CN114561635B - LDHs film on magnesium alloy surface and in-situ crystallization preparation method thereof - Google Patents

LDHs film on magnesium alloy surface and in-situ crystallization preparation method thereof Download PDF

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CN114561635B
CN114561635B CN202210065182.5A CN202210065182A CN114561635B CN 114561635 B CN114561635 B CN 114561635B CN 202210065182 A CN202210065182 A CN 202210065182A CN 114561635 B CN114561635 B CN 114561635B
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magnesium alloy
ldhs film
precursor solution
ldhs
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CN114561635A (en
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陈东初
王乘风
杜小青
聂宝华
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Foshan University
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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
    • 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
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

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: pre-treating a magnesium alloy substrate; s2: soaking the magnesium alloy substrate treated in the step S1 in a precursor solution for pretreatment; the precursor solution solutes are aluminum nitrate, magnesium nitrate, trisodium citrate, potassium sodium tartrate and tetrasodium ethylenediamine tetraacetate, and the solvent is water. S3: regulating the pH value of the precursor solution in the step S2 to 9-12, and putting the magnesium alloy substrate treated in the step S2 into the precursor solution with the pH value regulated for continuous dipping treatment; s4: and (3) flushing the surface of the magnesium alloy with the LDHs film obtained after the treatment in the step (S3) with deionized water, and then drying with hot air. The preparation method has the advantages of simple process, low energy consumption, capability of being used for large-area production, flaky laminate structure of the prepared LDHs film, high film compactness and better corrosion resistance.

Description

LDHs film on magnesium alloy surface and in-situ crystallization preparation method thereof
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, low density (about 1/3 of that of titanium alloy) and the like of the magnesium alloy lead the magnesium alloy to be used in high-tech products such as: aerospace product parts, automotive industry, computer industry, sporting goods in daily life, mobile phones, home appliances, etc. are widely used. However, the relatively high chemical activity of magnesium alloys results in poor corrosion resistance, and thus, some applications thereof are limited.
In order to improve the corrosion resistance of magnesium alloys, various magnesium alloy corrosion resistant coatings such as chemical conversion films, micro-arc oxidation films, polymer coatings, electrochemical deposition plating layers, plasma electrolytic oxidation coatings, super-hydrophobic coatings, laser surface treatment coatings 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 metal substrate has better binding force, and meanwhile, the technology is simple in process, low in energy consumption and free from the limitation of the size and shape of a workpiece, so that the metal substrate is widely applied to the field of metal corrosion prevention. In the current chemical conversion process of the magnesium alloy surface, the chemical conversion film generated by adopting chromate has relatively excellent corrosion resistance and good binding force with a matrix. However, the chromates contain Cr 6+ The ion has carcinogenicity and teratogenicity to human body. There is therefore a need to find new environmentally friendly conversion coatings that can replace chromate conversion coatings.
Layered double hydroxides (layered double hydroxides, LDH or LDHs) LDHs are anionic intercalation materials of the general formula [ M2+1-x M3+x (OH) 2 ] x+ (A n- ) x/n ·m H 2 O, where M 2+ And M 3+ Representing cations occupying octahedral pores in the lamellar layer, A n- Represents an interlayer charge compensation anion, n is the charge of an intercalation anion, M is the number of water molecules, x represents M 3+ /(M 2+ +M 3+ ) Molar ratio of (3). The existing research shows that: the LDHs film layer has simple preparation process and good physical barrier effect, and the unique interlayer anion exchange capacity enables the LDHs film layer to capture aggressive anions, so that the corrosion resistance of the magnesium alloy is greatly improved, and therefore, the LDHs film layer has been widely focused in the field of corrosion protection. The existing method for preparing the LDHs film is mostly a hydrothermal method, but the hydrothermal method needs high temperature and high pressure, which results in the establishment of the environmentHigh preparation requirement and high energy consumption.
Disclosure of Invention
The invention aims at solving 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 magnesium alloy surface in large-area production.
In order to achieve the above object, the present invention provides an in-situ crystallization preparation method of an LDHs film on a magnesium alloy surface, comprising the following steps:
s1: pre-treating a magnesium alloy substrate;
s2: soaking the magnesium alloy substrate treated in the step S1 in a precursor solution for pretreatment; the precursor solution solutes are aluminum nitrate, magnesium nitrate, trisodium citrate, potassium sodium tartrate and tetrasodium ethylenediamine tetraacetate, and the solvent is water.
S3: regulating the pH value of the precursor solution in the step S2 to 9-12, and putting the magnesium alloy substrate treated in the step S2 into the precursor solution with the pH value regulated for continuous dipping treatment;
s4: and (3) flushing the surface of the magnesium alloy with the LDHs film obtained after the treatment in the step (S3) with deionized water, and then drying with hot air.
Compared with the prior art, the LDHs film can be obtained on the surface of the magnesium alloy by adopting an in-situ crystallization method under the condition of normal temperature and normal pressure through simple impregnation, and the LDHs film obtained by adopting the preparation method has the same layered structure and composition components as those of the LDHs film obtained by adopting a hydrothermal method and an electrodeposition method, and has higher corrosion resistance. The preparation method has the advantages of simple process, low energy consumption, capability of being used for large-area production, lamellar laminate structure of the LDHs film obtained by the preparation method, high film compactness and better corrosion resistance.
Preferably, in step S2, the concentration of the solute in the precursor solution is calculated according to the mass concentration of the substance, and the concentration of aluminum nitrate is: 0.1 to 0.5mol/L, and the concentration of magnesium nitrate is as follows: 0.05 to 0.25mol/L, and the concentration of the trisodium citrate is as follows: 0.01-0.05 mol/L, the concentration of potassium sodium tartrate is as follows: the concentration of the ethylene diamine tetraacetic acid tetrasodium is 0.01-0.05 mol/L: 0.04 to 0.2mol/L.
Preferably, in step S2, the pretreatment temperature is 20-50 ℃ and the pretreatment time is 10-30 min.
Preferably, in step S1, the pretreatment includes a pre-coating and a sanding polishing cleaning treatment.
Preferably, in step S1, the pre-cladding step is as follows: the magnesium alloy substrate is coated by polytetrafluoroethylene, and only the surface of the magnesium alloy with the thickness of 1cm < 2 > is exposed for post-treatment and corrosion resistance test.
Preferably, in step S1, the lapping and polishing cleaning process includes the steps of: the magnesium alloy substrate is respectively polished by 200 meshes, 400 meshes, 800 meshes, 1200 meshes and 2000 meshes of sand paper, and Al with the grain diameter of 2.5-5 mu m is adopted 2 O 3 Polishing the ground magnesium alloy substrate by using polishing powder, and finally degreasing, cleaning and drying by using absolute ethyl alcohol and deionized water.
Preferably, in step S3, the pH of the precursor solution in step S2 is adjusted with a sodium hydroxide solution having a concentration of 1 to 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 the step S4, the hot air drying temperature 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 magnesium alloy surface.
The invention provides an in-situ crystallization preparation method of an LDHs film on the surface of a magnesium alloy, 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; the prepared LDHs film has a lamellar laminate structure, and the film layer has high compactness and better corrosion resistance.
Drawings
FIG. 1 is an SEM image of an LDHs film on the surface of a magnesium alloy obtained in example 1
FIG. 2 is a graph showing the impedance of the low frequency region of the finished products obtained in each of the examples and comparative examples when immersed in a 3.5wt.% NaCl solution
FIG. 3 is a graph showing the polarization curves of the finished products obtained in each of the examples and comparative examples when immersed in a 3.5wt.% NaCl solution
Detailed Description
The invention will be further illustrated with reference to specific examples. It should be understood that the practice of the invention is not limited to the following examples, but is intended to be within the scope of the invention in any form or modification thereof.
Example 1:
the LDHs film is prepared 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 is 1cm 2 The magnesium alloy electrode adopts 200 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper and 2.5 μm Al 2 O 3 Polishing the polishing powder, degreasing, cleaning and blow-drying by using absolute ethyl alcohol and secondary deionized water; then the treated magnesium alloy electrode is placed in a precursor aqueous solution composed of 0.1mol/L aluminum nitrate, 0.5mol/L magnesium nitrate, 0.01mol/L trisodium citrate (metal ion complexing agent), 0.01mol/L potassium sodium tartrate and 0.05mol/L tetra sodium ethylenediamine tetraacetate, and is pretreated for 10min at 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 ℃; and finally, washing the dipped magnesium alloy LDHs membrane electrode with secondary deionized water, and drying in hot air at 25 ℃ for 3 hours. The surface morphology of the LDHs film on the surface of the magnesium alloy obtained in this example is shown in fig. 1.
Example 2:
the LDHs film is prepared 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 is 1cm 2 The magnesium alloy electrode adopts 200 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper and 2.5 μm Al 2 O 3 Polishing with anhydrous BDeoiling, cleaning and blow-drying the alcohol and the secondary deionized water; then the treated magnesium alloy electrode is put into a precursor aqueous solution composed of 0.2mol/L aluminum nitrate, 0.25mol/L magnesium nitrate, 0.01mol/L trisodium citrate, 0.01mol/L potassium sodium tartrate and 0.2mol/L tetra sodium ethylenediamine tetraacetate, and is pretreated for 30min at 50 ℃; then adjusting the pH value of the precursor solution to 12 by using 2mol/L sodium hydroxide, and continuously soaking the magnesium alloy in the precursor solution for 6 hours at the soaking temperature of 35 ℃; and finally, washing the dipped magnesium alloy LDHs membrane electrode with secondary deionized water, and drying in hot air at 50 ℃ for 3 hours.
Example 3:
the LDHs film is prepared 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 is 1cm 2 The magnesium alloy electrode adopts 200 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper and 2.5 μm Al 2 O 3 Polishing the polishing powder, degreasing, cleaning and blow-drying by using absolute ethyl alcohol and secondary deionized water; then the treated magnesium alloy electrode is put into a precursor aqueous solution composed 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 tetra sodium ethylenediamine tetraacetate, and is pretreated for 20min at 35 ℃; then adjusting the pH value of the precursor solution to 11 by using 2mol/L sodium hydroxide, and continuously soaking the magnesium alloy in the precursor solution for 1h at the soaking temperature of 40 ℃; and finally, washing the dipped magnesium alloy LDHs membrane electrode by using secondary deionized water, and drying in hot air at 50 ℃ for 0.5h.
Example 4:
the LDHs film is prepared 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 is 1cm 2 The magnesium alloy electrode adopts 200 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper and 2.5 μm Al 2 O 3 Polishing the polishing powder, degreasing, cleaning and blow-drying by using absolute ethyl alcohol and secondary deionized water; then the treated magnesium alloy electrode is placed at a position from 02mol/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 tetrasodium ethylenediamine tetraacetate, and pretreating for 30min at 50 ℃; then adjusting the pH value of the precursor solution to 12 by using 2mol/L sodium hydroxide, and continuously soaking the magnesium alloy in the precursor solution for 6 hours at the soaking temperature of 35 ℃; and finally, washing the dipped magnesium alloy LDHs membrane electrode with secondary deionized water, and drying in hot air at 50 ℃ for 3 hours.
Example 5:
the LDHs film is prepared 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 is 1cm 2 The magnesium alloy electrode adopts 200 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper and 5 μm Al 2 O 3 Polishing the polishing powder, degreasing, cleaning and blow-drying by using absolute ethyl alcohol and secondary deionized water; then the treated magnesium alloy electrode is put into a precursor aqueous solution composed of 0.05mol/L aluminum nitrate, 0.1mol/L magnesium nitrate, 0.05mol/L trisodium citrate, 0.05mol/L potassium sodium tartrate and 0.15mol/L tetra sodium ethylenediamine tetraacetate, and is pretreated for 10min at 50 ℃; then adjusting the pH value of the precursor solution to 10 by using 2mol/L sodium hydroxide, and continuously soaking the magnesium alloy in the precursor solution for 3 hours at a soaking temperature of 55 ℃; and finally, flushing the dipped magnesium alloy LDHs membrane electrode with secondary deionized water, and drying in hot air at 30 ℃ for 3 hours.
Comparative example 1:
the comparative example was conducted by selecting an AZ91D magnesium alloy sheet without any surface treatment as a sample, and comparing the sample with the example.
Comparative example 2:
the present comparative example adopts the existing hydrothermal method to prepare LDHs film on the surface of magnesium alloy.
First, the selected exposed surface area is 1cm 2 The magnesium alloy electrode adopts 200 mesh, 400 mesh, 800 mesh, 1200 mesh, 2000 mesh sand paper and 5 μm Al 2 O 3 Polishing with anhydrous ethanol and secondaryDeoiling and cleaning with deionized water; the chemical conversion solution is 0.05mol/L aluminum nitrate, 0.1mol/L magnesium nitrate aqueous solution, then the pH value of the solution is regulated to 12 by 2mol/L sodium hydroxide, the solution is transferred into a hydrothermal reaction kettle, a magnesium alloy electrode is placed, and the AZ91D magnesium alloy covered with the Mg-Al LDHs film is prepared by hydrothermal reaction for 5 hours at 120 ℃.
Performance test:
the surface morphology analysis is carried out on the LDHs film on the surface of the magnesium alloy prepared by the dipping treatment in the embodiment 1 by adopting a scanning electron microscope, as shown in fig. 1, the surface of the magnesium alloy subjected to the dipping conversion treatment presents a compact Mg-Al LDHs film layer, and presents the lamellar morphology peculiar to the LDHs film.
The finished products prepared in each example and comparative example were subjected to electrochemical testing in a 3.5wt.% NaCl solution to obtain corrosion current density and low frequency zone resistance values thereof. Wherein: the electrochemical test system is a three-electrode system, wherein a magnesium alloy sheet is a working electrode; a saturated calomel electrode is used as a reference electrode; the platinum sheet is a counter electrode. The corrosive medium is a 3.5wt.% NaCl solution and the operating temperature is 2522 ℃. Firstly, testing an open circuit potential, and testing an Electrochemical Impedance Spectrum (EIS) and a polarization curve after the open circuit potential is stabilized; the test range of the EIS is 100 kHZ-0.1 HZ, the amplitude is 10mV, the scanning speed of the polarization curve is 0.01V/s, and the scanning range is: open circuit potential relative E ocp is-0.5V to 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 low frequency region impedance curves and corrosion current density curves of LDHs films on magnesium alloy surfaces prepared in examples and comparative examples, respectively, in which: the abscissa in fig. 2 is frequency (frequency) in Hertz (HZ); the ordinate |Z| represents impedance and takes the logarithm in Ω cm 2 (ohm cm 2 ) The method comprises the steps of carrying out a first treatment on the surface of the In fig. 3, the abscissa represents the Potential (V) V and SCE is an abbreviation for the reference electrode used; the ordinate indicates the derivative of the current (Log i) in A/cm 2 。
TABLE 1 self-etching potential, self-etching current and low frequency region impedance values of different samples after immersion in 3.5wt% NaCl for 30min
As can be seen from the figure 1, the preparation method provided by the invention can be used for obtaining a flaky LDHs film laminate structure. The corrosion resistance data of LDHs films obtained from this preparation method are shown in table 1, in combination with polarization curves and electrochemical impedance spectroscopy tests (fig. 2 and 3). As can be seen from Table 1, compared with the blank magnesium alloy of comparative example 1, the LDHs film on the surface of the magnesium alloy prepared by the embodiments of the invention has the advantages that the self-corrosion current is reduced by 2 orders of magnitude, and the impedance value in the low frequency region is also obviously improved, so that the LDHs film obtained by the in-situ crystallization method of the invention has better corrosion protection effect on the magnesium alloy, and the effect is equivalent to that of the sample prepared by the hydrothermal method of comparative example 2. In addition, the samples of each embodiment have no obvious corrosion points after 12h salt spray test under ASTM-B117-09 neutral salt spray test standard, which shows that the LDHs film layer prepared by the invention has better protection durability. Compared with the existing hydrothermal method or electrodeposition method, the method has the advantages of simple operation process, no high-energy consumption problems such as high temperature, high pressure and the like, and the required equipment and environment are not involved, so that the method has good application and popularization values.
The invention is not limited to the use of the description and embodiments listed, which can be applied to various fields suitable for the invention, and further modifications and variations can be easily realized by those skilled in the art without departing from the spirit and the essence of the invention, but these corresponding modifications and variations shall fall within the scope of protection claimed by the invention.
The above description is only a few examples of the present invention and is not intended to limit the embodiments and the protection scope of the present invention, and it should be appreciated by those skilled in the art that equivalent substitutions and obvious changes made by the content of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. An in-situ crystallization preparation method of an LDHs film on the surface of a magnesium alloy is characterized by comprising the following steps of: the method comprises the following steps:
s1: pre-treating a magnesium alloy substrate;
s2: soaking the magnesium alloy substrate treated in the step S1 in a precursor solution for pretreatment; the precursor solution solutes are aluminum nitrate, magnesium nitrate, trisodium citrate, potassium sodium tartrate and tetrasodium ethylenediamine tetraacetate, and the solvent is water; the pretreatment temperature is 20-50 ℃ and the pretreatment time is 10-30 min;
s3: regulating the pH value of the precursor solution in the step S2 to 9-12, and putting the magnesium alloy substrate treated in the step S2 into the precursor solution with the pH value regulated for continuous dipping treatment, wherein the dipping treatment temperature is 25-65 ℃ and the treatment time is 1-6 h;
s4: and (3) flushing the surface of the magnesium alloy with the LDHs film obtained after the treatment in the step (S3) with deionized water, and then drying with hot air.
2. The method for preparing the LDHs film on the surface of the magnesium alloy in situ crystallization according to claim 1, which is characterized in that: in step S2, the concentration of the solute in the precursor solution is calculated according to the mass concentration of the substance, and the concentration of aluminum nitrate is as follows: 0.1 to 0.5mol/L, and the concentration of magnesium nitrate is as follows: 0.05 to 0.25mol/L, and the concentration of the trisodium citrate is as follows: 0.01-0.05 mol/L, the concentration of potassium sodium tartrate is as follows: the concentration of the ethylene diamine tetraacetic acid tetrasodium is 0.01-0.05 mol/L: 0.04 to 0.2mol/L.
3. The method for preparing the LDHs film on the surface of the magnesium alloy in situ crystallization according to claim 1, which is characterized in that: in step S1, the pretreatment includes a pre-coating and polishing and cleaning treatment.
4. The method for preparing the LDHs film on the surface of the magnesium alloy according to claim 3, wherein the method comprises the following steps: in step S1, the pre-cladding step is as follows: coating the magnesium alloy substrate with polytetrafluoroethylene to expose only 1cm 2 Magnesium alloy meter of (2)The faces were used for post-treatment and corrosion resistance testing.
5. The method for preparing the LDHs film on the surface of the magnesium alloy according to claim 3, wherein the method comprises the following steps: in step S1, the polishing and cleaning process includes the following steps: the magnesium alloy substrate is respectively polished by 200 meshes, 400 meshes, 800 meshes, 1200 meshes and 2000 meshes of sand paper, and Al with the grain diameter of 2.5-5 mu m is adopted 2 O 3 Polishing the ground magnesium alloy substrate by using polishing powder, and finally degreasing, cleaning and drying by using absolute ethyl alcohol and deionized water.
6. The method for preparing the LDHs film on the surface of the magnesium alloy in situ crystallization according to claim 1, which is characterized in that: in the step S3, the pH value of the precursor solution in the step S2 is regulated by adopting a sodium hydroxide solution with the concentration of 1-5 mol/L.
7. The method for preparing the LDHs film on the surface of the magnesium alloy in situ crystallization according to claim 1, which is characterized in that: in the step S4, the hot air drying temperature is 40-80 ℃ and the drying time is 0.5-3 h.
8. The LDHs film on the surface of the magnesium alloy is characterized in that: the method for preparing the LDHs film on the surface of the magnesium alloy by in-situ crystallization according to any one of claims 1 to 7.
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Xinfang Zhang et al.."Active Corrosion Protection of Mg–Al Layered Double Hydroxide for Magnesium Alloys: A Short Review".《COATINGS》.2021,1-18. *
水滑石作为缓蚀剂的优点及其制备与表征;惠宝华;;新疆有色金属(05);66-70 *

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