CN114561635A - LDHs film on surface of magnesium alloy and in-situ crystallization preparation method thereof - Google Patents
LDHs film on surface of magnesium alloy and in-situ crystallization preparation method thereof Download PDFInfo
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- CN114561635A CN114561635A CN202210065182.5A CN202210065182A CN114561635A CN 114561635 A CN114561635 A CN 114561635A CN 202210065182 A CN202210065182 A CN 202210065182A CN 114561635 A CN114561635 A CN 114561635A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/78—Pretreatment of the material to be coated
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses an in-situ crystallization preparation method of an LDHs film on the surface of a magnesium alloy, which comprises the following steps: s1: pretreating a magnesium alloy substrate; s2: soaking the magnesium alloy substrate treated in the step S1 in a precursor solution for pretreatment; the solute of the precursor solution is aluminum nitrate, magnesium nitrate, trisodium citrate, potassium sodium tartrate and tetrasodium ethylene diamine tetraacetate, and the solvent is water. S3: adjusting the pH value of the precursor solution in the step S2 to 9-12, and placing the magnesium alloy substrate treated in the step S2 in the precursor solution after the pH value is adjusted to continue dipping treatment; s4: and (4) washing the surface of the magnesium alloy with the LDHs film obtained after the treatment of the step S3 with deionized water, and drying with hot air. The preparation method has simple process and low energy consumption, can be used for large-area production, and the prepared LDHs film has a sheet-shaped laminate structure, high film compactness and better corrosion resistance.
Description
Technical Field
The invention belongs to the technical field of surface treatment of magnesium alloy, and particularly relates to an LDHs film on the surface of magnesium alloy and an in-situ crystallization preparation method thereof.
Background
The characteristics of high specific strength, good castability and low density (about 1/3 for titanium alloy) of magnesium alloy make it possible to produce magnesium alloy in high-tech products such as: aerospace parts, automotive industry, computer industry, and sporting goods, mobile phones, home appliances, etc. are widely used in daily life. However, magnesium alloys have a high chemical activity, resulting in poor corrosion resistance, and thus have limited applications.
In order to improve the corrosion resistance of magnesium alloy, various magnesium alloy corrosion resistant coatings, such as chemical conversion coating, micro-arc oxidation coating, polymer coating, electrochemical deposition coating, plasma electrolytic oxidation coating, super-hydrophobic coating, laser surface treatment coating, and the like, have been prepared. The chemical conversion film can be synthesized in situ on the surface of the metal substrate, so that the good binding force is shown, and meanwhile, the technology is simple in process, low in energy consumption and free from the limitation of the size and the shape of a workpiece, so that the chemical conversion film is generally applied to the field of metal corrosion prevention. In the prior chemical conversion process of the magnesium alloy surface, a chemical conversion coating generated by adopting chromate has relatively excellent corrosion resistance and good bonding force with a matrix. However, chromate contains Cr6+And the ions have carcinogenicity and teratogenicity on human bodies. There is therefore a need to find new environmentally friendly conversion coatings that can replace chromate conversion coatings.
Layered double hydroxides (LDH or LDHs) LDHs are anionic intercalation materials with general formula of [ M2+1-x M3+ x (OH)2]x+(An-)x/n·m H2O, wherein M2+And M3+Represents a cation occupying octahedral pores in the lamellar layer, An-Represents interlayer charge compensation anion, n is charge of interlayer anion, M is number of water molecule, and x represents M3+/(M2++M3+) In a molar ratio of (a). The existing research shows that: the LDHs film has simple preparation process, good physical barrier effect and unique interlayer anion exchange capacity, and can be capturedThe corrosion resistance of the magnesium alloy is greatly improved by the corrosive anions, so that the magnesium alloy is widely concerned in the field of corrosion protection. Most of the existing methods for preparing LDHs films adopt a hydrothermal method, but the hydrothermal method requires a high-temperature and high-pressure environment, so that the equipment requirement is high and the energy consumption is high.
Disclosure of Invention
The invention aims to solve the technical problems and provides an LDHs film in-situ crystallization preparation method which is simple in process, low in energy consumption and capable of being used for large-area production of magnesium alloy surfaces.
In order to realize the aim, the invention provides an in-situ crystallization preparation method of an LDHs film on the surface of a magnesium alloy, which comprises the following steps:
s1: pretreating a magnesium alloy substrate;
s2: soaking the magnesium alloy substrate treated in the step S1 in a precursor solution for pretreatment; the solute of the precursor solution is aluminum nitrate, magnesium nitrate, trisodium citrate, potassium sodium tartrate and tetrasodium ethylene diamine tetraacetate, and the solvent is water.
S3: adjusting the pH value of the precursor solution in the step S2 to 9-12, and placing the magnesium alloy substrate treated in the step S2 in the precursor solution after the pH value is adjusted to continue dipping treatment;
s4: and (4) washing the surface of the magnesium alloy with the LDHs film obtained after the treatment of the step S3 with deionized water, and drying with hot air.
Compared with the prior art, the LDHs film can be obtained on the surface of the magnesium alloy by simple immersion under the conditions of normal temperature and normal pressure by adopting an in-situ crystallization method, and the LDHs film obtained by adopting the preparation method has the same layered structure and composition as LDHs films obtained by a hydrothermal method and an electrodeposition method, and has higher corrosion resistance. The preparation method has simple process and low energy consumption, can be used for large-area production, and the LDHs film obtained by the preparation method has a sheet-shaped laminate structure, high film compactness and better corrosion resistance.
Preferably, in step S2, the solute in the precursor solution has the following concentration by mass: 0.1-0.5 mol/L, and the concentration of magnesium nitrate is as follows: 0.05-0.25 mol/L, wherein the concentration of trisodium citrate is as follows: 0.01-0.05 mol/L, wherein the concentration of potassium sodium tartrate is as follows: 0.01-0.05 mol/L, wherein the concentration of the ethylenediaminetetraacetic acid tetrasodium salt is as follows: 0.04 to 0.2 mol/L.
Preferably, in step S2, the temperature of the pretreatment is 20-50 ℃ and the pretreatment time is 10-30 min.
Preferably, in step S1, the pre-treatment includes a pre-coating and a polishing cleaning treatment.
Preferably, in step S1, the early coating step is: the magnesium alloy substrate is coated with polytetrafluoroethylene, and only the surface of the magnesium alloy with the exposed thickness of 1cm2 is used for post-treatment and corrosion resistance test.
Preferably, in step S1, the grinding, polishing and cleaning process includes the following steps: the magnesium alloy substrate is respectively polished by sand paper of 200 meshes, 400 meshes, 800 meshes, 1200 meshes and 2000 meshes, and Al with the particle size of 2.5-5 mu m is adopted2O3Polishing the polished magnesium alloy substrate by using the polishing powder, and finally, removing oil and cleaning by using absolute ethyl alcohol and deionized water, and drying by blowing.
Preferably, in step S3, the pH value of the precursor solution in step S2 is adjusted by using a sodium hydroxide solution with a concentration of 1-5 mol/L.
Preferably, in step S3, the temperature of the dipping treatment is 25-65 ℃, and the treatment time is 1-6 h.
Preferably, in step S4, the drying temperature of the hot air is 40-80 ℃, and the drying time is 0.5-3 h.
The invention also provides the LDHs film prepared by the in-situ crystallization preparation method of the LDHs film on the surface of the magnesium alloy.
The invention provides an in-situ crystallization preparation method of an LDHs film on a magnesium alloy surface, which has low energy consumption and simple process. The preparation method has simple process and low energy consumption, and can be used for large-area production; and the prepared LDHs film has a sheet-shaped laminate structure, and the film has high compactness and good corrosion resistance.
Drawings
FIG. 1 is an SEM photograph of LDHs film on the surface of the magnesium alloy prepared in example 1
FIG. 2 is a diagram showing the impedance of the finished products of the examples and comparative examples in the low frequency region when they are immersed in a 3.5 wt.% NaCl solution
FIG. 3 is a graph showing the polarization curves of the finished products of the examples and comparative examples when they are immersed in 3.5 wt.% NaCl solution
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations or modifications made based on the present invention are intended to be within the scope of the present invention.
Example 1:
preparing the LDHs film on the surface of the magnesium alloy by adopting an in-situ crystallization method according to the following steps:
first, the selected exposed surface area was set to 1cm2The magnesium alloy electrode adopts 200 meshes, 400 meshes, 800 meshes, 1200 meshes and 2000 meshes of sand paper and 2.5 mu m of Al2O3Polishing the polishing powder, removing oil by using absolute ethyl alcohol and secondary deionized water, cleaning and drying; then the treated magnesium alloy electrode is put in a precursor water solution consisting of 0.1mol/L of aluminum nitrate, 0.5mol/L of magnesium nitrate, 0.01mol/L of trisodium citrate (metal ion complexing agent), 0.01mol/L of potassium sodium tartrate and 0.05mol/L of ethylenediaminetetraacetic acid tetrasodium salt, and is pretreated for 10min at the temperature of 20 ℃; then, adjusting the pH value of the precursor solution to 9 by using 1mol/L sodium hydroxide, and continuously soaking the magnesium alloy in the precursor solution for 6 hours at the soaking temperature of 65 ℃; finally, washing the magnesium alloy LDHs membrane electrode obtained by dipping with secondary deionized water, and drying in hot air at 25 ℃ for 3 h. The surface topography of the LDHs film on the surface of the magnesium alloy obtained in this example is shown in fig. 1.
Example 2:
preparing the LDHs film on the surface of the magnesium alloy by adopting an in-situ crystallization method according to the following steps:
first, the selected exposed surface area was set to 1cm2The magnesium alloy electrode adopts 200-mesh, 400-mesh, 800-mesh, 1200-mesh and 2000-mesh sandpaper and 2.5 mu m Al respectively2O3Polishing the polishing powder, removing oil by using absolute ethyl alcohol and secondary deionized water, cleaning and blow-drying; then, the treated magnesium alloy electrode is put into a precursor water solution consisting of 0.2mol/L of aluminum nitrate, 0.25mol/L of magnesium nitrate, 0.01mol/L of trisodium citrate, 0.01mol/L of potassium sodium tartrate and 0.2mol/L of ethylenediaminetetraacetic acid tetrasodium salt, and is pretreated for 30min at the temperature of 50 ℃; then 2mol/L sodium hydroxide is used for adjusting the pH value of the precursor solution to 12, and the magnesium alloy is continuously put into the precursor solution for soaking for 6 hours at the soaking temperature of 35 ℃; finally, washing the magnesium alloy LDHs membrane electrode obtained by dipping with secondary deionized water, and drying in hot air at 50 ℃ for 3 h.
Example 3:
preparing the LDHs film on the surface of the magnesium alloy by adopting an in-situ crystallization method according to the following steps:
first, the selected exposed surface area was set to 1cm2The magnesium alloy electrode adopts 200 meshes, 400 meshes, 800 meshes, 1200 meshes and 2000 meshes of sand paper and 2.5 mu m of Al2O3Polishing the polishing powder, removing oil by using absolute ethyl alcohol and secondary deionized water, cleaning and drying; then, the treated magnesium alloy electrode is put into a precursor water solution consisting of 0.25mol/L aluminum nitrate, 0.4mol/L magnesium nitrate, 0.02mol/L trisodium citrate, 0.02mol/L potassium sodium tartrate and 0.1mol/L ethylene diamine tetraacetic acid tetrasodium salt, and is pretreated for 20min at the temperature of 35 ℃; then, 2mol/L sodium hydroxide is used for adjusting the pH value of the precursor solution to 11, and the magnesium alloy is continuously put into the precursor solution for soaking for 1 hour at the soaking temperature of 40 ℃; finally, washing the magnesium alloy LDHs membrane electrode obtained by dipping with secondary deionized water, and drying in hot air at 50 ℃ for 0.5 h.
Example 4:
preparing the LDHs film on the surface of the magnesium alloy by adopting an in-situ crystallization method according to the following steps:
first, the selected exposed surface area was set to 1cm2The magnesium alloy electrodes of (1) are respectively 200 meshes and 400 meshes800 mesh, 1200 mesh, 2000 mesh sandpaper and 2.5 μm Al2O3Polishing the polishing powder, removing oil by using absolute ethyl alcohol and secondary deionized water, cleaning and drying; then, the treated magnesium alloy electrode is put into a precursor water solution consisting of 0.2mol/L of aluminum nitrate, 0.25mol/L of magnesium nitrate, 0.01mol/L of trisodium citrate, 0.01mol/L of potassium sodium tartrate and 0.2mol/L of ethylenediaminetetraacetic acid tetrasodium salt, and is pretreated for 30min at the temperature of 50 ℃; then, 2mol/L sodium hydroxide is used for adjusting the pH value of the precursor solution to 12, and the magnesium alloy is continuously put into the precursor solution to be soaked for 6 hours at the soaking temperature of 35 ℃; finally, washing the magnesium alloy LDHs membrane electrode obtained by dipping with secondary deionized water, and drying in hot air at 50 ℃ for 3 h.
Example 5:
preparing the LDHs film on the surface of the magnesium alloy by adopting an in-situ crystallization method according to the following steps:
first, the selected exposed surface area was set to 1cm2The magnesium alloy electrode adopts 200 meshes, 400 meshes, 800 meshes, 1200 meshes and 2000 meshes of sand paper and 5 mu m of Al2O3Polishing the polishing powder, removing oil by using absolute ethyl alcohol and secondary deionized water, cleaning and drying; then, the treated magnesium alloy electrode is put into a precursor water solution consisting of 0.05mol/L of aluminum nitrate, 0.1mol/L of magnesium nitrate, 0.05mol/L of trisodium citrate, 0.05mol/L of potassium sodium tartrate and 0.15mol/L of tetrasodium ethylene diamine tetraacetic acid, and is pretreated for 10min at the temperature of 50 ℃; then, 2mol/L sodium hydroxide is used for adjusting the pH value of the precursor solution to 10, and the magnesium alloy is continuously put into the precursor solution to be soaked for 3 hours at the soaking temperature of 55 ℃; finally, washing the magnesium alloy LDHs membrane electrode obtained by soaking with secondary deionized water, and drying in hot air at 30 ℃ for 3 h.
Comparative example 1:
the comparative example used a sheet of AZ91D magnesium alloy without any surface treatment as a sample, and comparative tests were conducted with the examples.
Comparative example 2:
the LDHs film is prepared on the surface of the magnesium alloy by adopting the conventional hydrothermal method.
First, willThe selected exposed surface area is 1cm2The magnesium alloy electrode adopts 200-mesh, 400-mesh, 800-mesh, 1200-mesh and 2000-mesh sandpaper and 5 mu m Al respectively2O3Polishing the polishing powder, and removing oil and cleaning with absolute ethyl alcohol and secondary deionized water; the chemical conversion solution is 0.05mol/L of aluminum nitrate and 0.1mol/L of magnesium nitrate aqueous solution, then 2mol/L of sodium hydroxide is used for adjusting the pH value of the solution to 12, the solution is transferred into a hydrothermal reaction kettle, a magnesium alloy electrode is placed into the hydrothermal reaction kettle, and the solution is reacted for 5 hours at 120 ℃ by a hydrothermal method to prepare the AZ91D magnesium alloy covered with the Mg-Al LDHs film.
And (3) performance testing:
the surface of the magnesium alloy surface LDHs film prepared by the dipping treatment in example 1 was analyzed by scanning electron microscopy, as shown in fig. 1, the magnesium alloy after the dipping conversion treatment had a compact Mg-Al LDHs film layer on the surface and a lamellar morphology peculiar to the LDHs film.
The corrosion current density and the low-frequency impedance of the finished products obtained in the examples and the comparative examples were measured electrochemically in a 3.5 wt.% NaCl solution. Wherein: the electrochemical test system is a three-electrode system, wherein the magnesium alloy sheet is a working electrode; a saturated calomel electrode is used as a reference electrode; the platinum sheet is the counter electrode. The corrosion medium was 3.5 wt.% NaCl solution with a working temperature of 2522 ℃. Firstly, testing an open-circuit potential, and testing an Electrochemical Impedance Spectroscopy (EIS) and a polarization curve after the open-circuit potential is stable; the EIS has a test range of 100-0.1 HZ, an amplitude of 10mV, a scanning speed of a polarization curve of 0.01V/s, and a scanning range of: open circuit potential phase pair Eocpis-0.5V-1V; therefore, the corrosion current density and the impedance value of the low frequency region are obtained, and the lower the corrosion current density is, the larger the impedance value is, the slower the corrosion rate is and the better the corrosion resistance is.
Fig. 2 and 3 are graphs of impedance curves in a low frequency region and corrosion current density curves of the LDHs films on the surface of the magnesium alloy prepared in each example and comparative example, respectively, in which: the abscissa in fig. 2 is frequency (frequency) in Hertz (HZ); the ordinate | Z | represents the impedance and takes the logarithm with the unit of Ω · cm2(ohm cm2) (ii) a Abscissa in FIG. 3Potential (Potential), V volts, SCE, abbreviation for reference electrode used; the ordinate is the derivative of the finger current (Log i) in A/cm2。
TABLE 1 magnitude of self-corrosion potential, self-corrosion current and low-frequency zone impedance values of different samples after 30min immersion in 3.5 wt% NaCl
As can be seen from the attached figure 1, the preparation method provided by the invention can be used for obtaining the sheet LDHs film plate structure. The corrosion resistance data of the LDHs films prepared by the preparation method are shown in table 1, which is obtained by combining the polarization curve with the electrochemical impedance spectroscopy test (fig. 2 and fig. 3). As can be seen from table 1, the self-corrosion current of the LDHs film on the surface of the magnesium alloy prepared by the embodiments of the present invention is reduced by 2 orders of magnitude compared with the blank magnesium alloy of comparative example 1, and the impedance value in the low frequency region is significantly improved, which indicates that the LDHs film obtained by the in-situ crystallization method of the present invention has a better corrosion protection effect on the magnesium alloy, and has an effect equivalent to that of the sample prepared by the hydrothermal method of comparative example 2. In addition, the samples of the embodiments have no obvious corrosion point after 12h salt spray test under the ASTM-B117-09 neutral salt spray test standard, which shows that the LDHs film layer prepared by the invention has better protection and durability performance. Compared with the existing hydrothermal method or electrodeposition method, the method has the advantages of simple operation process, no need of equipment and environment, no concern of high energy consumption such as high temperature and high pressure and the like, and thus has good application and popularization values.
While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiment, but on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims.
The above description is only a few examples of the present invention, and does not limit the scope of the present invention, and it should be appreciated by those skilled in the art that the equivalent alternatives and obvious variations of the present invention are included in the scope of the present invention.
Claims (10)
1. An in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy is characterized in that: the method comprises the following steps:
s1: pretreating a magnesium alloy substrate;
s2: soaking the magnesium alloy substrate treated in the step S1 in a precursor solution for pretreatment; the solute of the precursor solution is aluminum nitrate, magnesium nitrate, trisodium citrate, potassium sodium tartrate and tetrasodium ethylene diamine tetraacetate, and the solvent is water.
S3: adjusting the pH value of the precursor solution in the step S2 to 9-12, and placing the magnesium alloy substrate treated in the step S2 in the precursor solution after the pH value is adjusted to continue dipping treatment;
s4: and (4) washing the surface of the magnesium alloy with the LDHs film obtained after the treatment of the step S3 with deionized water, and drying with hot air.
2. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 1, which is characterized in that: in step S2, the solute in the precursor solution has the following concentration of aluminum nitrate according to the concentration of the solute: 0.1-0.5 mol/L, and the concentration of magnesium nitrate is as follows: 0.05-0.25 mol/L, wherein the concentration of trisodium citrate is as follows: 0.01-0.05 mol/L, wherein the concentration of potassium sodium tartrate is as follows: 0.01-0.05 mol/L, and the concentration of the ethylenediaminetetraacetic acid tetrasodium salt is as follows: 0.04 to 0.2 mol/L.
3. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 1, which is characterized in that: in step S2, the temperature of the pretreatment is 20-50 ℃, and the time of the pretreatment is 10-30 min.
4. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 1, which is characterized in that: in step S1, the pretreatment includes pre-coating and polishing cleaning.
5. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 4, which is characterized in that: in step S1, the early coating step includes: coating magnesium alloy substrate with polytetrafluoroethylene to expose only 1cm2The surface of the magnesium alloy is used for post treatment and corrosion resistance test.
6. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 4, which is characterized in that: in step S1, the polishing and cleaning process includes the following steps: the magnesium alloy substrate is respectively polished by sand paper of 200 meshes, 400 meshes, 800 meshes, 1200 meshes and 2000 meshes, and Al with the particle size of 2.5-5 mu m is adopted2O3Polishing the polished magnesium alloy substrate by using the polishing powder, and finally, removing oil and cleaning by using absolute ethyl alcohol and deionized water, and drying by blowing.
7. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 1, which is characterized in that: in the step S3, a sodium hydroxide solution with the concentration of 1-5 mol/L is adopted to adjust the pH value of the precursor solution in the step S2.
8. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 1, which is characterized in that: in step S3, the temperature of the dipping treatment is 25-65 ℃, and the treatment time is 1-6 h.
9. The in-situ crystallization preparation method of LDHs film on the surface of magnesium alloy as claimed in claim 1, which is characterized in that: in step S4, the hot air drying temperature is 40-80 ℃, and the drying time is 0.5-3 h.
10. The LDHs film on the surface of the magnesium alloy is characterized in that: the LDHs film on the surface of the magnesium alloy is prepared by the in-situ crystallization preparation method of the LDHs film on the surface of the magnesium alloy as defined in any one of claims 1 to 9.
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