L, ethylenediamine tetramethylene phosphonic acid sodium 1-2 g/L and the rest is water.
The NaOH is used for adjusting pH, increasing conductivity and reducing arcing voltage; na (Na)2SiO3As a film forming agent, SiO plays a role in passivation3 2-But also can improve the conductivity of the solution and play the role of a conductive agent. KF can increase the conductivity of the electrolyte and the density of the film layer, reduce the voltage, reduce the aperture and the surface roughness of the film layer and enhance the surface hardness and the wear resistance of the film; h2O2O necessary for film formation2The film forming speed and the film thickness are improved. The glycerol can better inhibit point discharge, thereby stabilizing the micro-arc oxidation process and reducing the micropores of the oxidation film. The ethylene diamine tetramethylene sodium phosphonate can be uniformly dispersed in the electrolyte, promotes the combination of metal elements in the magnesium alloy and film forming elements in the electrolyte in the micro-arc oxidation process, regulates the generation rate of an oxide film and reduces pores in the oxide film.
In order to further improve the appearance characteristic of an oxidation film generated by micro-arc oxidation and reduce the number of micropores, the method adds zeolite powder into the electrolyte after the micro-arc oxidation reaction is carried out for 5-10 minutes by applying voltage, adds gamma-alumina nano micro powder into the electrolyte after the reaction is continued for 5-10 minutes, and continues the reaction for 5-10 minutes to form the oxidation film on the surface of the magnesium alloy. Wherein, the adding amount of the zeolite powder is 0.5-1% of the weight of the electrolyte, and the adding amount of the gamma-alumina nano micro powder is 1-2% of the weight of the electrolyte. The zeolite powder inhibits the formation and growth of holes and microcracks in an oxidation film in the micro-arc oxidation process; the added gamma-alumina nanometer micropowder can increase the conductivity of the solution, and can be deposited on micropores and the surface of the film layer due to good dispersibility, so that the appearance of the film layer is improved, and the surface is smoother.
The zeolite powder and the gamma-alumina nanopowder are preferably added under stirring so that they are repeatedly dispersed in the electrolyte. For this purpose, a stirring device may be provided in the electrolytic cell used to mix and stir the electrolyte. The electrolytic cell may be coupled to a heat exchange device such that an electrolyte flows between the electrolytic cell and the heat exchange device to control the temperature during the micro-arc oxidation process.
The micro-arc oxidation film formed on the surface of the magnesium alloy by adopting the electrolyte and the micro-arc oxidation mode has the main component of Mg2SiO4、MgO、MgF2And Mg3Al2Si3O12The spinel-type oxide has good compactness, flat and smooth surface, small number of micropores, small pore diameter, higher wear resistance and hardness, and can effectively improve the corrosion resistance of the magnesium alloy.
Example 1
The magnesium alloy is cleaned by alkali solution to remove the surface oil, and then is cleaned by water. The magnesium alloy is placed in an electrolytic cell, and the electrolyte component in the electrolytic cell is NaOH 10g/L, Na2SiO315g/L、KF 6g/L、H2O2(30%) 3mL/L, glycerol 6mL/L, ethylenediamine tetramethylene phosphonic acid sodium 2g/L, and the balance of water. Applying voltage to the electrolysis anode and the electrolysis cathode by adopting a pulse power supply with the frequency of 400 Hz and the duty ratio of 15 percent to ensure that plasma discharge occurs on the magnesium alloy, controlling the temperature in the electrolytic cell to be 35 ℃ in the process, continuously reacting for 45 minutes, and introducingAnd forming an oxide film on the surface of the magnesium alloy in a micro-arc oxidation mode.
Example 2
The magnesium alloy is cleaned by alkali solution to remove the surface oil, and then is cleaned by water. The magnesium alloy is placed in an electrolytic cell, and the electrolyte component in the electrolytic cell is NaOH 10g/L, Na2SiO315g/L、KF 6g/L、H2O2(30%) 3mL/L, glycerol 6mL/L, ethylenediamine tetramethylene phosphonic acid sodium 2g/L, and the balance of water. Applying voltage to an electrolysis anode and an electrolysis cathode by adopting a pulse power supply with the frequency of 400 Hz and the duty ratio of 15 percent to ensure that plasma discharge occurs on the magnesium alloy, controlling the temperature in an electrolytic cell to be 35 ℃ in the process, adding zeolite powder into the electrolyte after reacting for 10 minutes, adding gamma-alumina nano micro powder into the electrolyte after continuously reacting for 10 minutes, and continuously reacting for 10 minutes to ensure that an oxide film is formed on the surface of the magnesium alloy. The addition amount of the zeolite powder is 0.5 percent of the weight of the electrolyte, and the addition amount of the gamma-alumina nano micro powder is 1 percent of the weight of the electrolyte.
Example 3
The magnesium alloy is cleaned by alkali solution to remove the surface oil, and then is cleaned by water. The magnesium alloy is placed in an electrolytic cell, and the electrolyte component in the electrolytic cell is NaOH 10g/L, Na2SiO315g/L、KF 6g/L、H2O2(30%) 3mL/L, glycerol 6mL/L, ethylenediamine tetramethylene phosphonic acid sodium 2g/L, and the balance of water. Applying voltage to an electrolysis anode and an electrolysis cathode by adopting a pulse power supply with the frequency of 400 Hz and the duty ratio of 15 percent to ensure that plasma discharge occurs on the magnesium alloy, controlling the temperature in an electrolytic cell to be 35 ℃ in the process, adding zeolite powder into the electrolyte after reacting for 10 minutes, adding gamma-alumina nano micro powder into the electrolyte after continuously reacting for 10 minutes, and continuously reacting for 10 minutes to ensure that an oxide film is formed on the surface of the magnesium alloy. The addition amount of the zeolite powder is 0.5 percent of the weight of the electrolyte, and the addition amount of the gamma-alumina nano micro powder is 1 percent of the weight of the electrolyte.
Example 4
The magnesium alloy is cleaned by alkali solution to remove the surface oil, and then is cleaned by water. Placing the magnesium alloy in an electrolytic tank, wherein the electrolyte in the electrolytic tank contains NaOH 8g/L、Na2SiO310g/L、KF 7g/L、H2O2(30%) 2mL/L, glycerol 6mL/L, sodium ethylene diamine tetramethylene phosphonate 2g/L, and the balance of water. Applying voltage to an electrolysis anode and an electrolysis cathode by adopting a pulse power supply with the frequency of 300 Hz and the duty ratio of 30 percent to ensure that plasma discharge occurs on the magnesium alloy, controlling the temperature in an electrolytic cell to be 30 ℃ in the process, adding zeolite powder into the electrolyte after reacting for 8 minutes, adding gamma-alumina nano micro powder into the electrolyte after continuously reacting for 8 minutes, and continuously reacting for 8 minutes to ensure that an oxide film is formed on the surface of the magnesium alloy. The addition amount of the zeolite powder is 0.8 percent of the weight of the electrolyte, and the addition amount of the gamma-alumina nano micro powder is 1.5 percent of the weight of the electrolyte.
Example 5
The magnesium alloy is cleaned by alkali solution to remove the surface oil, and then is cleaned by water. The magnesium alloy is placed in an electrolytic cell, and the electrolyte component in the electrolytic cell is NaOH 12g/L, Na2SiO315g/L、KF 8g/L、H2O2(30%) 3mL/L, glycerol 8mL/L, ethylenediamine tetramethylene phosphonic acid sodium 1g/L, and the balance of water. Applying voltage to an electrolysis anode and an electrolysis cathode by adopting a pulse power supply with the frequency of 100Hz and the duty ratio of 10 percent to ensure that plasma discharge occurs on the magnesium alloy, controlling the temperature in an electrolytic cell to be 40 ℃ in the process, adding zeolite powder into the electrolyte after reacting for 10 minutes, adding gamma-alumina nano micro powder into the electrolyte after continuously reacting for 10 minutes, and continuously reacting for 5 minutes to ensure that an oxide film is formed on the surface of the magnesium alloy. The addition amount of the zeolite powder is 1 percent of the weight of the electrolyte, and the addition amount of the gamma-alumina nano micro powder is 2 percent of the weight of the electrolyte.
Example 6
The magnesium alloy is cleaned by alkali solution to remove the surface oil, and then is cleaned by water. The magnesium alloy is placed in an electrolytic cell, and the electrolyte component in the electrolytic cell is NaOH 12g/L, Na2SiO312g/L、KF 8g/L、H2O2(30%) 3mL/L, glycerol 7mL/L, sodium ethylene diamine tetramethylene phosphonate 2g/L, and the balance of water. Applying voltage to the electrolytic anode and the electrolytic cathode by adopting a pulse power supply with the frequency of 500Hz and the duty ratio of 15 percent to generate plasma on the magnesium alloyAnd (3) performing sub-discharge, wherein the temperature in the electrolytic cell is controlled to be 35 ℃ in the process, after the reaction is carried out for 5 minutes, adding zeolite powder into the electrolyte, after the reaction is continued for 5 minutes, adding gamma-alumina nano micro powder into the electrolyte, and continuing the reaction for 10 minutes to form an oxide film on the surface of the magnesium alloy. The addition amount of the zeolite powder is 1 percent of the weight of the electrolyte, and the addition amount of the gamma-alumina nano micro powder is 2 percent of the weight of the electrolyte.
The magnesium alloy AZ91D is used as a sample, and the corrosion resistance of the treated sample is tested by a grouping test method. The chemical composition of the die-cast AZ91D magnesium alloy is shown in the following table (mass fraction%):
Al Mn Zn Si Cu Ni Fe Mg
8.5—9.5 0.17—0.40 0.45—0.90 0.05 0.25 0.001 0.004 balance of
The AZ91D magnesium alloy was divided into 2 experimental groups, and experimental group 1 prepared an oxide film in the manner of example 1. Experimental group 2 an oxide film was prepared in the manner of example 2. Another group of AZ91D magnesium alloy is taken as a control group, and NaOH 8g/L, Na is adopted as the component2SiO315g/L, KF 6g/L, 30% H2O22mL/L and the balance of water, and generating an oxide film by micro-arc oxidation, wherein a surface SEM photograph is shown in figure 2.
According to GB/T10125-1997 salt spray experiment for artificial atmosphere corrosion experiments, all groups of samples are sealed at four sides by organic protective glue and then are placed into a salt spray experiment box after being sealed, wherein the temperature in the box is 35 +/-2 ℃, and NaCl with the mass concentration of 5% is used as a corrosion medium for continuous spraying. And observing the corrosion condition of the surface of the sample in the spraying process. The corrosion rate of each group as a function of spray time is shown in FIG. 1.
And after spraying for 240h, the corrosion resistance level is evaluated according to GB5944-86, a large number of corrosion spots are distributed on the whole surface of the control group sample, and the corrosion resistance level is evaluated as 6. A small number of spots are uniformly distributed on the surface of the sample of the experimental group 1, and the corrosion resistance rating is 7. The surface of the sample of the experimental group 2 is sporadically distributed with corrosion points, and the corrosion resistance grade is evaluated as 8 grade.
From the experimental results, the electrolyte component and the zeolite powder and the gamma-alumina nano micro powder added in the micro-arc oxidation process can improve the corrosion resistance of the magnesium alloy to different degrees.
The above description of the specific embodiments is only for the purpose of helping understanding the technical idea of the present invention and the core idea thereof, and although the technical solution is described and illustrated herein using the specific preferred embodiments, it should not be construed as limiting the present invention itself. Various changes in form and detail may be made therein by those skilled in the art without departing from the technical spirit of the present invention. Such modifications and substitutions are intended to be included within the scope of the present invention.

Claims (5)

1. A method for preparing an oxide film on the surface of magnesium alloy by utilizing micro-arc oxidation is characterized in that the magnesium alloy is placed in an electrolytic tank filled with alkaline electrolyte, the magnesium alloy is used as an electrolytic anode, the electrolytic tank is used as an electrolytic cathode, voltage is applied to enable the magnesium alloy to generate plasma discharge, and the oxide film is formed on the surface of the magnesium alloy by utilizing the micro-arc oxidation, and the method is characterized in that: the alkaline electrolyte comprises 8-12 g/L, Na of NaOH2SiO310—15g/L、KF 6—8g/L、H2O22-3 mL/L, 6-8 mL/L of glycerol, 1-2 g/L of ethylene diamine tetramethylene phosphonic acid sodium and the balance of water; in the process of micro-arc oxidation, zeolite powder and gamma-alumina nano micro powder are sequentially added into the electrolyte, and then micro-arc oxidation reaction is continued until the preparation of an oxide film is finished;
the addition amount of the zeolite powder is 0.5-1% of the weight of the electrolyte, and the addition amount of the gamma-alumina nano micro powder is 1-2% of the weight of the electrolyte.
2. The method for preparing the oxide film on the surface of the magnesium alloy by using the micro-arc oxidation according to claim 1, wherein the method comprises the following steps: after voltage is applied and micro-arc oxidation reaction is started for 5-10 minutes, firstly adding zeolite powder into the electrolyte, continuing the reaction for 5-10 minutes, then adding gamma-alumina nano micro powder into the electrolyte, and continuing the reaction for 5-10 minutes to form an oxide film on the surface of the magnesium alloy.
3. The method for preparing the oxide film on the surface of the magnesium alloy by using the micro-arc oxidation as claimed in claim 1 or 2, wherein: applying voltage to the electrolytic anode and the electrolytic cathode by adopting a pulse power supply, wherein the current density is 5mA/cm2～40mA/cm2The frequency range is 100 Hz-500 Hz, and the duty ratio is 10% -30%.
4. The method for preparing the oxide film on the surface of the magnesium alloy by using the micro-arc oxidation as claimed in claim 1 or 2, wherein: in the process of micro-arc oxidation, the temperature in the electrolytic bath is controlled to be 30-40 ℃.
5. The method for preparing the oxide film on the surface of the magnesium alloy by using the micro-arc oxidation as claimed in claim 1 or 2, wherein: before the magnesium alloy is put into an electrolytic bath, the surface of the magnesium alloy is cleaned by alkaline solution or sodium gluconate and then cleaned by water.
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