CN112080773A - Electrolyte and aluminum alloy welded joint micro-arc oxidation treatment process - Google Patents

Electrolyte and aluminum alloy welded joint micro-arc oxidation treatment process Download PDF

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Publication number
CN112080773A
CN112080773A CN202010996391.2A CN202010996391A CN112080773A CN 112080773 A CN112080773 A CN 112080773A CN 202010996391 A CN202010996391 A CN 202010996391A CN 112080773 A CN112080773 A CN 112080773A
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aluminum alloy
electrolyte
welding joint
alloy welding
washing
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张伟
苗景国
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Sichuan Engineering Technical College
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Sichuan Engineering Technical College
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/026Anodisation with spark discharge
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated

Abstract

The invention discloses an electrolyte, which comprises the following components in concentration: 0.2-0.8 g/L of sodium hydroxide, 6-14 g/L of sodium tetraborate, 5-10 ml/L of organic amine arc inhibitor, 0.6-2.4 g/L of complexing agent and 5-10 ml/L of hydrogen peroxide. The invention also discloses a micro-arc oxidation treatment process of the aluminum alloy welding joint. The electrolyte and the micro-arc oxidation treatment process can form an oxidation protection film layer on the surface of the aluminum alloy welding joint, the surface of the protection film layer is in a volcano spray opening-shaped convex shape, the hole sealing effect is obvious, the film layer is level and has small waviness, the film layer has large thickness and high microhardness, and therefore the corrosion resistance and the wear resistance are very good.

Description

Electrolyte and aluminum alloy welded joint micro-arc oxidation treatment process
Technical Field
The invention relates to the technical field of micro-arc oxidation, in particular to an electrolyte and an aluminum alloy welding joint micro-arc oxidation treatment process.
Background
The anti-rust aluminum alloy mainly comprises Al-Mn series and Al-Mg series alloys which can not be strengthened by heat treatment. It has good corrosion resistance and weldability. The excellent corrosion resistance enables the antirust alloy to be widely used for marine applications such as ships, automobile and airplane welding parts, subway light rails, pressure vessels needing strict fire prevention and the like. Complicated equipment usually needs to be welded, but because the local connection part adopts welding treatment, protective gas is added in the welding process, welding defects such as base metal melting, smoke dust, splashing, welding deformation and the like and impurities are introduced, so that the mechanical property of a welding joint is deteriorated, the corrosion and the damage of the whole aluminum alloy, particularly a welding area in the service process are accelerated, and great loss is brought to the equipment. Therefore, in order to overcome the defects, the prior art adopts a micro-arc oxidation technology to treat the welding joint of the aluminum alloy.
Micro-arc oxidation (MAO) is a technology for growing an oxide ceramic membrane on the surface of metals such as Al, Mg, Ti, Zr and the like in situ by utilizing the phenomenon of micro-area plasma discharge in electrolyte. The wear resistance, corrosion resistance, insulation and other properties of the material can be obviously improved, the process is simple, and the film and the matrix are tightly combined. The method is applied to the anti-rust aluminum alloy, so that the characteristics of good weldability and low processing cost of the anti-rust aluminum alloy can be fully exerted, the corrosion resistance and the wear resistance of the anti-rust aluminum alloy product (particularly at a welding seam) can be greatly improved, and the purpose of surface coloring can be achieved. However, the aluminum alloy welding joint treated by the existing electrolyte and the micro-arc oxidation process has the problem of poor corrosion resistance and wear resistance.
Disclosure of Invention
The invention aims to solve the problem that an aluminum alloy welding joint subjected to micro-arc oxidation treatment in the prior art is poor in corrosion resistance and wear resistance, and provides an electrolyte and an aluminum alloy welding joint micro-arc oxidation treatment process.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: an electrolyte comprises the following components in concentration: 0.2-0.8 g/L of sodium hydroxide, 6-14 g/L of sodium tetraborate, 5-10 ml/L of organic amine arc inhibitor, 0.6-2.4 g/L of complexing agent and 5-10 ml/L of hydrogen peroxide.
Preferably, the concentration of the sodium tetraborate is 10g/L
Preferably, the organic amine arc inhibitor is triethanolamine.
Preferably, the complexing agent is boric acid.
Further preferably, the mass ratio of the complexing agent to the sodium hydroxide is 3: 1.
The invention also provides a micro-arc oxidation treatment process of the aluminum alloy welding joint, which comprises the following steps:
s1, preprocessing an aluminum alloy welding joint;
s2, polishing the pretreated aluminum alloy welding joint by using sand paper, adding acetone to remove oil, cleaning by using ethanol, cleaning by using deionized water, and drying by using an oven;
s3, putting the aluminum alloy welding joint dried in the step S2 into electrolyte for electrolytic oxidation;
and S4, cleaning the aluminum alloy welding joint subjected to electrolytic oxidation in the step S3 by using deionized water, and then drying in an oven.
Preferably, the parameters of the electrolytic oxidation in the step S3 are: cathode current density 8A/dm2Anode current density 12A/dm2Positive duty ratio of 20%, negative duty ratio of 10%, frequency of 300Hz, and oxidation time of 30 min.
Preferably, the pretreatment of the aluminum alloy welded joint in the step S1 includes the following steps:
A. washing with alkali, namely washing the surface of the aluminum alloy welding joint with a degreasing agent at the temperature of 40-55 ℃ for 5-10 min, and then washing with water in a washing tank;
B. acid washing, namely washing the aluminum alloy welding joint subjected to alkali washing in the step A by using 200-250 g/L lactic acid and 100-120 g/L tartaric acid at the temperature of 40-50 ℃ for 20-40 s, and then washing the aluminum alloy welding joint in a water washing tank;
C. b, performing alkaline etching, namely performing alkaline etching on the aluminum alloy welded joint subjected to the acid cleaning in the step B by using 120-150 g/L sodium hydroxide and 25-35 g/L sodium nitrate at the temperature of 80-90 ℃, treating for 5-10 min, and then putting into a water washing tank for water washing;
D. and drying the washed aluminum alloy welded joint, wherein the temperature of an oven is 90-110 ℃, and the drying time is 30-40 min.
During micro-arc oxidation in the prior art, an electrolyte can form an oxidation film layer on the surface of the aluminum alloy, the oxidation film layer has a protection effect on an aluminum alloy matrix, a plurality of holes are formed in the surface of the oxidation film layer, the holes are generally through holes, the aluminum alloy matrix is communicated with the outside, and the aluminum alloy matrix is easily corroded and abraded. The concentration of the sodium tetraborate in the invention directly influences the size of the holes on the oxide film layer and the thickness and hardness of the oxide film layer. The invention can obtain that when the concentration of the sodium tetraborate is 10g/L, the obtained oxidation film layer has the highest comprehensive indexes of pore size, film layer thickness, hardness, corrosion resistance and wear resistance.
At the initial stage of micro-arc oxidation, numerous small and relatively independent small arc points float on the surface of the aluminum alloy, and along with the extension of micro-arc oxidation time, the small arc points are gathered and aggregated into numerous flaky large arc points, and the positions of the large arc points are relatively fixed and concentrated at one position to flicker, so that an oxide film layer at the position is damaged. After the organic amine inhibitor is added, a protective layer can be quickly formed on the surface of the aluminum alloy substrate, the time for generating a large arc point can be effectively prolonged, the test is finished before the large arc point is generated, the ablation effect of the large arc point is avoided, the hardness of an oxide film is improved, holes are reduced, and the performance of the film is effectively improved.
The sodium hydroxide in the invention, on one hand, increases the conductivity of the solution, on the other hand, adjusts the pH value of the solution, and the film layer is greatly influenced by the over-high or over-low concentration of the sodium hydroxide, and the oxidation film layer is seriously damaged by the over-high concentration of the sodium hydroxide and the over-strong alkalinity; the concentration of sodium hydroxide is too low, the conductivity is reduced, the conductivity of the solution is reduced, the voltage can be increased rapidly, and the oxide film layer can be ablated.
The complexing agent in the invention is boric acid, and the addition of boric acid plays a complexing role, so that the electrolyte has certain stability, and the solution can be repeatedly used for a long time.
The hydrogen peroxide in the invention can provide more oxygen sources for the micro-arc oxidation reaction. The violent oxidation-reduction reaction occurs in the micro-arc oxidation process, and a large amount of oxygen is needed. The hydrogen peroxide can be electrolyzed into a large number of oxygen atoms, and simultaneously, a large number of hydrogen is released to provide a plurality of oxygen sources for the reaction, thereby being beneficial to the smooth proceeding of the micro-arc oxidation reaction.
In conclusion, the oxidation protection film can be formed on the surface of the aluminum alloy welding joint, the surface of the protection film is in a volcano spray opening-shaped convex shape, the hole sealing effect is obvious, the film is level and has small waviness, the film is large in thickness and high in microhardness, and therefore the corrosion resistance and the wear resistance are good.
The invention has the following beneficial effects:
the electrolyte is used for treating the aluminum alloy welding joint, an oxidation protection film layer can be formed on the surface of the aluminum alloy welding joint, the surface of the protection film layer is in a volcano spray opening-shaped convex shape, the hole sealing effect is obvious, the film layer is parallel and level, the waviness is small, the film layer is large in thickness and high in microhardness, and therefore the corrosion resistance and the wear resistance of the aluminum alloy welding joint are remarkably improved;
secondly), the comprehensive performance index of the oxide film layer obtained by micro-arc oxidation is optimal when the concentration of the sodium tetraborate in the electrolyte is 10 g/L.
Drawings
FIG. 1 is a surface appearance and cross-sectional appearance of an oxide film layer of an aluminum alloy welded joint according to the present invention;
FIG. 2 is an appearance and appearance diagram of an aluminum alloy welded joint after an oxidation film corrosion resistance test according to the present invention;
FIG. 3 is a surface topography diagram of the aluminum alloy welded joint of the present invention after the oxide film wear resistance test.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
The electrolyte is prepared from the following components: 0.5g/L of sodium hydroxide, 10g/L of sodium tetraborate, 5ml/L of triethanolamine arc inhibitor, 1.8g/L of boric acid complexing agent and 10ml/L of hydrogen peroxide.
The pretreatment before micro-arc oxidation is carried out on the aluminum alloy welding joint, which comprises the following steps: cleaning the surface of the aluminum alloy welding joint by using a degreasing agent, treating at 55 ℃ for 5min, and then putting into a water washing tank for water washing; pickling the aluminum alloy welded joint subjected to alkali washing with 250g/L lactic acid and 100g/L tartaric acid at the temperature of 50 ℃ for 40s, and then putting the aluminum alloy welded joint into a water washing tank for water washing; carrying out alkaline etching on the aluminum alloy welded joint subjected to acid cleaning by using 130g/L sodium hydroxide and 30g/L sodium nitrate at the temperature of 85 ℃, treating for 8min, and then putting into a water washing tank for water cleaning; and drying the washed aluminum alloy welded joint, wherein the drying oven temperature is 90 ℃, and the drying time is 35 min.
Polishing the pretreated aluminum alloy welding joint by using sand paper, adding acetone to remove oil, cleaning by using ethanol, cleaning by using deionized water, and drying by using an oven; putting the dried aluminum alloy welding joint into electrolyte for electrolytic oxidation, wherein the parameters of the electrolytic oxidation are as follows: cathode current density 8A/dm2Anode current density 12A/dm2Positive duty ratio of 20%, negative duty ratio of 10%, frequency of 300Hz, and oxidation time of 30 min; and cleaning the aluminum alloy welding joint subjected to electrolytic oxidation by using deionized water, and then drying in an oven.
Example 2
The electrolyte is prepared from the following components: 0.2g/L of sodium hydroxide, 6g/L of sodium tetraborate, 7ml/L of triethanolamine arc inhibitor, 2.4g/L of boric acid complexing agent and 8ml/L of hydrogen peroxide.
The pretreatment before micro-arc oxidation is carried out on the aluminum alloy welding joint, which comprises the following steps: cleaning the surface of the aluminum alloy welding joint by using a degreasing agent, treating for 7min at the temperature of 40 ℃, and then putting into a water washing tank for water washing; pickling the aluminum alloy welded joint subjected to alkali washing with 200g/L lactic acid and 120g/L tartaric acid at 45 ℃ for 30s, and then putting the aluminum alloy welded joint into a water washing tank for water washing; performing alkaline etching on the aluminum alloy welded joint subjected to acid cleaning by using 150g/L sodium hydroxide and 30g/L sodium nitrate at the temperature of 80 ℃, treating for 10min, and then putting into a water washing tank for water cleaning; and drying the washed aluminum alloy welding joint, wherein the drying oven temperature is 100 ℃, and the drying time is 40 min.
Polishing the pretreated aluminum alloy welding joint by using sand paper, adding acetone to remove oil, cleaning by using ethanol, cleaning by using deionized water, and drying by using an oven; putting the dried aluminum alloy welding joint into electrolyte for electrolytic oxidation, wherein the parameters of the electrolytic oxidation are as follows: cathode current density 8A/dm2Anode current density 12A/dm2Positive duty ratio of 20%, negative duty ratio of 10%, frequency of 300Hz, and oxidation time of 30 min; and cleaning the aluminum alloy welding joint subjected to electrolytic oxidation by using deionized water, and then drying in an oven.
Example 3
The electrolyte is prepared from the following components: 0.6g/L of sodium hydroxide, 14g/L of sodium tetraborate, 10ml/L of triethanolamine arc inhibitor, 0.6g/L of boric acid complexing agent and 5ml/L of hydrogen peroxide.
The pretreatment before micro-arc oxidation is carried out on the aluminum alloy welding joint, which comprises the following steps: cleaning the surface of the aluminum alloy welding joint by using a degreasing agent, treating at 50 ℃ for 8min, and then putting into a water washing tank for water washing; pickling the aluminum alloy welded joint subjected to alkali washing with 220g/L lactic acid and 110g/L tartaric acid at 40 ℃ for 20s, and then putting the aluminum alloy welded joint into a water washing tank for water washing; performing alkaline etching on the aluminum alloy welded joint subjected to acid cleaning by using 120g/L sodium hydroxide and 30g/L sodium nitrate at the temperature of 85 ℃, treating for 5min, and then putting into a water washing tank for water cleaning; and drying the washed aluminum alloy welding joint, wherein the temperature of an oven is 90 ℃, and the drying time is 30 min.
Polishing the pretreated aluminum alloy welding joint by using sand paper, adding acetone to remove oil, cleaning by using ethanol, cleaning by using deionized water, and drying by using an oven; putting the dried aluminum alloy welding joint into electrolyte for electrolytic oxidation, wherein the parameters of the electrolytic oxidation are as follows: cathode current density 8A/dm2Anode current density 12A/dm2Positive duty ratio of 20%, negative duty ratio of 10%, frequency of 300Hz, and oxidation time of 30 min; and cleaning the aluminum alloy welding joint subjected to electrolytic oxidation by using deionized water, and then drying in an oven.
Performance detection test of micro-arc oxidation film layer of aluminum alloy welding joint under condition of different concentrations of sodium tetraborate
The test method comprises the following steps: a, B, C, D, E5 test groups were set up. A. B, C, D, E5 test groups all adopt the same electrolyte formula and micro-arc oxidation process as those of example 1, and only the concentration of sodium tetraborate is different, and the concentration of sodium tetraborate in A, B, C, D, E electrolyte is 6g/L, 8g/L, 10g/L, 12g/L and 14g/L respectively.
And a result detection method comprises the following steps: the test mainly detects 5 indexes of the size of the hole of the oxidation film layer formed by micro-arc oxidation of the aluminum alloy welding joint, the thickness of the film layer, the hardness of the film layer, the corrosion resistance and the wear resistance, and the specific detection basis is detailed in Table 1
TABLE 1 test results
Serial number Item Basis of detection
1 Thickness of Adopt the portable calibrator of Oualscope
2 Hardness of Adopts an HXS-1000A microhardness meter
3 Corrosion resistance GB/T10125-1997 (salt spray test)
4 Wear resistance MS-T3001 friction wear tester
And (3) analyzing test results:
influence of sodium tetraborate with different concentrations on surface appearance and cross-sectional appearance of oxide film layer
As can be seen from the attached figure 1, a large number of holes in the volcano-jet orifice shape are distributed on the surface of the micro-arc oxidation film layer prepared by A, B, C, D, E5 test groups, the holes are all small, and obvious melting and sintering traces and microcracks with different sizes are arranged around the holes, as shown in B (surface appearance is 5000 times). Fig. 1 illustrates that the invention can obviously reduce the size of the holes formed on the oxide film layer, and has obvious hole sealing effect, for example, as shown in A (surface appearance 5000 times), B (surface appearance 5000 times) and C (surface appearance 5000 times), the holes on the oxide film layer are very small, and the hole sealing effect is obvious.
Influence of different concentrations of sodium tetraborate on thickness and hardness of oxide film layer
TABLE 2
Categories A B C D E
Thickness value of oxide film layer 14.8μm 21.4μm 26.2μm 29.7μm 30.8μm
Hardness value H of oxide film layerV 830 880 905 852 829
The average thickness of the micro-arc oxide film layers prepared by A, B, C, D, E5 test groups in Table 2 is 24.58 μm; an average hardness value of 859.2; the invention shows that the thickness of the oxide film layer formed on the surface of the aluminum alloy welding joint is larger, and the hardness value of the oxide film layer is also higher.
Effect of different concentrations of sodium tetraborate on oxide film corrosion resistance
As can be seen from the attached figure 2, serious corrosion spots and corrosion pits appear on the surface of the aluminum alloy matrix sample after the aluminum alloy matrix sample is corroded for 2 hours, and the surface of the micro-arc oxidation film layer prepared by A, B, C, D, E5 test groups has no change after the aluminum alloy matrix sample is corroded for 48 hours, which shows that the corrosion resistance of the aluminum alloy matrix is greatly improved by the oxidation film layer prepared by the micro-arc oxidation treatment of the electrolyte. The method is mainly characterized in that the micro-arc oxidation film prepared by the method has very small holes, the hole sealing effect is obvious, and the holes are not communicated, so that the corrosion resistance of the oxidation film is greatly improved.
Effect of different concentrations of sodium tetraborate on oxide film abrasion resistance
And taking the time length of the aluminum alloy matrix after being rubbed as a standard for judging the wear resistance of the sample. A. Under the same load, rotating speed and other conditions, the surface of the film layer of B, C, D, E5 test groups is worn uniformly, and no shedding phenomenon is found at the worn part (as shown in figure 3), which indicates that the bonding force between the film layer and the substrate is good. A. The wear time for group B, C, D, E was, in order: 1.65, 1.80, 2.5, 2.2 and 2.05, and has long abrasion time.
In conclusion, the oxide film layer formed by micro-arc oxidation of the electrolyte on the surface of the aluminum alloy welding joint has the characteristics of small holes, large thickness and large hardness, so that the corrosion resistance and the wear resistance of the oxide film layer are obviously improved. Particularly, when the concentration of the sodium tetraborate in the electrolyte is 10g/L, the comprehensive performance index of an oxide film formed by micro-arc oxidation is optimal, holes on the oxide film are small, the thickness of the film is 26.2 mu m, the hardness is 905, the corrosion resistance is good, and the abrasion time is more than or equal to 2.5 min.
The present specification and figures are to be regarded as illustrative rather than restrictive, and it is intended that all such alterations and modifications that fall within the true spirit and scope of the invention, and that all such modifications and variations are included within the scope of the invention as determined by the appended claims without the use of inventive faculty.

Claims (8)

1. The electrolyte is characterized by comprising the following components in concentration: 0.2-0.8 g/L of sodium hydroxide, 6-14 g/L of sodium tetraborate, 5-10 ml/L of organic amine arc inhibitor, 0.6-2.4 g/L of complexing agent and 5-10 ml/L of hydrogen peroxide.
2. The electrolyte of claim 1, wherein the sodium tetraborate concentration is 10 g/L.
3. The electrolyte of claim 1, wherein the organic amine arc suppressor is triethanolamine.
4. The electrolyte of claim 1, wherein the complexing agent is boric acid.
5. The electrolyte of claim 1, wherein the mass ratio of the complexing agent to the sodium hydroxide is 3: 1.
6. The micro-arc oxidation treatment process of the aluminum alloy welding joint is characterized by comprising the following steps of:
s1, preprocessing an aluminum alloy welding joint;
s2, polishing the pretreated aluminum alloy welding joint by using sand paper, adding acetone to remove oil, cleaning by using ethanol, cleaning by using deionized water, and drying by using an oven;
s3, putting the aluminum alloy welding joint dried in the step S2 into electrolyte for electrolytic oxidation;
and S4, cleaning the aluminum alloy welding joint subjected to electrolytic oxidation in the step S3 by using deionized water, and then drying in an oven.
7. The micro-arc oxidation treatment process for the aluminum alloy welded joint according to claim 6, wherein the parameters of the electrolytic oxidation in the step S3 are as follows: cathode current density 8A/dm2Anode current density 12A/dm2Positive duty ratio of 20%, negative duty ratio of 10%, frequency of 300Hz, and oxidation time of 30 min.
8. The micro-arc oxidation treatment process for the aluminum alloy welded joint as claimed in claim 6, wherein the pretreatment of the aluminum alloy welded joint in the step S1 comprises the following steps:
A. washing with alkali, namely washing the surface of the aluminum alloy welding joint with a degreasing agent at the temperature of 40-55 ℃ for 5-10 min, and then washing with water in a washing tank;
B. acid washing, namely washing the aluminum alloy welding joint subjected to alkali washing in the step A by using 200-250 g/L lactic acid and 100-120 g/L tartaric acid at the temperature of 40-50 ℃ for 20-40 s, and then washing the aluminum alloy welding joint in a water washing tank;
C. b, performing alkaline etching, namely performing alkaline etching on the aluminum alloy welded joint subjected to the acid cleaning in the step B by using 120-150 g/L sodium hydroxide and 25-35 g/L sodium nitrate at the temperature of 80-90 ℃, treating for 5-10 min, and then putting into a water washing tank for water washing;
D. and drying the washed aluminum alloy welded joint, wherein the temperature of an oven is 90-110 ℃, and the drying time is 30-40 min.
CN202010996391.2A 2020-09-21 2020-09-21 Electrolyte and aluminum alloy welded joint micro-arc oxidation treatment process Pending CN112080773A (en)

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