CN112522697A - Method for improving corrosion resistance of cold spraying coating - Google Patents
Method for improving corrosion resistance of cold spraying coating Download PDFInfo
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- CN112522697A CN112522697A CN202011389140.4A CN202011389140A CN112522697A CN 112522697 A CN112522697 A CN 112522697A CN 202011389140 A CN202011389140 A CN 202011389140A CN 112522697 A CN112522697 A CN 112522697A
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/66—Treatment of aluminium or alloys based thereon
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Abstract
The invention relates to a method for improving the corrosion resistance of a cold spraying coating, which comprises the following steps: pretreating the surface of the substrate; cold spraying aluminum powder on the surface of the matrix; and carrying out oxidation treatment on the surface of the cold spraying layer. The invention combines the cold spraying and the in-situ oxidation method, a layer of aluminum coating is cold sprayed on the surface of the magnesium-aluminum alloy, and then the surface of the aluminum coating is oxidized into the corrosion-resistant aluminum oxide film, the aluminum oxide film and the aluminum coating are tightly combined, and the corrosion resistance of the coating is improved.
Description
Technical Field
The invention relates to the technical field of cold spraying, in particular to a method for improving corrosion resistance of a cold spraying layer.
Background
The magnesium-aluminum alloy has small density, high specific strength and specific rigidity and good cutting performance, and is of great significance to light-weight design in the fields of aviation, aerospace, automobiles, electronics and the like. However, magnesium-aluminum alloys have poor corrosion resistance and wear resistance, which has prevented their widespread use.
The surface treatment of the magnesium-aluminum alloy is a common means for improving the corrosion resistance and wear resistance of the magnesium-aluminum alloy. Surface painting is the most widely used surface protection method for industrial applications. The cold spraying is a novel spraying technology based on reasonable utilization of aerodynamic principle. The technology takes high-pressure gas such as helium, nitrogen, argon or air as a carrier, accelerates the carrier through a convergent-divergent nozzle, enables the speed of sprayed particles to reach 300-1200 m/s, impacts the surface of a matrix at a high speed in a solid state, and forms a coating mainly by means of large plastic deformation. The aluminum-based composite material is sprayed on the surface of the magnesium-aluminum alloy in a cold spraying manner, so that the corrosion resistance can be improved when the cold spraying aluminum coating is prepared, but the corrosion resistance of the pure aluminum coating is not good enough. The aluminum-based composite material coating is prepared by introducing a proper amount of ceramic particles into the aluminum coating or adopting alloying measures, so that the corrosion resistance of the aluminum coating is improved, and the coating has higher hardness, strength and wear resistance. However, due to the difference between the properties of the ceramic particles and the aluminum powder, the ceramic particles added in the composite coating still exist in a mechanical mosaic manner, the particles still fall off in the corrosion process to cause pitting corrosion of the coating, and the corrosion resistance is not good enough.
Disclosure of Invention
Based on the method, the cold spraying technology and the in-situ oxidation method are combined, so that the aluminum oxide film is tightly combined with the cold spraying layer, and the corrosion resistance of the cold spraying layer is improved.
The technical scheme of the invention is as follows:
a method of improving the corrosion resistance of a cold sprayed coating comprising the steps of:
pretreating the surface of the substrate;
cold spraying aluminum powder on the surface of the matrix;
and carrying out oxidation treatment on the surface of the cold spraying layer.
In one embodiment, the aluminum powder is spherical, the weight percentage of the aluminum powder with the particle size of 20-30 μm is 20-40%, the weight percentage of the aluminum powder with the particle size of 30-50 μm is 40-60%, and the weight percentage of the aluminum powder with the particle size of 50-70 μm is 10-30%.
The compactness of the coating can be improved by combining the aluminum powder with different particle sizes.
In one embodiment, the aluminum powder is subjected to surface treatment to remove an aluminum oxide film on the surface.
Because a compact alumina layer is formed on the surface of the aluminum powder in the process of storing the aluminum powder again, the yield stress of the alumina layer is greater than that of the aluminum layer wrapped in the alumina layer, and the deposition effect is poor under the lower spraying pressure.
In one embodiment, the aluminum powder surface treatment method comprises the following steps:
soaking aluminum powder in a sodium hydroxide aqueous solution with the concentration of 8-15% and the temperature of 40-60 ℃ until no bubbles are generated on the surface of the aluminum powder;
washing with deionized water;
and (4) drying in the shade by using vacuum cold air to remove surface water vapor, and then carrying out vacuum sealing storage on the aluminum powder.
In some of these embodiments, the cold spray process is: the spraying gas is compressed nitrogen or air, the spraying pressure is 0.6-1.5 Mpa, the distance from the front end of the nozzle to the surface of the base material is 10-30 mm, and the powder feeding speed is 10-30 g/min.
In some embodiments, the thickness of the aluminum cold spraying layer is 20-30 μm.
In some of these embodiments, the process of pretreating the substrate is: and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.7 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra1.0-3.8 mu m.
In some of these embodiments, the oxidation process applied to the cold sprayed layer is: and (3) placing the sprayed workpiece in a reactor, heating to 120-140 ℃, introducing oxygen at the flow rate of 10-20 ml/min, and preserving heat for 10 min.
In some of these embodiments, the oxygen purity is greater than 99.7%.
It is another object of the present invention to provide a corrosion resistant coating prepared by any of the above methods for improving the corrosion resistance of a cold spray coating.
The invention has the beneficial effects that:
(1) the invention combines the cold spraying and the in-situ oxidation method, a layer of aluminum coating is cold sprayed on the surface of the magnesium-aluminum alloy, and then the surface of the aluminum coating is oxidized into the corrosion-resistant aluminum oxide film, the aluminum oxide film and the aluminum coating are tightly combined, and the corrosion resistance of the coating is improved.
(2) The process has low energy consumption, easily obtained raw materials and convenient operation.
Detailed Description
The raw material sources are as follows:
the base material is AZ31B magnesium aluminum alloy with the thickness of 2 cm. The purity of the aluminum powder is 99.95%.
The purity of the oxygen is more than 99.7 percent.
The coating method has simple process and low energy consumption. To a cold sprayed coating with low porosity and good corrosion resistance.
The raw materials not specifically described in the examples and comparative examples were commercially available.
The steps not described in detail in the examples and comparative examples were carried out by a conventional process in the art.
Example 1
The embodiment provides a method for improving the corrosion resistance of a cold spraying layer, which comprises the following steps:
s1, mixing aluminum powder with different grades; weighing 20% by weight of 20-30 μm aluminum powder, 50% by weight of 30-50 μm aluminum powder, and adding 30% by weight of 50-70 μm aluminum powder into a ball mill, wherein the rotating speed of the ball mill is 250-300 r/min, and the ball milling time is 4 h.
S2, performing surface treatment on the aluminum powder mixed in the step S1; the method comprises the following steps:
(1) taking the aluminum powder uniformly mixed in the step S1, adding the aluminum powder into a sodium hydroxide aqueous solution with the mass percentage concentration of 8% and the temperature of 60 ℃, stirring until no bubbles are generated on the surface of the aluminum powder, filtering, and collecting an aluminum powder filter cake;
(2) washing and flushing the aluminum powder filter cake for three times by using deionized water;
(3) and (3) drying in the shade by using vacuum cold air to remove water vapor on the surface of the aluminum powder, and then carrying out vacuum sealing storage on the aluminum powder.
S3, preprocessing the surface of the substrate; and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.5 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra2.0-3.8 mu m.
S4, cold spraying; and cold spraying the aluminum powder subjected to surface treatment to the surface of the substrate pretreated in the step S3, wherein the spraying process parameters are as follows: the gas is compressed air, the spraying pressure is 1.5Mpa, the distance between the front end of the nozzle and the surface of the base material is 10mm, and the powder feeding speed is 10 g/min.
S5, oxidizing; and (4) placing the workpiece sprayed in the step S2 in a reactor of a device to be temperature controlled, heating to 120 ℃, introducing oxygen at the flow rate of 20ml/min, and preserving heat for 10 min.
Example 2
The embodiment provides a method for improving the corrosion resistance of a cold spraying layer, which comprises the following steps:
s1, mixing aluminum powder with different grades; weighing 30 wt% of aluminum powder with the particle size of 20-30 microns, 60 wt% of aluminum powder with the particle size of 30-50 microns, and 10 wt% of aluminum powder with the particle size of 50-70 microns, adding the mixture into a ball mill, wherein the rotating speed of the ball mill is 250-300 r/min, and the ball milling time is 4 hours.
S2, performing surface treatment on the aluminum powder mixed in the step S1; the method comprises the following steps:
(1) taking the aluminum powder uniformly mixed in the step S1, adding the aluminum powder into a sodium hydroxide aqueous solution with the mass percentage concentration of 10% and the temperature of 50 ℃, stirring until no bubbles are generated on the surface of the aluminum powder, filtering, and collecting an aluminum powder filter cake;
(2) washing and flushing the aluminum powder filter cake for three times by using deionized water;
(3) and (3) drying in the shade by using vacuum cold air to remove water vapor on the surface of the aluminum powder, and then carrying out vacuum sealing storage on the aluminum powder.
S3, preprocessing the surface of the substrate; and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.5 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra2.0-3.8 mu m.
S4, cold spraying; and cold spraying the aluminum powder subjected to surface treatment to the surface of the substrate pretreated in the step S3, wherein the spraying process parameters are as follows: the gas is compressed air, the spraying pressure is 1.0Mpa, the distance between the front end of the nozzle and the surface of the base material is 30mm, and the powder feeding speed is 30 g/min.
S5, oxidizing; and (4) placing the workpiece sprayed in the step S2 in a reactor of a device to be temperature controlled, heating to 130 ℃, introducing oxygen at the flow rate of 15ml/min, and preserving heat for 10 min.
Example 3
The embodiment provides a method for improving the corrosion resistance of a cold spraying layer, which comprises the following steps:
s1, mixing aluminum powder with different grades; weighing 40% by weight of aluminum powder with the particle size of 20-30 microns, 40% by weight of aluminum powder with the particle size of 30-50 microns, and adding 20% by weight of aluminum powder with the particle size of 50-70 microns into a ball mill, wherein the rotating speed of the ball mill is 250-300 r/min, and the ball milling time is 4 hours.
S2, performing surface treatment on the aluminum powder mixed in the step S1; the method comprises the following steps:
(1) taking the aluminum powder uniformly mixed in the step S1, adding the aluminum powder into a sodium hydroxide aqueous solution with the mass percentage concentration of 15% and the temperature of 40 ℃, stirring until no bubbles are generated on the surface of the aluminum powder, filtering, and collecting an aluminum powder filter cake;
(2) washing and flushing the aluminum powder filter cake for three times by using deionized water;
(3) and (3) drying in the shade by using vacuum cold air to remove water vapor on the surface of the aluminum powder, and then carrying out vacuum sealing storage on the aluminum powder.
S3, preprocessing the surface of the substrate; and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.5 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra2.0-3.8 mu m.
S4, cold spraying; and cold spraying the aluminum powder subjected to surface treatment to the surface of the substrate pretreated in the step S3, wherein the spraying process parameters are as follows: the gas is compressed air, the spraying pressure is 0.6Mpa, the distance between the front end of the nozzle and the surface of the base material is 20mm, and the powder feeding speed is 20 g/min.
S5, oxidizing; and (4) placing the workpiece sprayed in the step S2 in a reactor of a device to be temperature controlled, heating to 140 ℃, introducing oxygen at the flow rate of 10ml/min, and preserving heat for 10 min.
Example 4
The embodiment provides a method for improving the corrosion resistance of a cold spraying layer, which comprises the following steps:
s1, weighing aluminum powder with the particle size of 30-50 mu m, and carrying out surface treatment; the method comprises the following steps:
(1) taking the aluminum powder uniformly mixed in the step S1, adding the aluminum powder into a sodium hydroxide aqueous solution with the mass percentage concentration of 8% and the temperature of 60 ℃, stirring until no bubbles are generated on the surface of the aluminum powder, filtering, and collecting an aluminum powder filter cake;
(2) washing and flushing the aluminum powder filter cake for three times by using deionized water;
(3) and (3) drying in the shade by using vacuum cold air to remove water vapor on the surface of the aluminum powder, and then carrying out vacuum sealing storage on the aluminum powder.
S2, preprocessing the surface of the substrate; and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.5 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra2.0-3.8 mu m.
S3, cold spraying; and cold spraying the aluminum powder subjected to surface treatment to the surface of the substrate pretreated in the step S3, wherein the spraying process parameters are as follows: the gas is compressed air, the spraying pressure is 1.5Mpa, the distance between the front end of the nozzle and the surface of the base material is 10mm, and the powder feeding speed is 10 g/min.
S4, oxidizing; and (4) placing the workpiece sprayed in the step S2 in a reactor of a device to be temperature controlled, heating to 120 ℃, introducing oxygen at the flow rate of 20ml/min, and preserving heat for 10 min.
Example 5
The present embodiment provides a method of cold spraying a layer, comprising the steps of:
s1, mixing aluminum powder with different grades; weighing 20% by weight of 20-30 μm aluminum powder, 50% by weight of 30-50 μm aluminum powder, and adding 30% by weight of 50-70 μm aluminum powder into a ball mill, wherein the rotating speed of the ball mill is 250-300 r/min, and the ball milling time is 4 h.
S2, preprocessing the surface of the substrate; and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.5 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra2.0-3.8 mu m.
S3, cold spraying; and cold spraying the aluminum powder subjected to surface treatment to the surface of the substrate pretreated in the step S3, wherein the spraying process parameters are as follows: the gas is compressed air, the spraying pressure is 1.5Mpa, the distance between the front end of the nozzle and the surface of the base material is 10mm, and the powder feeding speed is 10 g/min.
S4, oxidizing; and (4) placing the workpiece sprayed in the step S2 in a reactor of a device to be temperature controlled, heating to 120 ℃, introducing oxygen at the flow rate of 20ml/min, and preserving heat for 10 min.
Comparative example 1
The comparative example provides a preparation method of an aluminum powder and aluminum oxide composite cold spraying coating, which comprises the following steps:
s1, weighing 30-50 μm aluminum powder with the particle size of 70 wt%, adding 30% aluminum oxide powder with the particle size of 40-50 μm into a ball mill at the rotating speed of 250-300 r/min for 4h to obtain the spraying powder.
S2, preprocessing the surface of the substrate; and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.5 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra2.0-3.8 mu m.
S3, cold spraying; and cold spraying the spraying powder prepared in the step S1 on the surface of the substrate pretreated in the step S3, wherein the spraying process parameters are as follows: the gas is compressed air, the spraying pressure is 2Mpa, the distance between the front end of the nozzle and the surface of the base material is 10mm, and the powder feeding speed is 10 g/min.
The coatings of examples 1-5 and comparative example 1 were subjected to electrochemical performance experiments, frictional wear experiments, and bonding strength experiments, and their corrosion resistance and mechanical properties were tested.
Experimental example 1 electrochemical Performance test
And performing potentiodynamic polarization test on each coating for 30d of test period, wherein the scanning range is-250 mV-1000 mV (vs. OCP), the scanning speed is 0.3333mV/s, and then fitting the measured polarization curve by adopting C-View software to obtain the experimental result parameters of each sample.
Experimental example 2 frictional wear test
Performing a friction and wear experiment on each coating in a linear contact reciprocating sliding mode, wherein the loading force is 1N, the relative movement speed is 3mm/s, the reciprocating stroke is 10mm, and the coatings are worn 10000 times; the relevant experimental result parameters of each example are obtained.
Experimental example 3 bonding Strength test
The method for testing the bonding strength of the composite coating and the surface of the substrate comprises the following steps: the composite coating is prepared on the surface of a standard wafer-shaped AZ31B magnesium-aluminum alloy substrate with the diameter of 25mm, a round rod is bonded on the outer surface of the composite coating and the outer surface of the substrate, the composite coating and the substrate are pulled apart by a tensile testing machine, and the bonding strength is tested. The results are shown in Table 1.
TABLE 1 test results
As can be seen from table 1, the coatings of examples 1 to 5 have a smaller absolute value of self-corrosion potential and better corrosion resistance than comparative example 1. The self-etching current density is smaller, and the etching speed is lower. The average friction parameter is smaller and the average wear amount is smaller. The bonding strength is higher.
Example 4 is different from example 1 in the composition of only the aluminum powder, indicating that aluminum powders of different particle sizes match to provide better corrosion resistance.
Compared with the example 1, the corrosion resistance and the mechanical property of the aluminum powder are poorer than those of the example 1 because the yield stress of the oxide layer on the surface of the aluminum powder is larger, and the plastic deformation is not easy to generate in the spraying process to influence the deposition of the aluminum powder on the substrate or the coating because the aluminum powder is not subjected to surface treatment in the example 5.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method of improving the corrosion resistance of a cold sprayed coating comprising the steps of:
pretreating the surface of the substrate;
cold spraying aluminum powder on the surface of the matrix;
and carrying out oxidation treatment on the surface of the cold spraying layer.
2. The method for improving the corrosion resistance of a cold spray coating according to claim 1, wherein the aluminum powder is spherical, the weight percentage of the aluminum powder with the particle size of 20-30 μm is 20-40%, the weight percentage of the aluminum powder with the particle size of 30-50 μm is 40-60%, and the weight percentage of the aluminum powder with the particle size of 50-70 μm is 10-30%.
3. The method of improving the corrosion resistance of a cold sprayed coating according to claim 1 wherein the aluminum powder is surface treated to remove a thin film of aluminum oxide from the surface.
4. The method for improving the corrosion resistance of a cold sprayed layer according to claim 3, wherein the aluminum powder surface treatment method comprises the steps of:
soaking aluminum powder in a sodium hydroxide aqueous solution with the concentration of 8-15% and the temperature of 40-60 ℃ until no bubbles are generated on the surface of the aluminum powder;
washing with deionized water;
and (4) drying in the shade by using vacuum cold air to remove surface water vapor, and then carrying out vacuum sealing storage on the aluminum powder.
5. The method for improving the corrosion resistance of the cold spray coating according to any one of claims 1 to 4, wherein the cold spray process is: the spraying gas is compressed nitrogen or air, the spraying pressure is 0.6-1.5 Mpa, the distance from the front end of the nozzle to the surface of the base material is 10-30 mm, and the powder feeding speed is 10-30 g/min.
6. The method for improving the corrosion resistance of a cold sprayed coating according to any one of claims 1 to 4, wherein the thickness of the cold sprayed aluminum powder layer is 20 to 30 μm.
7. The method for improving the corrosion resistance of the cold sprayed coating according to any one of claims 1 to 4, wherein the process for pretreating the substrate comprises: and cleaning and drying the surface of the matrix by using acetone before spraying, and then performing sand blasting and coarsening treatment on the surface of the matrix by using corundum sand with the diameter of 0.4-0.7 mm under the condition that the pressure of compressed air is 0.4MPa to ensure that the roughness reaches Ra1.0-3.8 mu m.
8. The method for improving the corrosion resistance of the cold spray coating according to any one of claims 1 to 4, wherein the cold spray coating is subjected to an oxidation process comprising: and (3) placing the sprayed workpiece in a reactor, heating to 120-140 ℃, introducing oxygen at the flow rate of 10-20 ml/min, and preserving heat for 10 min.
9. The method of increasing the corrosion resistance of a cold sprayed coating of claim 8 where the oxygen purity is greater than 99.7%.
10. A corrosion-resistant cold-sprayed coating produced by the method for improving the corrosion resistance of a cold-sprayed coating according to any one of claims 1 to 9.
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| CN115007848A (en) * | 2022-07-01 | 2022-09-06 | 长安大学 | Coating for retarding crevice corrosion of aluminum-copper connector and preparation method and application thereof |
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