CN109652754B - Preparation method of magnesium alloy surface anticorrosive coating - Google Patents
Preparation method of magnesium alloy surface anticorrosive coating Download PDFInfo
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- CN109652754B CN109652754B CN201910110707.0A CN201910110707A CN109652754B CN 109652754 B CN109652754 B CN 109652754B CN 201910110707 A CN201910110707 A CN 201910110707A CN 109652754 B CN109652754 B CN 109652754B
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/129—Flame spraying
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
Abstract
The invention belongs to the technical field of magnesium alloy corrosion prevention. The invention provides a preparation method of a magnesium alloy surface anticorrosive coating, which comprises the following steps: (1) pretreating a magnesium alloy matrix; (2) will be provided withHeating the magnesium alloy matrix pretreated in the step (1) to 60-100 ℃, then maintaining the temperature of the magnesium alloy matrix at 60-100 ℃, taking the iron-based amorphous alloy particles as a material to be sprayed, performing supersonic flame spraying on the surface of the magnesium alloy matrix, and obtaining the iron-based amorphous alloy anticorrosive coating on the surface of the magnesium alloy matrix. The preparation method provided by the invention can not deform the magnesium alloy matrix, and the surface hardness reaches 580HV0.2The self-corrosion potential of the iron-based amorphous alloy anticorrosive coating is higher than that of the AZ91 magnesium alloy, and the self-corrosion current density is lower than that of the AZ91 magnesium alloy.
Description
Technical Field
The invention relates to the technical field of magnesium alloy corrosion prevention, in particular to a preparation method of a magnesium alloy surface anticorrosive coating.
Background
In the metal structure material, the magnesium alloy is one of the alloys with lighter weight, has lower density, good mechanical property and higher specific strength and specific rigidity. The magnesium alloy also has the advantages of good dimensional stability, excellent heat and electricity conductivity and the like, and the processing and forming difficulty is low when the magnesium alloy is cast into a structural member. Therefore, the method is widely applied to various aspects in the industrial field, and particularly has great attention in the fields of aerospace, electronics and the like. However, the magnesium alloy has very poor corrosion resistance and wear resistance, cannot meet the use requirements of severe environments, and limits the application of the magnesium alloy.
At present, the surface protection method of the magnesium alloy mainly prepares a pure aluminum coating on the surface of the magnesium alloy by an electric arc spraying method, but the magnesium alloy component is deformed due to overhigh energy of the electric arc spraying, and the aluminum coating has low hardness and lower corrosion resistance.
Disclosure of Invention
The invention aims to provide a preparation method of a magnesium alloy surface anticorrosive coating, which can not deform a magnesium alloy substrate, and has high surface anticorrosive coating hardness and excellent corrosion resistance.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a magnesium alloy surface anticorrosive coating, which comprises the following steps:
(1) pretreating a magnesium alloy matrix;
(2) heating the magnesium alloy matrix pretreated in the step (1) to 60-100 ℃, maintaining the temperature of the magnesium alloy matrix at 60-100 ℃, and performing supersonic flame spraying on the surface of the magnesium alloy matrix by taking the iron-based amorphous alloy particles as a material to be sprayed to obtain the iron-based amorphous alloy anticorrosive coating on the surface of the magnesium alloy matrix.
Preferably, the pretreatment comprises cleaning, sand blasting and grinding which are carried out in sequence.
Preferably, the sand blasting treatment is dry sand blasting treatment, the abrasive used in the sand blasting treatment is 20# white corundum sand, the pressure of the sand blasting treatment is 0.65MPa, the speed of the sand blasting treatment is 0.5cm/s, and the time of the sand blasting treatment is 5 min.
Preferably, the particle size of the iron-based amorphous alloy particles is 250-300 meshes.
Preferably, the speed of the supersonic flame spraying is 15-25 m/min, and the flow of the oxygen for the supersonic flame spraying is 20-50 m3And h, the flow rate of the fuel oil for supersonic flame spraying is 14-25L/h, and the spray distance of the supersonic flame spraying is 260-380 mm.
Preferably, the fuel oil is kerosene.
Preferably, the powder feeding amount of the supersonic flame spraying is 20-50 g/min.
Preferably, in the supersonic flame spraying process, the temperature of the magnesium alloy substrate is reduced by adopting an air cooling mode.
Preferably, the thickness of the iron-based amorphous alloy anticorrosive coating is 300-600 mu m.
The invention provides a preparation method of a magnesium alloy surface anticorrosive coating, which comprises the following steps: (1) pretreating a magnesium alloy matrix; (2) heating the magnesium alloy matrix pretreated in the step (1) to 60-100 ℃, maintaining the temperature of the magnesium alloy matrix at 60-100 ℃, and performing supersonic flame spraying on the surface of the magnesium alloy matrix by taking the iron-based amorphous alloy particles as a material to be sprayed to obtain the iron-based amorphous alloy anticorrosive coating on the surface of the magnesium alloy matrix. In the invention, the magnesium alloy matrix is heated to 60-100 ℃, and the iron-based amorphous alloy anticorrosive coating is sprayed while maintaining the temperature of the magnesium alloy matrix within the temperature range, so that the magnesium alloy matrix is not deformed, and the iron-based amorphous alloy anticorrosive coating can keep an amorphous state, so that the obtained coating has high hardness and excellent corrosion resistance. Experimental results show that the preparation method of the anticorrosive coating provided by the invention can not deform the magnesium alloy substrate, and the surface hardness reaches 580HV0.2And the self-corrosion potential of the iron-based amorphous alloy anticorrosive coating is higher than that of the AZ91 magnesium alloy, and the self-corrosion current density is lower than that of the AZ91 magnesium alloy.
Drawings
FIG. 1 is a cross-sectional view of a magnesium alloy substrate containing an anticorrosive coating obtained in example 1;
FIG. 2 is an XRD pattern of the anticorrosive coating of the Fe-based amorphous alloy obtained in example 1;
FIG. 3 shows polarization curves of the AZ91 magnesium alloy substrate and the Fe-based amorphous alloy anticorrosive coating obtained in example 1.
Detailed Description
The invention provides a preparation method of a magnesium alloy surface anticorrosive coating, which comprises the following steps:
(1) pretreating a magnesium alloy matrix;
(2) heating the magnesium alloy matrix pretreated in the step (1) to 60-100 ℃, maintaining the temperature of the magnesium alloy matrix at 60-100 ℃, and performing supersonic flame spraying on the surface of the magnesium alloy matrix by taking the iron-based amorphous alloy particles as a material to be sprayed to obtain the iron-based amorphous alloy anticorrosive coating on the surface of the magnesium alloy matrix.
The invention carries out pretreatment on the magnesium alloy matrix.
In the present invention, the pretreatment preferably includes cleaning, blasting and polishing, which are performed in this order. In the invention, the cleaning in the pretreatment process can remove oil stains on the surface of the magnesium alloy matrix, the sand blasting treatment can remove an oxide layer on the surface of the magnesium alloy matrix, and the polishing can remove solid particles left in the sand blasting treatment, so that a clean magnesium alloy matrix is obtained, and the binding force between the coating and the matrix is further improved.
In the present invention, the cleaning is preferably ultrasonic cleaning; the cleaning agent is preferably ethanol or acetone. The intensity and time of the ultrasonic cleaning are not particularly limited in the present invention, and can be selected by those skilled in the art as desired. In the present invention, the cleaning can remove oil stains on the surface of the magnesium alloy substrate.
In the present invention, the blasting treatment is preferably dry blasting treatment; the abrasive used for the sand blasting treatment is preferably 20# white corundum sand; the pressure of the sand blasting treatment is preferably 0.65 MPa; the speed of the sand blasting treatment is preferably 0.5 cm/s; the time of the blasting treatment is preferably 5 min.
The polishing mode is not particularly limited, and a person skilled in the art can adjust the polishing mode according to actual conditions and can clean particles on the surface of the magnesium alloy substrate. In the embodiment of the present invention, the grinding is preferably performed by steel brush grinding.
In the invention, the sand blasting treatment and the polishing are preferably carried out within 1-2 hours before the spraying. In the invention, the magnesium alloy matrix is subjected to sand blasting and polishing within 1-2 h before spraying, so that an oxide layer can be prevented from being generated again before spraying.
After the pretreatment is finished, heating the pretreated magnesium alloy matrix to 60-100 ℃, then maintaining the temperature of the magnesium alloy matrix at 60-100 ℃, taking the iron-based amorphous alloy particles as a material to be sprayed, performing supersonic flame spraying on the surface of the magnesium alloy matrix, and obtaining the iron-based amorphous alloy anticorrosive coating on the surface of the magnesium alloy matrix. In the invention, the magnesium alloy matrix is heated to 60-100 ℃, and the iron-based amorphous alloy anticorrosive coating is sprayed while maintaining the temperature of the magnesium alloy matrix within the temperature range, so that the magnesium alloy matrix is not deformed, and the iron-based amorphous alloy anticorrosive coating can keep an amorphous state, so that the obtained coating has high hardness and excellent corrosion resistance.
The heating rate of 60-100 ℃ is not particularly limited, and can be any heating rate.
In the invention, the particle size of the iron-based amorphous alloy particles is preferably 250-300 meshes. In the present invention, the iron-based amorphous alloy particles are preferably dried and then sprayed to enhance the flowability of the powder. The drying mode is not particularly limited, and the dried iron-based amorphous alloy particles can be obtained. In the present embodiment, the drying is preferably vacuum drying; the temperature of the drying is preferably 100 ℃; the drying time is preferably 1-3 h.
In the invention, the supersonic flame spraying speed is preferably 15-25 m/min, and more preferably 20-22 m/min; the flow of the oxygen for supersonic flame spraying is preferably 20-50 m3More preferably 30 to 48 m/h3H; the flow rate of the fuel oil for supersonic flame spraying is preferably 14-25L/h, and more preferably 16-20L/h; the spraying distance of the supersonic flame spraying is preferably 260-380 mm, and more preferably 300-330 mm.
The time of the supersonic flame spraying is not specially limited, and the person skilled in the art can adjust the time of the supersonic flame spraying according to the thickness requirement of the anticorrosive coating. In the embodiment of the invention, the thickness of the iron-based amorphous alloy anticorrosive coating is preferably 300-600 μm.
In the present invention, the fuel is preferably kerosene.
In the invention, the powder feeding amount of the supersonic flame spraying is preferably 20-50 g/min, and more preferably 30-40 g/min.
In the invention, during the supersonic flame spraying process, the temperature of the magnesium alloy substrate is preferably reduced by adopting an air cooling mode. In the invention, the air cooling can slow down the heating rate of the magnesium alloy matrix so as to better maintain the temperature of the magnesium alloy matrix to be 60-100 ℃.
In the invention, the temperature of the magnesium alloy matrix is preferably maintained at 60-100 ℃ by adopting the following method: and when the temperature of the magnesium alloy matrix reaches 100 ℃, stopping the supersonic flame spraying, and continuing the supersonic flame spraying when the temperature of the magnesium alloy matrix is reduced to 60 ℃.
The following will explain the preparation method of the magnesium alloy surface anticorrosive coating provided by the present invention in detail with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Placing the AZ91 magnesium alloy substrate in ethanol for ultrasonic cleaning;
(2) 1h before spraying, carrying out dry sand blasting treatment on the AZ91 magnesium alloy substrate subjected to ultrasonic cleaning, wherein the grinding material used for the sand blasting treatment is 20# white corundum sand, the pressure of the sand blasting treatment is 0.65MPa, the speed of the sand blasting treatment is 0.5cm/s, and the time of the sand blasting treatment is 5 min;
(3) polishing the surface of the AZ91 magnesium alloy substrate subjected to dry sand blasting by using a steel brush, and removing particles to obtain a clean AZ91 magnesium alloy substrate;
(4) drying the iron-based amorphous alloy particles of 250-300 meshes for 1h under a vacuum condition at 100 ℃ to obtain dried iron-based amorphous alloy particles;
(5) fixing the AZ91 magnesium alloy substrate obtained in the step (3); loading the dried iron-based amorphous alloy particles obtained in the step (4) into supersonic flame spraying equipment;
(6) heating the AZ91 magnesium alloy substrate to 60 ℃, carrying out supersonic flame spraying on the surface of the AZ91 magnesium alloy substrate, simultaneously carrying out air cooling on the AZ91 magnesium alloy substrate, stopping the supersonic flame spraying when the temperature of the AZ91 magnesium alloy substrate reaches 100 ℃, continuing the supersonic flame spraying when the temperature of the AZ91 magnesium alloy substrate is reduced to 60 ℃, and repeating the steps until an iron-based amorphous alloy anticorrosive coating with the thickness of 500 mu m is obtained on the surface of the AZ91 magnesium alloy substrate; the spray distance of the supersonic flame spraying is 320mm, and the flow rate of the used oxygen is 48m3The flow rate of kerosene used was 16L/h, the length of the lance used was 5 inches, the speed of supersonic flame spraying was 22m/min, and the powder feed amount was 35 g/min.
The morphology of the cross section of the magnesium alloy substrate with the anticorrosion coating obtained in this example was characterized, and the result is shown in fig. 1. As can be seen from fig. 1, the magnesium alloy substrate with the anticorrosion coating obtained in this example has the anticorrosion coating (i.e., the iron-based amorphous alloy anticorrosion coating) that is well bonded to the substrate, and the coating is dense and has a lamellar structure with few gaps.
The porosity of the corrosion-resistant coating was 2.53% as determined using imagepro6 software.
The self-corrosion potential of the iron-based amorphous alloy anticorrosive coating obtained in the embodiment is detected to be-0.7V and higher than AZ91 magnesium alloy (-1.58V) by adopting an electrochemical workstation method.
The hardness of the iron-based amorphous alloy anticorrosive coating obtained in the embodiment is tested by a Vickers hardness tester and is up to 580HV0.2。
XRD characterization is carried out on the iron-based amorphous alloy anticorrosive coating obtained in the embodiment, and the result is shown in FIG. 2. As can be seen from FIG. 2, the steamed bun-shaped diffuse scattering peak of the amorphous phase appears when the diffraction angle 2 theta is about 44 degrees, and no diffraction peak appears, which indicates that the iron-based amorphous alloy anticorrosive coating has a high-content amorphous structure. The exothermic enthalpy of the amorphous powder and the obtained anticorrosive coating is obtained through DSC test, and the content of the amorphous structure in the iron-based amorphous alloy anticorrosive coating is 88.4 percent calculated by a formula Pcoating ═ Δ Hcoating/Δ Hpowder × 100 percent.
FeCl at 1mol/L2The polarization curves of the AZ91 magnesium alloy substrate and the iron-based amorphous alloy anticorrosive coating obtained in the example were tested in the solution, and the results are shown in FIG. 3. As can be seen from fig. 3, compared with the AZ91 magnesium alloy substrate, the iron-based amorphous alloy anticorrosive coating has a high self-corrosion potential, a longer passivation interval and obvious passivation characteristics, which indicates that a stable passivation film is generated during the corrosion process, and the corrosion resistance of the passivation film is superior to that of the AZ91 magnesium alloy; in addition, the self-corrosion current density of the iron-based amorphous alloy anti-corrosion coating is lower than that of AZ91 magnesium alloy, which shows that the corrosion speed is slower and the corrosion resistance is stronger.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A preparation method of a magnesium alloy surface anticorrosive coating comprises the following steps:
(1) pretreating a magnesium alloy matrix;
(2) heating the magnesium alloy matrix pretreated in the step (1) to 60-100 ℃, maintaining the temperature of the magnesium alloy matrix at 60-100 ℃, and performing supersonic flame spraying on the surface of the magnesium alloy matrix by taking the iron-based amorphous alloy particles as a material to be sprayed to obtain an iron-based amorphous alloy anticorrosive coating on the surface of the magnesium alloy matrix; the temperature of the magnesium alloy matrix is maintained to be 60-100 ℃ by adopting the following method: when the temperature of the magnesium alloy matrix reaches 100 ℃, stopping the supersonic flame spraying, and continuing the supersonic flame spraying when the temperature of the magnesium alloy matrix is reduced to 60 ℃;
the supersonic flame spraying speed is 15-25 m/min, and the flow of oxygen for supersonic flame spraying is 20-50 m3The flow rate of the fuel oil for supersonic flame spraying is 14-25L/h, and the spray distance of the supersonic flame spraying is 260-380 mm; the fuel oil is kerosene; the powder feeding amount of the supersonic flame spraying is 20-50 g/min.
2. The production method according to claim 1, wherein the pretreatment comprises cleaning, blasting and polishing which are performed in this order.
3. The production method according to claim 2, wherein the blasting treatment is dry blasting treatment, the abrasive used in the blasting treatment is 20# white corundum sand, the pressure of the blasting treatment is 0.65MPa, the speed of the blasting treatment is 0.5cm/s, and the time of the blasting treatment is 5 min.
4. The preparation method according to claim 1, wherein the particle size of the iron-based amorphous alloy particles is 250-300 meshes.
5. The preparation method of claim 1, wherein the supersonic flame spraying process is carried out by reducing the temperature of the magnesium alloy substrate by air cooling.
6. The preparation method according to claim 1, wherein the thickness of the iron-based amorphous alloy anticorrosive coating is 300-600 μm.
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