CN110656366A - Anodic oxidation method of aluminum alloy - Google Patents
Anodic oxidation method of aluminum alloy Download PDFInfo
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- CN110656366A CN110656366A CN201810712029.0A CN201810712029A CN110656366A CN 110656366 A CN110656366 A CN 110656366A CN 201810712029 A CN201810712029 A CN 201810712029A CN 110656366 A CN110656366 A CN 110656366A
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- aluminum alloy
- treatment
- anodic oxidation
- anodizing
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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
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
-
- 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
-
- 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
-
- 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 provides an anodic oxidation method of an aluminum alloy, which comprises the following steps: providing an aluminum alloy piece; carrying out anodic oxidation treatment on the aluminum alloy piece to form an anodic oxidation film on the surface of the aluminum alloy piece, wherein electrolyte used for the anodic oxidation treatment comprises sulfuric acid and oxalic acid, the mass concentration of the sulfuric acid is 50-70 g/L, and the mass concentration of the oxalic acid is 15-25 g/L; and contacting the aluminum alloy piece with a nitric acid solution with the mass concentration of 5-200 g/L to perform acid treatment on the aluminum alloy piece, wherein the temperature of the acid treatment is 0-40 ℃, and the time is 30-120 seconds. The nitric acid solution is capable of dissolving a portion of the anodized film to reduce the yellowness of the anodized film.
Description
Technical Field
The invention relates to the field of anodic oxidation, in particular to an anodic oxidation method of aluminum alloy.
Background
Aluminum alloys have advantages of low specific gravity, good machinability, high strength ratio, etc., and are increasingly used in the field of electronic products such as mobile phone housings, computer housings, frames, etc. in recent years. Due to the low chemical stability and poor corrosion resistance of aluminum alloys, it is often necessary to surface treat the aluminum alloy products appropriately. At present, a common aluminum alloy surface treatment method is anodic oxidation, and the treated aluminum alloy has certain wear resistance and corrosion resistance.
The 7-series aluminum alloy (aluminum alloy mainly doped with zinc) has higher hardness and strength than the more commonly used 6-series aluminum alloy (aluminum alloy mainly doped with magnesium and silicon). As materials for electronic product housings and middle frames, 7-series aluminum alloys have advantages of light weight and less bending and deformation, and are favored by more and more electronic product manufacturers. However, the electronic product has a high requirement for color difference management and control, and the color difference of the anodic oxide film obtained by the existing anodic oxidation method is large, so that the requirement of the product on the color difference is difficult to meet.
Disclosure of Invention
In view of the above situation, it is necessary to provide a method for anodizing an aluminum alloy that can satisfy the requirement of color difference to solve the above problems.
A method of anodizing an aluminum alloy comprising the steps of: providing an aluminum alloy piece; carrying out anodic oxidation treatment on the aluminum alloy piece to form an anodic oxidation film on the surface of the aluminum alloy piece, wherein electrolyte used for the anodic oxidation treatment comprises sulfuric acid and oxalic acid, the mass concentration of the sulfuric acid is 50-70 g/L, and the mass concentration of the oxalic acid is 15-25 g/L; and contacting the aluminum alloy piece with a nitric acid solution with the mass concentration of 5-200 g/L to perform acid treatment on the aluminum alloy piece, wherein the temperature of the acid treatment is 0-40 ℃, and the time is 30-120 seconds.
The aluminum alloy anodizing method comprises the steps of anodizing and acid treatment, wherein the aluminum alloy is subjected to acid treatment by using a nitric acid solution, and a part of an anodized film can be dissolved, so that yellowish aluminum oxalate in the anodized film is dissolved, the color difference value Db of the anodized film is effectively reduced, the yellowness of the anodized film is reduced, and the anodized film meets the color difference control requirement.
Drawings
FIG. 1 is a flow chart of a method for anodizing an aluminum alloy according to an embodiment of the present invention.
FIG. 2 is a statistical chart of the color difference value Db of the aluminum alloy pieces of examples 1-3 and comparative examples 1-3.
Detailed Description
So that the manner in which the above recited objects, features and advantages of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings. In addition, the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth to provide a thorough understanding of the present invention, and the described embodiments are merely a subset of the embodiments of the present invention, rather than a complete embodiment. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an anodizing method of an aluminum alloy according to an embodiment of the present invention includes:
step S101, an aluminum alloy part is provided.
Preferably, the aluminum alloy member is a 7-series aluminum alloy.
And S102, performing pre-anode pretreatment on the aluminum alloy part to remove defects, oil stains or natural oxidation films on the surface of the aluminum alloy part.
It is understood that the pre-anodic pretreatment includes one or more of degreasing, alkali-biting, chemical polishing, and desmutting.
The degreasing can remove pollutants such as grease and dust on the surface of the aluminum alloy piece, so that the surface of the aluminum alloy piece is hydrophilic. The degreasing solution is sodium phosphate with a mass concentration of 40 to 70 grams per liter (g/L). The degreasing temperature is 50-60 ℃, and the time is 3-5 minutes.
The alkali bite can further remove pollutants on the surface of the aluminum alloy piece and remove a natural oxide film on the surface of the aluminum alloy piece. The alkali-biting solution is sodium hydroxide with the mass concentration of 30-60 g/L. The temperature of alkali biting is 50-55 ℃, and the time is 20-60 seconds.
Chemical polishing is used to obtain a smooth, high-brightness surface of the aluminum alloy part. The chemical polishing solution is phosphoric acid, and the mass concentration of the chemical polishing solution is 1000-1200 g/L. The temperature of the chemical polishing is 75-80 ℃, and the time is 20-60 seconds.
The desmutting removes the surface layer of intermetallic particles from the surface of the aluminum alloy part after chemical polishing, thereby obtaining a bright surface. The stripping solution is sulfuric acid, and the volume ratio of the stripping solution is 15-35%. The black stripping temperature is room temperature, and the time is 20-120 seconds.
It is understood that other chemical solutions may be used for degreasing, alkaline biting, chemical polishing, or desmearing processes, respectively. In addition, according to actual needs, pretreatment before anode such as mechanical polishing or sand blasting can be added, so that the aluminum alloy part presents different surface effects.
It is understood that degreasing, alkaline biting, chemical polishing, or desmearing may be followed by a water washing step.
Step S103, carrying out anodic oxidation treatment on the aluminum alloy piece to form an anodic oxidation film on the surface of the aluminum alloy piece.
During anodic oxidation treatment, the aluminum alloy part with a clean surface is placed into electrolyte, voltage is applied, the aluminum alloy part is used as an anode and is connected to an external connectorAnd anodizing the positive electrode of the current source to form a porous anodic oxide film on the surface of the aluminum alloy piece. The main component of the anodic oxide film is aluminum oxide (Al)2O3) The anodic oxide film is also doped with a small amount of aluminum oxalate (Al)2(C2O4)3). The anodized film was approximately silvery white, but was slightly yellowish in color due to the inclusion of aluminum oxalate in the anodized film.
In the embodiment, the electrolyte comprises sulfuric acid and oxalic acid, wherein the mass concentration of the sulfuric acid is 50-70 g/L, and the mass concentration of the oxalic acid is 15-25 g/L. The voltage of the anodic oxidation treatment is 14-16V, the time of the anodic oxidation is 35-50 minutes, and the temperature is 20-40 ℃. The thickness of the anodic oxide film is 10-14 micrometers (um).
It is understood that after the formation of the anodic oxide film, the aluminum alloy member may be subjected to ultrasonic water washing in clean water at room temperature to remove the electrolyte remaining in the aluminum alloy member.
And step S104, performing acid treatment on the aluminum alloy piece.
Contacting an aluminum alloy part with a nitric acid solution to perform acid treatment on the aluminum alloy part, thereby reducing the yellowness of the anodic oxide film. The nitric acid solution may be contacted with the aluminum alloy part by immersing the aluminum alloy part in the nitric acid solution, or by spraying the nitric acid solution onto the surface of the aluminum alloy part. Specifically, the aluminum alloy piece is subjected to acid treatment by using a nitric acid solution with the mass concentration of 5-200 g/L. The temperature of the acid treatment is 0-40 ℃, and the time is 30-120 seconds.
The reaction equation in the acid treatment is as follows:
Al2(C2O4)3+6HNO3＝2HAlO2+6NO2+6CO2+2H2O
Al2O3+6HNO3＝2Al(NO3)3+3H2O
therefore, the acid treatment can dissolve part of the anodic oxide film on the surface of the aluminum alloy piece, thereby reducing the yellowness of the anodic oxide film, improving the problem of partial yellowness of the anodic oxide film and reducing the color difference of the anodic oxide film.
And S105, sealing the holes of the aluminum alloy piece.
And sealing the hole of the anodized aluminum alloy part to improve the corrosion resistance of the anodic oxide film. The hole sealing time is 15-40 minutes, the hole sealing temperature is 90-95 ℃, and the hole sealing liquid is nickel acetate solution with the mass concentration of 5-10 g/L. And drying the aluminum alloy piece after hole sealing.
It is understood that in other embodiments, step S102 may be eliminated when the surface of the aluminum alloy member is relatively clean.
It is understood that in other embodiments, step S105 may be eliminated when the wear resistance requirement of the aluminum alloy part is not high.
It is understood that, in other embodiments, when the aluminum alloy member needs to be colored, between step S104 and step S105, the anodizing method further includes the step of immersing the aluminum alloy member in a coloring agent for a coloring treatment. The dyeing process may be a conventional dyeing method, and is not described herein again.
To further explain the above-described anodizing method of an aluminum alloy, specific examples and comparative examples will be described below.
Example 1
S1, providing an aluminum alloy part.
The aluminum alloy piece is made of 7 series aluminum alloy.
S2: pretreatment before anode.
The method comprises the following steps of degreasing the aluminum alloy piece by using a 40g/L sodium phosphate solution, carrying out alkali biting on the aluminum alloy piece by using a 30g/L sodium hydroxide solution, carrying out chemical polishing on the aluminum alloy piece by using a 1000g/L phosphoric acid solution, and stripping a black film on the aluminum alloy piece by using a 15% sulfuric acid solution in volume ratio.
S3: and (4) anodizing.
The electrolyte comprises sulfuric acid and oxalic acid, wherein the mass concentration of the sulfuric acid is 50g/L, and the mass concentration of the oxalic acid is 15 g/L. The voltage of the anodic oxidation treatment was 16V, the time was 35 minutes, and the temperature was 40 ℃.
S4: and (4) acid treatment.
And (3) carrying out acid treatment on the aluminum alloy piece by using a nitric acid solution with the mass concentration of 5g/L, wherein the temperature of the acid treatment is 0 ℃ and the time is 120 seconds.
S5: and (6) sealing the holes.
And sealing the hole of the aluminum alloy part by using a nickel acetate solution with the mass concentration of 8g/L, and drying.
Example 2
S1, providing an aluminum alloy part.
The aluminum alloy piece is made of 7 series aluminum alloy.
S2: pretreatment before anode.
Degreasing the aluminum alloy part by using 70g/L sodium phosphate solution, alkali biting the aluminum alloy part by using 60g/L sodium hydroxide solution, and stripping a black film of the aluminum alloy part by using 35% sulfuric acid solution in volume ratio.
S3: and (4) anodizing.
The electrolyte comprises sulfuric acid and oxalic acid, wherein the mass concentration of the sulfuric acid is 60g/L, and the mass concentration of the oxalic acid is 20 g/L. The voltage of the anodic oxidation treatment was 15V, the time was 40 minutes, and the temperature was 30 ℃.
S4: and (4) acid treatment.
And (3) carrying out acid treatment on the aluminum alloy piece by using a nitric acid solution with the mass concentration of 60g/L, wherein the temperature of the acid treatment is 20 ℃, and the time is 90 seconds.
S5: and (6) sealing the holes.
And sealing the hole of the aluminum alloy part by using a nickel acetate solution with the mass concentration of 8g/L, and drying.
Example 3
S1, providing an aluminum alloy part.
The material of the aluminum alloy member is 7 series aluminum alloy.
S2: pretreatment before anode.
The aluminum alloy part is degreased by using 50g/L sodium phosphate solution, and is subjected to black film stripping by using 20% sulfuric acid solution in volume ratio.
S3: and (4) anodizing.
The electrolyte comprises sulfuric acid and oxalic acid, wherein the mass concentration of the sulfuric acid is 70g/L, and the mass concentration of the oxalic acid is 25 g/L. The anodic oxidation treatment was carried out at a voltage of 14V for 50 minutes and at a temperature of 20 ℃.
S4: and (4) acid treatment.
And (3) carrying out acid treatment on the aluminum alloy piece by using a nitric acid solution with the mass concentration of 200g/L, wherein the temperature of the acid treatment is 40 ℃, and the time is 30 seconds.
S5: and (6) sealing the holes.
And sealing the hole of the aluminum alloy part by using a nickel acetate solution with the mass concentration of 10g/L, and drying.
Comparative example 1
Comparative example 1 is the same as example 1 in terms of the composition and concentration of the solution for the pretreatment for anode and the anodic oxidation treatment, except that comparative example 1 does not include the step of acid treatment.
Comparative example 2
Comparative example 2 the composition and concentration of the solution for the pretreatment for anode and the anodic oxidation treatment in example 2 were the same, except that comparative example 2 did not include the step of acid treatment.
Comparative example 3
Comparative example 3 the same components and concentrations as those of the solutions of the anodic pretreatment and the anodic oxidation treatment of example 3 were used, except that comparative example 3 did not include the step of acid treatment.
Samples of 25 aluminum alloy pieces were randomly sampled from the 3 sets of aluminum alloy pieces of examples 1 to 3, and samples of 25 aluminum alloy pieces were randomly sampled from the 3 sets of aluminum alloy pieces of comparative examples 1 to 3, and then the color difference value Db (the yellow-blue color difference is reflected in the LAB color model) of all the aluminum alloy piece samples, which can be measured and displayed by a color difference meter, was measured and displayed, the color difference value Db reflecting the yellowness of the anodic oxide film on the aluminum alloy pieces. FIG. 2 is a statistical schematic diagram of the color difference value Db of the aluminum alloy sample, and it can be seen from FIG. 2 that the aluminum alloy samples of examples 1-3 are treated by the anodic oxidation method provided by the present invention, the color difference value Db of the aluminum alloy samples is between-0.4 and 0.4, while the aluminum alloy samples of comparative examples 1-3 are not treated by acid, and the color difference value Db of the aluminum alloy samples is between 0.3 and 0.8. Therefore, the anodic oxidation method of the aluminum alloy effectively reduces the color difference value Db of the anodic oxide film and improves the problem of yellow aluminum alloy.
The aluminum alloy anodizing method comprises the steps of anodizing and acid treatment, wherein the aluminum alloy is subjected to acid treatment by using a nitric acid solution, and a part of an anodized film can be dissolved, so that yellowish aluminum oxalate in the anodized film is dissolved, the color difference value Db of the anodized film is effectively reduced, the yellowness of the anodized film is reduced, and the anodized film meets the color difference control requirement.
Finally, it should be noted that the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method of anodizing an aluminum alloy comprising the steps of:
providing an aluminum alloy piece;
carrying out anodic oxidation treatment on the aluminum alloy piece to form an anodic oxidation film on the surface of the aluminum alloy piece, wherein electrolyte used for the anodic oxidation treatment comprises sulfuric acid and oxalic acid, the mass concentration of the sulfuric acid is 50-70 g/L, and the mass concentration of the oxalic acid is 15-25 g/L; and
and contacting the aluminum alloy piece with a nitric acid solution with the mass concentration of 5-200 g/L to perform acid treatment on the aluminum alloy piece, wherein the temperature of the acid treatment is 0-40 ℃, and the time is 30-120 seconds.
2. The method for anodizing an aluminum alloy according to claim 1, wherein: the anodic oxide film comprises aluminum oxide and aluminum oxalate.
3. The method for anodizing an aluminum alloy according to claim 2, wherein: the nitric acid solution is used to dissolve a portion of the anodized film during the acid treatment.
4. The method for anodizing an aluminum alloy according to claim 1, wherein: the aluminum alloy piece is contacted with the nitric acid solution in a mode that the aluminum alloy piece is immersed in the nitric acid solution, or the nitric acid solution is sprayed on the surface of the aluminum alloy piece.
5. The method for anodizing an aluminum alloy according to claim 1, wherein: the voltage of the anodic oxidation treatment is 14-16V, the time of the anodic oxidation is 35-50 minutes, and the temperature is 20-40 ℃.
6. The method for anodizing an aluminum alloy according to claim 1, wherein: the thickness of the anodic oxide film is 10-14 microns.
7. The method for anodizing an aluminum alloy according to claim 1, wherein: before the aluminum alloy piece is subjected to anodic oxidation treatment, the anodic oxidation method further comprises the step of pretreatment before the anode, wherein the pretreatment before the anode comprises one or more of degreasing, alkali biting, chemical polishing and black film stripping treatment.
8. The method for anodizing an aluminum alloy according to claim 1, wherein: after the aluminum alloy piece is subjected to acid treatment, the anodic oxidation method further comprises a hole sealing treatment step, wherein the hole sealing treatment time is 15-40 minutes, the temperature is 90-95 ℃, and the hole sealing liquid is a nickel acetate solution with the mass concentration of 5-10 g/L.
9. The method for anodizing an aluminum alloy according to claim 7, wherein: the anodic oxidation method further comprises a step of immersing the aluminum alloy member in a coloring agent for dyeing treatment between the steps of performing acid treatment and hole sealing treatment on the aluminum alloy member.
10. The method for anodizing an aluminum alloy according to claim 1, wherein: the aluminum alloy piece is made of 7 series aluminum alloy.
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| CN201810712029.0A CN110656366A (en) | 2018-06-29 | 2018-06-29 | Anodic oxidation method of aluminum alloy |
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| CN201810712029.0A CN110656366A (en) | 2018-06-29 | 2018-06-29 | Anodic oxidation method of aluminum alloy |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51138545A (en) * | 1975-05-27 | 1976-11-30 | Fuji Satsushi Kogyo Kk | Process for painting aluminum or aluminum alloy |
| JPS57140894A (en) * | 1981-02-23 | 1982-08-31 | Pilot Pen Co Ltd:The | Dip coloring method for aluminum alloy |
| JPS58157993A (en) * | 1982-03-12 | 1983-09-20 | Tateyama Alum Kogyo Kk | Method for coloring aluminum or aluminum alloy |
| JPH09165687A (en) * | 1995-12-12 | 1997-06-24 | Ykk Corp | Water-repellent aluminum material and its production |
| EP1867757A2 (en) * | 2006-06-16 | 2007-12-19 | FUJIFILM Corporation | Microstructure and method of manufacturing the same |
| CN104685110A (en) * | 2012-09-24 | 2015-06-03 | 美铝公司 | Anodized aluminum alloy products having improved appearance and/or abrasion resistance, and methods of making the same |
| CN108441918A (en) * | 2018-04-25 | 2018-08-24 | 合肥市旺友门窗有限公司 | A kind of aluminum alloy surface treatment process |
-
2018
- 2018-06-29 CN CN201810712029.0A patent/CN110656366A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS51138545A (en) * | 1975-05-27 | 1976-11-30 | Fuji Satsushi Kogyo Kk | Process for painting aluminum or aluminum alloy |
| JPS57140894A (en) * | 1981-02-23 | 1982-08-31 | Pilot Pen Co Ltd:The | Dip coloring method for aluminum alloy |
| JPS58157993A (en) * | 1982-03-12 | 1983-09-20 | Tateyama Alum Kogyo Kk | Method for coloring aluminum or aluminum alloy |
| JPH09165687A (en) * | 1995-12-12 | 1997-06-24 | Ykk Corp | Water-repellent aluminum material and its production |
| EP1867757A2 (en) * | 2006-06-16 | 2007-12-19 | FUJIFILM Corporation | Microstructure and method of manufacturing the same |
| CN104685110A (en) * | 2012-09-24 | 2015-06-03 | 美铝公司 | Anodized aluminum alloy products having improved appearance and/or abrasion resistance, and methods of making the same |
| CN108441918A (en) * | 2018-04-25 | 2018-08-24 | 合肥市旺友门窗有限公司 | A kind of aluminum alloy surface treatment process |
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