CN112267114A - Method for improving compactness and corrosion resistance of hydrotalcite coating on surface of magnesium alloy - Google Patents
Method for improving compactness and corrosion resistance of hydrotalcite coating on surface of magnesium alloy Download PDFInfo
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- CN112267114A CN112267114A CN202010937501.8A CN202010937501A CN112267114A CN 112267114 A CN112267114 A CN 112267114A CN 202010937501 A CN202010937501 A CN 202010937501A CN 112267114 A CN112267114 A CN 112267114A
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- 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
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Abstract
The invention discloses a method for improving compactness and corrosion resistance of a hydrotalcite coating on the surface of a magnesium alloy, which comprises the steps of preprocessing a magnesium alloy sample and preparing a MgAl-ASP-LDH coating on the surface of the magnesium alloy: 0.769g Mg (NO) is taken first when preparing the coating3)2·6H2O、0.375g Al(NO3)3·9H2Dissolving 0.044g of aspartic acid and O in 50ml of deionized water, magnetically stirring uniformly, and adjusting the pH value of the mixed solution to 9-10 by using NaoH; then transferring the magnesium alloy and the treated magnesium alloy into a hydrothermal kettle, carrying out hydrothermal reaction for 3-12 h at the temperature of 110-125 ℃, and standing for 2-3 h at room temperature; and finally, taking out the sample from the hydrothermal kettle, ultrasonically cleaning the sample for 15min by using deionized water, and drying the sample. According to the invention, the MgAl-ASP-LDH film is deposited on the surface of the AZ31 magnesium alloy by using a hydrothermal method, and the MgAl-ASP-LDH coating which grows for 12 hours in a hydrothermal mode has the highest compactness and pore coverage rate, has an anode corrosion potential and an extremely low corrosion current density, and greatly improves the corrosion resistance of the magnesium alloy.
Description
Technical Field
The invention belongs to the technical field of alloy material corrosion prevention, and particularly relates to a method for improving compactness and corrosion resistance of a hydrotalcite coating on the surface of a magnesium alloy.
Background
Magnesium alloy is the lightest metal structure material, has many advantages such as high specific strength, good electromagnetic shielding performance, good castability and easy recovery, and is widely applied to many fields such as electronic communication, automobiles and aerospace. However, magnesium alloys have a low equilibrium potential and are not dense in an oxide film formed on the surface during oxidation. Although the oxide film can provide a certain protection effect, the oxide film has no practical value, and the surface treatment needs to be carried out on the magnesium alloy before the application. Many of the traditional magnesium alloy surface treatment methods have some significant problems. For example, micro-arc oxidation has high power consumption, electroplating chemical plating has strong pollution discharge capacity, and the pollution is serious, which is not favorable for sustainable development. In recent years, many studies (for example, the documents of Feng Peng, et al. ACS Applied Materials & Interfaces,2016,8, 35033-. Moreover, the LDH coating is deposited on the surface of the magnesium alloy, and the method is simple and environment-friendly, and is expected to replace the traditional magnesium alloy surface treatment method. Currently, magnesium alloy LDH coatings which are much researched are mainly MgAl-LDH coatings. In order to improve the corrosion resistance of the MgAl-LDH coating, a corrosion inhibitor can be inserted into the layered structure of the MgAl-LDH. For example, the documents Rong-Chang Zeng, et al, journal of Materials Chemistry A,2014,2,13049-13057 and the Chinese patent of invention 201310368527.5 describe a method for inserting molybdate into MgAl-LDH coatings which has a corrosion inhibiting function on magnesium alloys. The Chinese patent 201611243442.4 describes a method for preparing glutamic acid intercalated hydrotalcite on the surface of medical magnesium alloy. The corrosion inhibitor intercalated LDH coating absorbs chloride ions with erosion capacity in a corrosion medium by utilizing the exchange action between interlaminar corrosion inhibitors such as molybdate and chloride ions, so that the corrosion resistance of the corrosion inhibitor intercalated LDH coating in a NaCl medium is enhanced. However, a great disadvantage of LDH coatings is that there are very many pores between the stereo-linked LDH sheets, and referring to fig. 1(a) and 1(b), the corrosive solution easily penetrates into the coating, which results in the LDH membrane layer losing its protective effect on the substrate. The MgAl-LDH corrosion-resistant coatings prepared by the existing documents are all in a typical three-dimensional sheet structure, and the existence of the porous gaps greatly reduces the corrosion-resistant effect of the MgAl-LDH corrosion-resistant coatings.
Disclosure of Invention
In order to overcome the defects, the invention provides a method for improving the compactness and the corrosion resistance of a hydrotalcite coating on the surface of a magnesium alloy.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a method for improving the compactness and the corrosion resistance of a hydrotalcite coating on the surface of a magnesium alloy comprises the following steps:
step 1, preprocessing a magnesium alloy sample:
grinding a magnesium alloy sample by 400-mesh, 800-mesh, 1500-mesh and 2000-mesh sand paper respectively, then ultrasonically cleaning and drying by using ethanol, then removing a surface oxide layer by using a 0.5% NaoH solution, ultrasonically cleaning by using the ethanol for 10min, and drying for later use;
a) 0.769g of Mg (NO) was taken3)2·6H2O、0.375g Al(NO3)3·9H2Dissolving 0.044g of aspartic acid and O in 50ml of deionized water, magnetically stirring uniformly, and adjusting the pH value of the mixed solution to 9-10 by using NaoH;
b) transferring the mixed solution in the step a) and the magnesium alloy treated in the step 1 into a hydrothermal kettle, carrying out hydrothermal reaction for 3-12 h at the temperature of 110-125 ℃, and standing for 2-3 h at room temperature;
c) and taking out the sample from the hydrothermal kettle, ultrasonically cleaning the sample by using deionized water for 15min, and drying the sample.
As a further improvement of the invention, the magnesium alloy sample in the step 1 is AZ31 magnesium alloy, which has the length of 25mm, the width of 20mm and the height of 2 mm.
As a further improvement of the invention, the hydrothermal reaction time of step b) of step 2 is 12 h.
The invention has the beneficial effects that: according to the invention, a MgAl-ASP-LDH film is deposited on the surface of the AZ31 magnesium alloy by using a hydrothermal method, and the compactness and the porosity of the MgAl-ASP-LDH coating are stably improved along with the increase of the hydrothermal growth time. The MgAl-ASP-LDH coating which grows for 12 hours in a hydrothermal mode has the highest compactness and porosity, has a positive corrosion potential and an extremely low corrosion current density, and greatly improves the corrosion resistance of the magnesium alloy.
Drawings
FIGS. 1(a) and 1(b) are micrographs of conventional MgAl-LDH;
FIGS. 2(a) and 2(b) are the morphology of MgAl-ASP-LDHs coatings of example 1 of the present invention;
FIGS. 2(c) and 2(d) are the morphology of MgAl-ASP-LDHs coatings of example 2 of the present invention;
FIGS. 2(e) and 2(f) are the morphology of MgAl-ASP-LDHs coatings of example 3 of the present invention;
FIGS. 2(g) and 2(h) are the morphology of MgAl-ASP-LDHs coatings of example 4 of the present invention;
FIG. 3 is a polarization curve of examples 1, 2, 3, 4 and a magnesium alloy substrate according to the present invention;
FIGS. 4(a), 4(b) are XRD and FT-IR of MgAl-ASP-LDHs powder scraped from a magnesium part in example 4 of the present invention.
Detailed Description
Several embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
Mixing AZ31 magnesium alloy (2 × 20 × 25 mm)3) The method comprises the steps of respectively polishing with 400-mesh, 800-mesh, 1500-mesh and 2000-mesh sandpaper, ultrasonically cleaning with ethanol, drying, removing a surface oxide layer with 0.5% of NaoH solution by mass, ultrasonically cleaning with ethanol for 10min, and drying for later use. 0.769g Mg (NO) is prepared3)2·6H2O、0.375g Al(NO3)3·9H2Dissolving 0.044g of aspartic acid and O in 50ml of deionized water, magnetically stirring uniformly, and adjusting the pH of the solution to 9-10 by using NaoH (2M). And transferring the prepared mixed solution and the treated magnesium alloy into a hydrothermal kettle, carrying out hydrothermal reaction for 3 hours at the temperature of 110-125 ℃, and immediately standing for 2-3 hours at room temperature. And finally, taking out the sample from the hydrothermal kettle, ultrasonically cleaning the sample for 15min by using deionized water, and drying the sample.
As shown in fig. 2(a) and 2(b), fig. 2(a) and 2(b) are scanning electron micrographs at 5kx and 50kx magnification of the present example, and the hydrotalcite thin film prepared in the present example has not grown sufficiently to be a nanosheet.
As shown in fig. 3, this example has a more positive corrosion potential and a lower corrosion current density than the magnesium alloy substrate, and the corrosion resistance is superior to the magnesium alloy substrate.
Example 2
Mixing AZ31 magnesium alloy (2 × 20 × 25 mm)3) The method comprises the steps of respectively polishing with 400-mesh, 800-mesh, 1500-mesh and 2000-mesh sandpaper, ultrasonically cleaning with ethanol, drying, removing surface oxidation with 0.5% of NaoH solution by mass, ultrasonically cleaning with ethanol for 10min, and drying for later use. 0.769g Mg (NO) is prepared3)2·6H2O、0.375g Al(NO3)3·9H2Dissolving 0.044g of aspartic acid and O in 50ml of deionized water, magnetically stirring uniformly, and adjusting the pH of the solution to 9-10 by using NaoH (2M). And transferring the prepared mixed solution and the treated magnesium alloy into a hydrothermal kettle, carrying out hydrothermal reaction at 110-125 ℃ for 6 hours, and immediately standing at room temperature for 2-3 hours. And finally, taking out the sample from the hydrothermal kettle, ultrasonically cleaning the sample for 15min by using deionized water, and drying the sample.
As shown in fig. 2(c) and 2(d), fig. 2(c) and 2(d) are scanning electron micrographs of the coating of this example at 5kx and 50kx magnification, and the coating surface prepared in this example has grown perfect and dense three-dimensional sheets, and it can be clearly seen that there are many pores between the three-dimensional cross-linked sheets.
As shown in fig. 3, this example has a lower corrosion current density than example 1, and the corrosion resistance is superior to example 1 and the magnesium alloy substrate.
Example 3
AZ31 magnesium alloy (2X 2)0 × 25mm3), respectively grinding with 400, 800, 1500 and 2000-mesh sand paper, ultrasonically cleaning and drying with ethanol, removing surface oxidation with 0.5% of NaoH solution by mass percentage, ultrasonically cleaning with ethanol for 10min, and drying for later use. 0.769g Mg (NO) is prepared3)2·6H2O、0.375g Al(NO3)3·9H2Dissolving 0.044g of aspartic acid and O in 50ml of deionized water, magnetically stirring uniformly, and adjusting the pH of the solution to 9-10 by using NaoH (2M). And transferring the prepared mixed solution and the treated magnesium alloy into a hydrothermal kettle, carrying out hydrothermal reaction at 110-125 ℃ for 9 hours, and immediately standing at room temperature for 2-3 hours. And finally, taking out the sample from the hydrothermal kettle, ultrasonically cleaning the sample for 15min by using deionized water, and drying the sample.
As shown in FIGS. 2(e) and 2(f), FIGS. 2(e) and 2(f) are SEM images of the present example at magnifications of 5kx and 50kx, and the coating layer prepared in this example is thick but uneven in film formation, and the surface of the coating layer begins to deposit flat LDH sheets on the basis of three-dimensional sheet LDH
As shown in fig. 3, this example has a lower corrosion current density than example 2, and is superior in corrosion resistance to examples 1 and 2 and the magnesium alloy substrate.
Example 4
Grinding AZ31 magnesium alloy (2 × 20 × 25mm3) with 400, 800, 1500 and 2000-mesh sandpaper respectively, ultrasonically cleaning and drying with ethanol, removing surface oxidation with 0.5% by mass of NaoH solution, ultrasonically cleaning with ethanol for 10min, and drying for later use. 0.769g Mg (NO) is prepared3)2·6H2O、0.375g Al(NO3)3·9H2Dissolving 0.044g of aspartic acid and O in 50ml of deionized water, magnetically stirring uniformly, and adjusting the pH of the solution to 9-10 by using NaoH (2M). And transferring the prepared mixed solution and the treated magnesium alloy into a hydrothermal kettle, carrying out hydrothermal reaction at 110-125 ℃ for 12 hours, and immediately standing at room temperature for 2-3 hours. And finally, taking out the sample from the hydrothermal kettle, ultrasonically cleaning the sample for 15min by using deionized water, and drying the sample.
As shown in fig. 2(g) and 2(h), fig. 2(g) and 2(h) are scanning electron micrographs of the present example at a magnification of 5kx and 50kx, the porosity coverage and the compactness of the coating prepared by the present example are greatly improved, and the LDH on the surface of the coating is changed into sparse rose type stereo sheets.
As shown in fig. 3, this example has a positive corrosion potential and a very low corrosion current density, and is superior in corrosion resistance to examples 1, 2, and 3 and the magnesium alloy substrate.
As shown in FIG. 4, FIGS. 4(a) and 4(b) are XRD and FT-IR, respectively, of MgAl-ASP-LDHs powder scraped from a magnesium part in an example of the present invention. In FIG. 3, MgAl-ASP-LDH shows characteristic diffraction peak position (003) to (006) peak (Standard ratio vs. card 22-700) of LDH, and 1635 cm-1, 1416cm-1 corresponding to-COOH vibration of SAP molecule can be seen in FIG. 4 (b). The XRD diffractogram and FT-IR chart indicated that MgAl-LDH was successfully prepared and aspartate ions were successfully intercalated into the MgAl-LDH laminae.
Therefore, the MgAl-ASP-LDH film is deposited on the surface of the AZ31 magnesium alloy by using a hydrothermal method, and the compactness and the porosity of the MgAl-ASP-LDH coating are stably improved along with the increase of the hydrothermal growth time. The MgAl-ASP-LDH coating which grows for 12 hours in a hydrothermal mode has the highest compactness and porosity, has a positive corrosion potential and an extremely low corrosion current density, and greatly improves the corrosion resistance of the magnesium alloy.
The MgAl-ASP-LDH coating grown for 12 hours in a hydrothermal mode has the following advantages:
the compactness of the coating is improved by high porosity, and the corrosion protection time of the coating is prolonged;
the existing three-dimensional sheet LDH increases the specific surface area contacted with the corrosive solution, improves the capture efficiency of corrosive ions (Cl-) and enhances the corrosion resistance;
aspartic acid, an environment-friendly corrosion inhibitor, is inserted into the MgAl-LDH laminate, and after the LDH captures corrosive ions in the solution through ion exchange and releases aspartic acid, the aspartic acid can inhibit the corrosion of the corrosive solution to the coating, so that the corrosion protection time of the coating is further prolonged.
In the previous description, numerous specific details were set forth in order to provide a thorough understanding of the present invention. The foregoing description is only a preferred embodiment of the invention, which can be embodied in many different forms than described herein, and therefore the invention is not limited to the specific embodiments disclosed above. And that those skilled in the art may, using the methods and techniques disclosed above, make numerous possible variations and modifications to the disclosed embodiments, or modify equivalents thereof, without departing from the scope of the claimed embodiments. Any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the scope of the technical solution of the present invention.
Claims (3)
1. A method for improving the compactness and the corrosion resistance of a hydrotalcite coating on the surface of a magnesium alloy is characterized by comprising the following steps of:
step 1, preprocessing a magnesium alloy sample:
grinding a magnesium alloy sample by 400-mesh, 800-mesh, 1500-mesh and 2000-mesh sand paper respectively, then ultrasonically cleaning and drying by using ethanol, then removing a surface oxide layer by using a 0.5% NaoH solution, ultrasonically cleaning by using the ethanol for 10min, and drying for later use;
step 2, preparing an MgAl-ASP-LDH coating on the surface of the magnesium alloy:
a) 0.769g of Mg (NO) was taken3)2·6H2O、0.375g Al(NO3)3·9H2Dissolving 0.044g of aspartic acid and O in 50ml of deionized water, magnetically stirring uniformly, and adjusting the pH value of the mixed solution to 9-10 by using NaoH;
b) transferring the mixed solution in the step a) and the magnesium alloy treated in the step 1 into a hydrothermal kettle, carrying out hydrothermal reaction for 3-12 h at the temperature of 110-125 ℃, and standing for 2-3 h at room temperature;
c) and taking out the sample from the hydrothermal kettle, ultrasonically cleaning the sample by using deionized water for 15min, and drying the sample.
2. The method for improving the compactness and the corrosion resistance of the hydrotalcite coating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: the magnesium alloy sample in the step 1 is AZ31 magnesium alloy, which has the length of 25mm, the width of 20mm and the height of 2 mm.
3. The method for improving the compactness and the corrosion resistance of the hydrotalcite coating on the surface of the magnesium alloy according to claim 1, wherein the method comprises the following steps: the hydrothermal reaction time of the step b) in the step 2 is 12 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114774863A (en) * | 2022-04-13 | 2022-07-22 | 佛山科学技术学院 | Li-Al LDH membrane on surface of magnesium alloy and rapid preparation method thereof |
| CN115999875A (en) * | 2022-10-31 | 2023-04-25 | 重庆大学 | Magnesium alloy composite coating with wear-resistant superhydrophobic and self-healing anti-corrosion functions and manufacturing method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106693044A (en) * | 2016-12-29 | 2017-05-24 | 山东科技大学 | Method for preparing glutamate intercalation hydrotalcite medicinal magnesium alloy coating |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106693044A (en) * | 2016-12-29 | 2017-05-24 | 山东科技大学 | Method for preparing glutamate intercalation hydrotalcite medicinal magnesium alloy coating |
Non-Patent Citations (2)
| Title |
|---|
| JIALING CHEN ，ET AL: "Corrosion resistance of a self-healing rose-like MgAl-LDH coating intercalated with aspartic acid on AZ31 Mg alloy", 《PROGRESS IN ORGANIC COATINGS》 * |
| 谢治辉: "镁合金表面原位生长高耐蚀水碳铝镁石涂层", 《兵器材料科学与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114774863A (en) * | 2022-04-13 | 2022-07-22 | 佛山科学技术学院 | Li-Al LDH membrane on surface of magnesium alloy and rapid preparation method thereof |
| CN114774863B (en) * | 2022-04-13 | 2023-11-14 | 佛山科学技术学院 | Li-Al LDH film on magnesium alloy surface and rapid preparation method thereof |
| CN115999875A (en) * | 2022-10-31 | 2023-04-25 | 重庆大学 | Magnesium alloy composite coating with wear-resistant superhydrophobic and self-healing anti-corrosion functions and manufacturing method thereof |
| CN115999875B (en) * | 2022-10-31 | 2023-07-18 | 重庆大学 | Magnesium alloy composite coating with wear-resistant superhydrophobic and self-healing anti-corrosion functions and manufacturing method thereof |
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