CN111441074A - Anodic oxidation treatment method for surface of aluminum alloy plate - Google Patents
Anodic oxidation treatment method for surface of aluminum alloy plate Download PDFInfo
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- CN111441074A CN111441074A CN202010359466.6A CN202010359466A CN111441074A CN 111441074 A CN111441074 A CN 111441074A CN 202010359466 A CN202010359466 A CN 202010359466A CN 111441074 A CN111441074 A CN 111441074A
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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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/32—Alkaline compositions
- C23F1/36—Alkaline compositions for etching aluminium or alloys thereof
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/12—Light metals
- C23G1/125—Light metals aluminium
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/22—Light metals
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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
- C25D11/16—Pretreatment, e.g. desmutting
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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
- C25D11/246—Chemical after-treatment for sealing layers
Abstract
The invention discloses an aluminum alloy plate surface anodic oxidation treatment method with high strength and high adhesion characteristics, which comprises the steps of degreasing the surface of an aluminum alloy raw material, alkaline etching, anodic oxidation and the like. The aluminum alloy treated by the method has high application value in the application of the composite material, particularly in the composite application of the aluminum alloy and the non-metal material, on one hand, the aluminum alloy can be better bonded with the non-metal material to improve the comprehensive performance, and on the other hand, the wear resistance, the corrosion resistance and the surface hardness of the surface of the aluminum alloy can be enhanced. In addition, an anti-electric layer can be formed between the aluminum alloy treated by the process and the interlayer of the combined non-metal material, so that the electrochemical corrosion phenomenon is prevented, and the stability of the aluminum-based non-metal composite material can be greatly improved.
Description
Technical Field
The invention relates to the technical field of aluminum alloy plate processing, in particular to a surface anodic oxidation treatment method of an aluminum alloy plate with high strength and high adhesion.
Background
The aluminum alloy material has wide application in various fields by the characteristics of weldability, easy forming, small relative density and high mechanical strength, and can be applied to aerospace, architectural decoration and daily life. The metal aluminum is easy to react with oxygen in the air to generate a film of aluminum oxide, but the strength of the film is poor, and the thickness of the film is too low, so that the film cannot play a good protection role.
At present, the surface oxidation film is generally formed on the aluminum alloy by anodic oxidation treatment in the market, but as mentioned above, the surface of the aluminum alloy anodic oxidation film prepared by the general method has high porosity and strong adsorbability, so the aluminum alloy anodic oxidation film is easily corroded by the external environment and loses the protection effect under long-term use.
Moldings made from laminates (also called metal fiber laminates, fiber metal fiber laminates or laminates) comprising at least one aluminum alloy sheet and at least one fiber-reinforced polymer layer bonded thereto are increasingly used in all kinds of industries, such as the transportation industry, and can be applied to automobiles, trains, aircraft and spacecraft.
In order to increase the adhesive force between the aluminum alloy plate and the binding resin during the lamination treatment of the aluminum alloy plate, the surface of the aluminum alloy plate needs to be treated, firstly, the surface of the aluminum alloy plate is roughened, and secondly, impurities such as oil seal, oil dirt, spot rust and the like on the surface of the aluminum alloy plate are removed; in addition, aluminum is an active metal, and a layer of compact oxide film is formed on the surface of the aluminum in dry air immediately, so that the aluminum is not further oxidized and can resist water; however, as described above, since the aluminum oxide film is relatively secured, the local oxide film is broken by mechanical friction or the like during storage, and rust is taken into the inside of the film, and therefore, a treatment for removing the oxide film is required. However, the existing surface treatment methods all have certain defects, specifically, the prepared aluminum alloy surface oxide film has general strength and poor adhesive property, so that the treated aluminum alloy plate cannot meet the production requirements of laminated plates.
Disclosure of Invention
In view of the above circumstances, the technical problems to be solved by the present invention are: provides an anodic oxidation method of an aluminum alloy plate, which aims to solve the problems that the aluminum alloy plate prepared by the conventional technology has poor bonding performance of an oxide film and can not meet the performance strength of a laminated plate.
In order to solve the problems, the invention provides an anodic oxidation treatment method for the surface of an aluminum alloy plate, which is characterized by comprising the following steps:
s1, surface polishing treatment: carrying out surface grinding and polishing treatment on the aluminum alloy plate by using a grinding machine and a polishing machine;
s2, pre-degreasing, namely immersing the aluminum alloy plate subjected to surface polishing in the step S1 into a dilute sulfuric acid solution with the concentration of 150-220 g/L, soaking for 2-10min at the temperature of 40-60 ℃, and then repeatedly washing the plate surface for 3min by using water to obtain a pre-degreased aluminum alloy plate;
s3, degreasing treatment: immersing the pre-degreased aluminum alloy plate obtained by the pre-degreasing treatment in the step S2 into an alkaline degreasing agent, and soaking for 10-20min at the temperature of 50-70 ℃ to obtain a degreased aluminum alloy plate;
s4, alkaline etching treatment: immersing the degreased aluminum alloy plate obtained by the degreasing treatment of S3 in alkaline etching solution, soaking for 5-20min at the temperature of 55-60 ℃, and then washing with water to obtain the alkaline etching aluminum alloy plate;
s5, anodic oxidation: carrying out anodic oxidation treatment on the alkali-etched aluminum alloy plate obtained by the alkali etching treatment of S4 in a sulfuric acid solution, keeping the temperature of the solution at 17-20 ℃, the current density at 1.5-2.0A/dm2, carrying out oxidation reaction for 8-15min, taking out after an oxide film is generated on the aluminum alloy plate for a period of time, and repeatedly washing the aluminum alloy plate for 3-4min by using pure water;
s6, sealing with boiling water: and (3) placing the aluminum alloy plate after the anodic oxidation of S5 in a sealing additive, sealing with boiling water, and taking out to obtain the treated aluminum alloy plate.
Preferably, in the step S1, after the surface of the aluminum alloy plate is roughly ground by 150 meshes, the surface is finely ground by 500-1500 meshes, and is washed by pure water, and finally is cleaned by ethanol and dried.
Preferably, the alkaline degreasing agent in the step S2 comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
Preferably, the alkaline etching solution in step S4 contains 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate, and 34 g/L of sorbitol as main components.
Preferably, the bath solution for anodic oxidation in the step S5 includes dilute sulfuric acid and Fe2(SO4)3Wherein the concentration of the dilute sulfuric acid is 170-190 g/L, Fe2(SO4)3It was 127 g/L.
Preferably, in the step S5, the aluminum alloy plate is taken out from the sulfuric acid solution after the thickness of the aluminum alloy plate reaches 4-8 μm
Preferably, in step S6, the condition of boiling water sealing is to soak at 55-60 ℃ for 5-20 min.
The aluminum alloy plate is prepared by reasonably polishing, degreasing, alkaline etching, anodizing and boiling water sealing the raw materials of the aluminum alloy plate, the bonding property of an oxide film is stronger, and the prepared anodic oxide film can effectively protect the surface of the aluminum alloy plate and prevent the aluminum alloy plate from being damaged by external corrosion; meanwhile, the aluminum alloy plate prepared by the invention can be better applied to composite materials, can be better bonded with non-metallic materials, and can improve the comprehensive performance of the non-metallic materials; the method is simple, complex equipment is not needed, the finally prepared product has excellent performance, can be applied to the treatment of various aluminum alloys, and has higher commercial value and popularization value.
Drawings
FIG. 1 is a flow chart of the surface treatment process of the present invention;
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, washing the sample with pure water for 3min, and finally washing and drying the sample with ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid, maintaining the solution temperature at 17-20 deg.C, current density at 1.4-1.8A/dm2, and oxidizing for 8-15min to reach oxide film thickness of 4-8 μm, taking out, and repeatedly washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 2:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand mill, then continuously and finely polishing the sample under the condition of 500 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.4A/dm2Carrying out anodic oxidation reaction for 10min to make the thickness of the oxide film reach 4-8 μm, taking out, and repeatedly washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 3:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand mill, then continuously and finely polishing the sample under the condition of 500 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.6A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 4:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand mill, then continuously and finely polishing the sample under the condition of 500 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.8A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 5:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand polisher, then continuously and finely polishing the sample under the condition of 1000 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.4A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 6:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand polisher, then continuously and finely polishing the sample under the condition of 1000 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.6A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 7:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand polisher, then continuously and finely polishing the sample under the condition of 1000 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.8A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 8:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand polisher, then continuously and finely polishing the sample under the condition of 1500 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.4A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 9:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand polisher, then continuously and finely polishing the sample under the condition of 1500 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.6A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Example 10:
1. preparing acid solution, namely preparing dilute sulfuric acid solution with the concentration of 150-220 g/L for later use;
2. preparing alkaline degreasing liquid, wherein the alkaline degreasing liquid comprises 8 g/L of sodium silicate, 6 g/L of sodium carbonate, 3.175 g/L of sodium polyphosphate, 0.5 g/L of surfactant, 15 g/L of surfactant and 6 g/L of triethanolamine undecanedioate.
3. The main components of the caustic etching solution are 60 g/L of NaOH, 160 g/L of sodium gluconate, 3 g/L of sodium dodecyl sulfate and 34 g/L of sorbitol.
4. Preparing anodic oxidation bath solution, wherein the concentration of dilute sulphuric acid is 170-190 g/L, and the concentration of Fe2(SO4)3 is 127 g/L.
5. Taking an aluminum alloy plate sample with the thickness of 2mm, roughly polishing the sample to 150 meshes by using a sand polisher, then continuously and finely polishing the sample under the condition of 1500 meshes, then washing the sample for 3min by using pure water, and finally washing and drying the sample by using ethanol. Then immersing into prepared acid liquor, heating to 40-60 ℃, staying for 2-10min, repeatedly washing the plate surface for 3min by using tap water after use, and obtaining a pre-degreased aluminum alloy plate; then immersing the aluminum alloy plate into a certain amount of alkaline degreasing agent, and staying for 10-20min at 50-70 ℃ to obtain a degreased aluminum alloy plate; immersing the aluminum alloy plate into alkaline etching solution, staying for 5-20min at 55-60 ℃, and then washing with pure water to obtain an alkaline etching aluminum alloy plate; anodizing with sulfuric acid at 17-20 deg.C and current density of 1.8A/dm2 for 10min to obtain oxide film with thickness of 4-8 μm, and washing with pure water for 3-4 min; and finally, placing the anodized aluminum alloy plate in a sealing additive, and sealing with boiling water at the temperature of over 96 ℃ for 20min to obtain the treated aluminum alloy plate.
6. Finally, the treated aluminum alloy sheet was cured and bonded with an adhesive (e.g., a one-component epoxy resin) under the same conditions, and the tensile shear strength was measured, and the tensile shear strength was as shown in table 1 below.
Table 1: examples 1-10 tensile shear Strength of aluminum alloy sheets after bonding
| Examples | Tensile shear strength |
| Example 1 | 8.24MPa |
| Example 2 | 12.03MPa |
| Example 3 | 14.89MPa |
| Example 4 | 14.30MPa |
| Example 5 | 13.01MPa |
| Example 6 | 15.8MPa |
| Example 7 | 14.52MPa |
| Example 8 | 12.26MPa |
| Example 9 | 15.13MPa |
| Example 10 | 14.81MPa |
From the tests in Table 1, it can be seen that the tensile shear strength of the aluminum alloy sheet obtained by the present invention after bonding is relatively excellent, especially after reasonable grinding and polishing, the bonding performance is optimal, the most preferable example in the present invention is example 6, when the grinding and polishing conditions are 1000 mesh, the anodic oxidation current is 1.6A/dm2, the bonding performance and the final tensile shear strength are optimal, and further, when the anodic oxidation current is 1.616A/dm2, the obtained aluminum alloy product forms an oxide film, and the bonding performance is optimal.
The foregoing has described preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary, and various changes made within the scope of the independent claims of the present invention are within the scope of the present invention.
Claims (7)
1. The surface anodic oxidation treatment method of the aluminum alloy plate is characterized by comprising the following steps of:
s1, surface polishing treatment: carrying out surface polishing treatment on the aluminum alloy plate by using a sand grinder and a polishing machine;
s2, pre-degreasing, namely immersing the aluminum alloy plate subjected to surface polishing in the step S1 into a dilute sulfuric acid solution with the concentration of 150-220 g/L, soaking for 2-10min at the temperature of 40-60 ℃, and then repeatedly washing the plate surface for 3min by using water to obtain a pre-degreased aluminum alloy plate;
s3, degreasing treatment: immersing the pre-degreased aluminum alloy plate obtained by the pre-degreasing treatment in the step S2 into an alkaline degreasing agent, and soaking for 10-20min at the temperature of 50-70 ℃ to obtain a degreased aluminum alloy plate;
s4, alkaline etching treatment: immersing the degreased aluminum alloy plate obtained by the degreasing treatment of S3 in alkaline etching solution, soaking for 5-20min at the temperature of 55-60 ℃, and then washing with water to obtain the alkaline etching aluminum alloy plate;
s5, anodic oxidation: carrying out anodic oxidation treatment on the alkali-etched aluminum alloy plate obtained by the alkali etching treatment of S4 in a sulfuric acid solution, keeping the temperature of the solution at 17-20 ℃, the current density at 1.5-2.0A/dm2, carrying out oxidation reaction for 8-15min, taking out after an oxide film is generated on the aluminum alloy plate for a period of time, and repeatedly washing the aluminum alloy plate for 3-4min by using pure water;
s6, sealing with boiling water: and (3) placing the aluminum alloy plate after the anodic oxidation of S5 in a sealing additive, sealing with boiling water, and taking out to obtain the treated aluminum alloy plate.
2. The method as claimed in claim 1, wherein the step S1 comprises rough polishing the surface of the aluminum alloy sheet with 150-mesh sand paper, fine polishing with 500-1500-mesh sand paper, rinsing with pure water, washing with ethanol, and drying.
3. The method of claim 1, wherein the alkaline degreasing agent in step S2 comprises 8 g/L g sodium silicate, 6 g/L g sodium carbonate, 3.175 g/L g sodium polyphosphate of 0.5 g/L g surfactant of 15 g/L g triethanolamine undecanedioate of 6 g/L.
4. The method as claimed in claim 1, wherein the alkaline etching solution in step S4 contains NaOH 60 g/L, sodium gluconate 160 g/L, sodium dodecylsulfate 3 g/L, and sorbitol 34 g/L.
5. The method of claim 1, wherein the surface of the aluminum alloy sheet is anodizedIn step S5, the bath solution for anodic oxidation includes dilute sulfuric acid and Fe2(SO4)3Wherein the concentration of the dilute sulfuric acid is 170-190 g/L, Fe2(SO4)3It was 127 g/L.
6. The method of claim 1, wherein in step S5, the aluminum alloy sheet is taken out from the sulfuric acid solution after the thickness of the aluminum alloy sheet reaches 4-8 μm.
7. The method for anodizing the surface of an aluminum alloy sheet as claimed in claim 1, wherein in said step S6, the condition of boiling water sealing is soaking at a temperature of 55-60 ℃ for 5-20 min.
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