CN114836805B - Aluminum alloy surface treatment method - Google Patents
Aluminum alloy surface treatment method Download PDFInfo
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/16—Pretreatment, e.g. desmutting
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
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Abstract
An aluminum alloy surface treatment method comprises the following steps: the method comprises the steps of preprocessing the surface of a matrix, preparing micro-arc oxidation electrolyte, micro-arc oxidation treatment and hole sealing, wherein the micro-arc oxidation electrolyte comprises silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and disodium ethylenediamine tetraacetate, and the impregnating solution used in the hole sealing process comprises sodium acetate, nano titanium powder, nano graphene and sodium silicate; by changing the components of the micro-arc oxidation electrolyte and the impregnating solution, a composite structural layer is formed on the surface of the matrix, and the wear resistance and corrosion resistance of the surface of the matrix are increased.
Description
Technical Field
The application relates to the technical field of material surface processing, in particular to an aluminum alloy surface treatment method.
Background
The micro-arc oxidation is to enhance and activate the reaction on the anode by arc discharge on the basis of common anodic oxidation, thereby forming a high-quality reinforced ceramic film on the surface of a workpiece made of metals such as aluminum, titanium, silicon and the like and alloys thereof.
The traditional preparation process of the micro-arc oxidation ceramic layer is to prepare the micro-arc oxidation ceramic layer by micro-arc oxidation under constant current or constant voltage conditions, and the obtained coating has better corrosion resistance and wear resistance through improving the preparation process although the micro-arc oxidation ceramic layer can play a certain role in protecting a matrix.
Disclosure of Invention
In order to solve the above problems, the present application provides an aluminum alloy surface treatment method, comprising the steps of: the method comprises the steps of substrate surface pretreatment, preparation of micro-arc oxidation electrolyte, micro-arc oxidation treatment and hole sealing, wherein the micro-arc oxidation electrolyte comprises silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and disodium ethylenediamine tetraacetate, and the impregnating solution used in the hole sealing process comprises sodium acetate, nano titanium powder, nano graphene and sodium silicate.
Further, the method sequentially comprises the following steps:
(1) Pretreatment of the surface of a substrate: polishing, impurity removing and degreasing are carried out on the surface of the aluminum alloy matrix;
the surface pretreatment of the matrix removes burrs on the surface of the aluminum alloy matrix and removes surface pollution and greasy dirt caused by the smelting process;
(2) Preparing a micro-arc oxidation electrolyte: adding silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and disodium ethylenediamine tetraacetate into deionized water, and performing ultrasonic dispersion;
the ultrasonic dispersion time is at least 3 hours, so that substances in the micro-arc oxidation electrolyte are fully dispersed;
(3) Micro-arc oxidation treatment: immersing the substrate material subjected to surface pretreatment into the prepared micro-arc oxidation electrolyte for micro-arc oxidation;
in the micro-arc oxidation process, the nano graphene plays a role in conducting electricity;
disodium ethylenediamine tetraacetate is used as a complexing agent;
sodium hydroxide provides an alkaline environment;
(4) And (3) hole sealing: placing the material subjected to the micro-arc oxidation treatment into impregnating liquid for impregnating, and then cleaning and drying;
in the hole sealing process, the nano graphene plays a role in loading, and micro holes and cracks generated by the ceramic film in the micro-arc oxidation process are filled, so that the corrosion resistance is improved.
Further, the micro-arc oxidation electrolyte comprises 1.5-1.8 parts of silicate, 2.5-3.2 parts of manganese powder, 3.5-5.5 parts of silicon powder, 2-4 parts of silicon carbide particles, 0.4-0.8 part of nano graphene, 0.5-0.6 part of sodium hydroxide and 1.2-1.3 parts of ethylenediamine tetraacetic acid disodium salt.
Further, the silicate is sodium silicate, the particle size of the sodium silicate is 50-80 nm, the particle size of the silicon carbide particles is 10-20 mu m, the particle size of the manganese powder is 2-10 mu m, and the particle size of the silicon powder is 2-10 mu m.
In the micro-arc oxidation process, silicon carbide particles, manganese powder and silicon powder with larger particle sizes can be precipitated to a certain extent and are precipitated on the surface of an aluminum alloy matrix, and each component is melted and mixed together due to the high temperature of micro-arc oxidation.
Further, the micro-arc oxidation is carried out, wherein a matrix material is used as an anode to be connected with a lead, the voltage of the micro-arc oxidation is 300-350V, the forward duty ratio is less than 25%, and the total time of the micro-arc oxidation is 3min.
Further, in the micro-arc oxidation, the temperature of the micro-arc oxidation electrolyte is 5-10 ℃.
The micro-arc oxidation time is short, and the low temperature of the electrolyte is more favorable for the stable formation of the ceramic layer.
Further, the impregnating solution comprises 1.0-1.5 parts of sodium acetate, 0.3-0.5 parts of nano titanium powder, 0.3-0.8 parts of nano graphene and 1.0-1.2 parts of sodium silicate.
Further, the soaking temperature is 50 ℃, the soaking time is 5-7 h, the drying temperature is 60-65 ℃, and the drying time is 20-24 h.
Further, a composite structure layer is formed on the surface of the aluminum alloy matrix, wherein the composite structure layer is a composite structure layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
Further, the thickness of the composite structure layer is less than 30 mu m.
The micro-arc oxidation time is short, the formed composite structure layer is thinner, but the formed composite structure layer has uniform components and stable performance.
The application has the following beneficial effects:
1. according to the application, by changing the components of the micro-arc oxidation electrolyte and the impregnating solution, a composite structural layer is formed on the surface of the substrate, so that the wear resistance and corrosion resistance of the surface of the substrate are increased.
2. According to the application, nano graphene is added into the micro-arc oxidation electrolyte, and the electrochemical performance of the electrolyte is increased by utilizing the conductivity of the nano graphene.
3. According to the application, the silicon carbide particles are added into the micro-arc oxidation electrolyte, so that the silicon carbide particles enter the ceramic layer, and the wear resistance is improved.
4. In the hole sealing process, the micro holes and cracks of the ceramic film are filled by utilizing the loading property of the nano graphene, so that the filling effect is better, and the performance of the composite structural layer is improved.
5. The application uses low-temperature electrolyte and shorter micro-arc oxidation time to stabilize the formed ceramic layer, and has fewer generated micro holes and cracks.
6. The application utilizes the instant high temperature generated during micro-arc oxidation to enable silicon and manganese to be doped into the aluminum alloy, and the aluminum alloy is matched with the generated ceramic layer to form a composite structure layer, so that the wear resistance and corrosion resistance of the surface of the aluminum alloy matrix are improved.
Detailed Description
In order to clearly illustrate the technical characteristics of the scheme, the application is explained in detail by the following specific embodiments.
In a specific embodiment of the present application, the matrix material used is 5052 aluminum alloy.
Example 1:
the composite structural layer is produced according to the following steps, which sequentially comprise the following steps:
(1) Pretreatment of the surface of a substrate: polishing the surface of the matrix by using sand paper, and cleaning the surface of the matrix by using absolute ethyl alcohol and deionized water after finishing treatment;
(2) Preparing a micro-arc oxidation electrolyte: adding 1.5 parts of sodium silicate with the particle size of 50nm, 0.5 part of sodium hydroxide, 0.4 part of nano graphene, 2.5 parts of manganese powder with the particle size of 2-10 mu m, 3.5 parts of silicon powder with the particle size of 2-10 mu m, 2 parts of silicon carbide particles with the particle size of 10-20 mu m and 1.2 parts of ethylene diamine tetraacetic acid disodium salt into 1000 parts of deionized water, and performing ultrasonic dispersion for 3 hours;
(3) Micro-arc oxidation treatment: immersing the substrate subjected to surface pretreatment into a prepared micro-arc oxidation electrolyte, connecting the substrate serving as an anode with a wire, wherein the temperature of the micro-arc oxidation electrolyte is 5 ℃, the micro-arc oxidation voltage is 300V, the forward duty ratio is less than 25%, and the total micro-arc oxidation duration is 3min;
(4) And (3) hole sealing: and (3) putting the material subjected to the micro-arc oxidation treatment into an impregnating solution of 1000 parts of deionized water, 1.0 part of sodium acetate, 0.3 part of nano titanium powder, 0.3 part of nano graphene and 1.0 part of sodium silicate, wherein the impregnating temperature is 50 ℃, the impregnating time is 5 hours, and then cleaning and drying the material, wherein the drying temperature is 60 ℃ and the drying time is 20 hours.
It can be understood that a composite structural layer is formed on the surface of the aluminum alloy matrix, and the composite structural layer is a composite structural layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
It will be appreciated that the composite structural layer is produced to a thickness of less than 30 μm.
Example 2:
the composite structural layer is produced according to the following steps, which sequentially comprise the following steps:
(1) Pretreatment of the surface of a substrate: polishing the surface of the matrix by using sand paper, and cleaning the surface of the matrix by using absolute ethyl alcohol and deionized water after finishing treatment;
(2) Preparing a micro-arc oxidation electrolyte: adding 1.6 parts of sodium silicate with the diameter of 70nm, 0.55 part of sodium hydroxide, 0.6 part of nano graphene, 3 parts of manganese powder with the particle size of 2-10 mu m, 4 parts of silicon powder with the particle size of 2-10 mu m, 3 parts of silicon carbide particles with the particle size of 10-20 mu m and 1.25 parts of ethylene diamine tetraacetic acid disodium salt into 1000 parts of deionized water, and performing ultrasonic dispersion for 3 hours;
(3) Micro-arc oxidation treatment: immersing the substrate subjected to surface pretreatment into a prepared micro-arc oxidation electrolyte, connecting the substrate serving as an anode with a wire, wherein the temperature of the micro-arc oxidation electrolyte is 8 ℃, the voltage of micro-arc oxidation is 320V, the forward duty ratio is less than 25%, and the total duration of micro-arc oxidation is 3min;
(4) And (3) hole sealing: and (3) putting the material subjected to the micro-arc oxidation treatment into an impregnating solution of 1000 parts of deionized water, 1.25 parts of sodium acetate, 0.4 part of nano titanium powder, 0.5 part of nano graphene and 1.1 part of sodium silicate, wherein the impregnating temperature is 50 ℃, the impregnating time is 6 hours, and then cleaning and drying the material, wherein the drying temperature is 62 ℃ and the drying time is 22 hours.
It can be understood that a composite structural layer is formed on the surface of the aluminum alloy matrix, and the composite structural layer is a composite structural layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
It will be appreciated that the composite structural layer is produced to a thickness of less than 30 μm.
Example 3:
the composite structural layer is produced according to the following steps, which sequentially comprise the following steps:
(1) Pretreatment of the surface of a substrate: polishing the surface of the matrix by using sand paper, and cleaning the surface of the matrix by using absolute ethyl alcohol and deionized water after finishing treatment;
(2) Preparing a micro-arc oxidation electrolyte: adding 1.8 parts of sodium silicate with the particle size of 80nm, 0.6 part of sodium hydroxide, 0.8 part of nano graphene, 3.2 parts of manganese powder with the particle size of 2-10 mu m, 5.5 parts of silicon powder with the particle size of 2-10 mu m, 4 parts of silicon carbide particles with the particle size of 10-20 mu m and 1.3 parts of ethylene diamine tetraacetic acid disodium salt into 1000 parts of deionized water, and performing ultrasonic dispersion for 3 hours;
(3) Micro-arc oxidation treatment: immersing the substrate subjected to surface pretreatment into a prepared micro-arc oxidation electrolyte, connecting the substrate serving as an anode with a wire, wherein the temperature of the micro-arc oxidation electrolyte is 10 ℃, the voltage of micro-arc oxidation is 350V, the forward duty ratio is less than 25%, and the total duration of micro-arc oxidation is 3min;
(4) And (3) hole sealing: and (3) putting the material subjected to the micro-arc oxidation treatment into an impregnating solution of 1000 parts of deionized water, 1.5 parts of sodium acetate, 0.5 part of nano titanium powder, 0.8 part of nano graphene and 1.2 parts of sodium silicate, wherein the impregnating temperature is 50 ℃, the impregnating time is 7 hours, and then cleaning and drying the material, wherein the drying temperature is 65 ℃ and the drying time is 24 hours.
It can be understood that a composite structural layer is formed on the surface of the aluminum alloy matrix, and the composite structural layer is a composite structural layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
It will be appreciated that the composite structural layer is produced to a thickness of less than 30 μm.
Comparative example:
comparative example the comparative example was set with reference to example 1, except for the specific explanation, the other conditions were the same as in example 1.
TABLE 1
Detection data:
(1) Corrosion resistance test
The testing means: the tafel curves of the samples were tested using an electrochemical workstation.
Test conditions: the three-electrode system is adopted, the auxiliary electrode is a platinum electrode, the reference electrode is a saturated calomel electrode, a sample to be tested is used as a research electrode, and the test medium is 3% NaCl aqueous solution.
Because the adopted treatment modes are approximately the same, the corrosion currents of all the materials are approximately the same, and under the condition that the corrosion currents are not different greatly, the corrosion resistance of the materials is mainly reflected on the corrosion potential, and the higher the corrosion potential is, the better the corrosion resistance of the materials is.
TABLE 2
(2) Wear resistance test
The testing means: MXD-02 coefficient of friction meter using Labthink blue light.
Test conditions: the friction coefficient was measured according to GB/T10006-1988 standard.
The testing means: a PHASE II micro vickers hardness tester was used.
Test conditions: the test was performed according to GB/T4340.3-2012, and the Vickers hardness was measured.
TABLE 3 Table 3
(3) Stability test
The testing means: the wear test is carried out by adopting an MRH-2 type high-speed ring block wear tester.
Test conditions: the temperature and the room temperature, the relative humidity and the rotating speed are respectively 50 percent, the rotating speed is 200r/min, the load is 100N, and after friction is carried out for 2 hours, 4 hours and 6 hours, the test is carried out according to the method used in the corrosion resistance test (1) and the abrasion resistance test (2).
TABLE 4 Table 4
From the results of the test data, silicon powder and manganese powder are added in the micro-arc oxidation process to improve the corrosion resistance of the composite structural layer, and silicon carbide and nano graphene are added to improve the wear resistance of the composite structural layer.
In the dipping process, the corrosion resistance can be improved by adding nano graphene and titanium powder, and the wear resistance can be improved by adding sodium silicate.
Comparative example 9 is a raw aluminum alloy, and the raw aluminum alloy not subjected to surface treatment is low in corrosion potential and vickers hardness as compared with other treated examples or comparative examples.
In the test of the friction coefficient of comparative example 9, the measured data is the friction coefficient of the original aluminum alloy, the influencing factor is mainly the roughness of the surface of the original aluminum alloy, and the reference value of the experimental data is not great.
In the comparison of example 5 and example 1, the electrolysis time is too long, the performance of the obtained composite structural layer is reduced, the electrolysis time is too long, so that tiny holes and cracks in the formed ceramic layer are increased, and after the composite structural layer with a certain thickness is formed, the components are reduced, the comprehensive performance is reduced, and the performance of the subsequently formed film layer is difficult to reach the required standard due to the defects in the micro-arc oxidation process.
In the stability test, the composite structural layer formed on the surface of the substrate was worn after long-time friction in example 1 and comparative example 5, and the composite structural layer in example 1 was basically damaged after 6 hours of wear due to the thinner composite structural layer formed in example 1, and the properties of the composite structural layer were not much different from those of the aluminum alloy substrate.
In comparative example 5, the composite structural layer is thicker due to long micro-arc oxidation time, but the micro-arc oxidation time is too long, micro holes and cracks of the composite structural layer are increased, the performance of the obtained composite structural layer is poor, after a period of abrasion, part of the composite structural layer with poor external comprehensive performance of the composite structural layer is abraded, and the composite structural layer with less internal holes and cracks and excellent performance is exposed, so that after 6 hours of abrasion experiment, the measured experimental data of comparative example 5 are better than the data measured at the beginning, and each performance is excellent.
The steps used in the present application are indispensable in comparison with examples 9, 10 and example 1, and have an effect on the properties of the final composite structural layer.
In this specification, each embodiment is described in a progressive manner, and identical and similar parts of each embodiment are all referred to each other, and each embodiment mainly describes differences from other embodiments. In particular, for system embodiments, since they are substantially similar to method embodiments, the description is relatively simple, as relevant to see a section of the description of method embodiments.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are to be included in the scope of the claims of the present application.
Claims (10)
1. The aluminum alloy surface treatment method is characterized by comprising the following steps of: pretreating the surface of a matrix, preparing micro-arc oxidation electrolyte, performing micro-arc oxidation treatment and sealing holes;
the micro-arc oxidation electrolyte comprises silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and ethylenediamine tetraacetic acid disodium salt, and the impregnating solution used in the hole sealing process comprises sodium acetate, nano titanium powder, nano graphene and sodium silicate.
2. The method for treating the surface of the aluminum alloy according to claim 1, comprising the following steps in order:
(1) Pretreatment of the surface of a substrate: polishing, impurity removing and degreasing are carried out on the surface of the aluminum alloy matrix;
(2) Preparing a micro-arc oxidation electrolyte: adding silicate, sodium hydroxide, nano graphene, silicon powder, manganese powder, silicon carbide particles and disodium ethylenediamine tetraacetate into deionized water, and performing ultrasonic dispersion;
(3) Micro-arc oxidation treatment: immersing the substrate material subjected to surface pretreatment into the prepared micro-arc oxidation electrolyte for micro-arc oxidation;
(4) And (3) hole sealing: and (3) placing the material subjected to the micro-arc oxidation treatment into impregnating solution for impregnation, and then cleaning and drying.
3. The method for treating the surface of an aluminum alloy according to claim 1, wherein: the micro-arc oxidation electrolyte comprises 1.5-1.8 parts of silicate, 2.5-3.2 parts of manganese powder, 3.5-5.5 parts of silicon powder, 2-4 parts of silicon carbide particles, 0.4-0.8 part of nano graphene, 0.5-0.6 part of sodium hydroxide and 1.2-1.3 parts of ethylenediamine tetraacetic acid disodium salt.
4. The method for treating the surface of an aluminum alloy according to claim 1, wherein: the silicate is sodium silicate, the particle size of the sodium silicate is 50-80 nm, the particle size of the silicon carbide particles is 10-20 mu m, the particle size of the manganese powder is 2-10 mu m, and the particle size of the silicon powder is 2-10 mu m.
5. The method for treating the surface of an aluminum alloy according to claim 1, wherein: and the micro-arc oxidation is carried out, wherein a matrix material is used as an anode to be connected with a lead, the voltage of the micro-arc oxidation is 300-350V, the forward duty ratio is less than 25%, and the total time of the micro-arc oxidation is 3min.
6. The method for treating the surface of an aluminum alloy according to claim 1, wherein: and in the micro-arc oxidation, the temperature of the micro-arc oxidation electrolyte is 5-10 ℃.
7. The method for treating the surface of an aluminum alloy according to claim 1, wherein: the impregnating solution comprises 1.0-1.5 parts of sodium acetate, 0.3-0.5 parts of nano titanium powder, 0.3-0.8 parts of nano graphene and 1.0-1.2 parts of sodium silicate.
8. The method for treating the surface of an aluminum alloy according to claim 1, wherein: the soaking temperature is 50 ℃, the soaking time is 5-7 h, the drying temperature is 60-65 ℃, and the drying time is 20-24 h.
9. The aluminum alloy surface treatment method according to any one of claims 1 to 8, characterized by comprising the steps of: and forming a composite structure layer on the surface of the aluminum alloy matrix, wherein the composite structure layer is a composite structure layer formed by mixing aluminum, manganese, silicon, aluminum silicate, nano graphene, silicon carbide and titanium.
10. The method for surface treatment of aluminum alloy according to claim 9, wherein: the thickness of the composite structure layer is less than 30 mu m.
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