CN114059129B - Color fixing agent for aluminum and aluminum alloy after anodic oxide film dyeing and preparation method - Google Patents
Color fixing agent for aluminum and aluminum alloy after anodic oxide film dyeing and preparation method Download PDFInfo
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/14—Producing integrally coloured layers
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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
- C25D11/243—Chemical after-treatment using organic dyestuffs
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Abstract
The invention provides a color fixing agent for aluminum and aluminum alloy after anodic oxide film dyeing and a preparation method thereof, wherein the color fixing agent comprises the following components in percentage by weight of 100 percent: 10-30% organic acid, 0.5-2% inhibitor, 1-2% accelerator, 2-5% protectant, 2-5% surfactant, 2-5% pH regulator, and the balance water. The color fixing agent does not contain fluorine and metal salt, the wastewater treatment is simple, the working temperature is 15-55 ℃, the dyed workpiece is subjected to color fixing and then subjected to high-temperature nickel-free hole sealing, and the fading degree and the hole sealing performance after hole sealing are superior to those of the mainstream high-temperature nickel-containing hole sealing in the market.
Description
Technical Field
The invention relates to the technical field of hole sealing of aluminum and aluminum alloy anodic oxide films, in particular to a color fixing agent for aluminum and aluminum alloy anodic oxide films after dyeing and a preparation method thereof.
Background
Aluminum and aluminum alloys have been used more and more widely in 3C industries, building materials, transportation, electronic and electric power, and other fields because of their advantages of wide reserves, light weight, good thermal conductivity, good ductility, and corrosion resistance. In order to improve the corrosion resistance of aluminum alloy, the industry widely adopts an anodic oxidation mode to improve the performance of the aluminum material at present, in order to meet the decorative requirement, the aluminum and the aluminum alloy need to be dyed or electrolytically colored after being anodized, the electrolytic coloring color is single, and the 3C products on the market mainly adopt anodic dyeing treatment at present.
After the anode is dyed, the aluminum and aluminum alloy workpieces need to be sealed, and the main sealing processes adopted at present are high-temperature nickel-containing sealing and high-temperature nickel-free sealing. The high-temperature nickel-containing sealing hole has excellent sealing performance, but has great harm to the environment and human body. Through development for many years, the performance of high-temperature nickel-free hole sealing is gradually improved, but the fading degree of a dyed piece after hole sealing is still obviously different from that of a nickel medium-temperature Wen Fengkong agent such as Oreodactylx 500 and the like, and particularly, the bright colors such as red, blue, green and the like are more obvious, so that color fixing treatment needs to be carried out before hole sealing.
At present, the main color fixing scheme on the market is to adopt a color fixing agent Y to fix the color of the material or adopt a cobalt salt pre-sealing scheme, wherein the color fixing agent Y contains formaldehyde, and the cobalt salt pre-sealing scheme contains heavy metal salt cobalt salt, so that the color fixing effect is not ideal. Therefore, it is necessary to develop a color fixing agent which is free of fluorine and heavy metal salt and simple in water treatment, and the color fixing agent is matched with a high-temperature nickel-free sealing agent to replace the mainstream middle and high temperature nickel-containing sealing hole in the market.
Disclosure of Invention
In view of the above, the invention provides a color fixing agent for aluminum and aluminum alloy after anodic oxide film dyeing, which is free of fluorine and heavy metal salts and has a good color fixing effect by matching with a high-temperature nickel-free sealant, and a preparation method thereof.
The technical scheme of the invention is realized as follows: the invention provides a color fixing agent for aluminum and aluminum alloy after anodic oxide film dyeing, which comprises the following components in percentage by weight of 100 percent: 10-30% organic acid, 0.5-2% inhibitor, 1-2% accelerator, 2-5% protectant, 2-5% surfactant, 2-5% pH regulator, and the balance deionized water.
Based on the above technical scheme, preferably, the inhibitor is one or more of hydroxyethylidene diphosphonic acid, amino trimethylene phosphoric acid, hydrolyzed polymaleic anhydride, acrylic acid-acrylate-sulfonate terpolymer, 2-naphthalene sulfonic acid formaldehyde condensate sodium salt and phosphono carboxylic acid copolymer.
On the basis of the above technical scheme, preferably, the organic acid is one or a combination of more of polyacrylic acid, polymethacrylic acid, tannic acid and phytic acid.
Based on the technical scheme, preferably, the polyacrylic acid is polyacrylic acid aqueous solution with the volume fraction of 40%, and the molecular weight is 2000-5000.
On the basis of the above technical scheme, preferably, the accelerator is one or a combination of more of ammonium dihydrogen phosphate, calcium dihydrogen phosphate, sodium dihydrogen pyrophosphate and sodium hexametaphosphate.
On the basis of the technical scheme, preferably, the protective agent is fatty alcohol ether phosphate which is selected from one or two of MOA-3P and MOA-9P.
On the basis of the above technical solution, preferably, the surfactant is composed of an anionic surfactant and a nonionic surfactant, and the ratio of the anionic surfactant: the mass ratio of the nonionic surfactant is 1 (1-3).
On the basis of the technical scheme, preferably, the anionic surfactant is one or a combination of more of fatty alcohol polyoxyethylene ether sodium sulfate, fatty alcohol polyoxyethylene ether ammonium sulfate, sodium dodecyl benzene sulfonate and sodium dodecyl diphenyl ether disulfonate; the nonionic surfactant is one or a combination of fatty alcohol-polyoxyethylene ether, alkylphenol ethoxylate and fatty acid-polyoxyethylene ether.
On the basis of the technical scheme, preferably, the pH regulator is one or a combination of more of polyhydroxy polyamine, ethanolamine, diethanolamine, triethanolamine, diethylamine, triethylamine and tetrahydroxy ethylenediamine.
The invention also provides a preparation method of the color fixing agent after the aluminum and aluminum alloy anodic oxide film is dyed, which comprises the steps of adding deionized water into a reaction kettle, then sequentially adding the organic acid, the discoloration inhibitor, the accelerator, the protective agent, the surfactant and the pH regulator into the reaction kettle while stirring, and after the organic acid, the discoloration inhibitor, the accelerator, the protective agent, the surfactant and the pH regulator are fully dissolved, adjusting the pH of the mixed solution to 4-5 to prepare the color fixing agent.
The invention also provides a use method of the color fixing agent for the dyed aluminum and aluminum alloy anodic oxide films, which comprises the step of immersing the dyed aluminum and aluminum alloy anodic oxide films into a color fixing agent aqueous solution with the concentration of 40-60g/L for 5-10min for color fixing, wherein the color fixing temperature is 15-55 ℃.
Compared with the prior art, the color fixing agent for dyed aluminum and aluminum alloy anodic oxide films and the preparation method thereof have the following beneficial effects:
(1) The sulfonic group or the carboxylic group in the dye molecule has stronger water solubility, is fixed on the anodic oxide film by virtue of Van der Waals force and hydrogen bond, has lower fastness and is easy to cause fading or staining phenomenon. This patent fixation component is network structure, can constitute macromolecular compound with the dyestuff, takes place the ionic bond with the anionic group in the dyestuff and combines, also can seal the water-soluble group of dyestuff simultaneously, generates the lake with the dyestuff to improve the dyestuff fastness.
(2) The components of the dye contain electrolyte, wetting agent, dust-proof agent, cosolvent and other reagents, so that a loose film layer with slight yellow light is easily formed on the surface of the aluminum material, and the sense is influenced. The inhibitor can be adsorbed on the surface of the oxide film to prevent the generation of the yellow film, so that the yellow film is inhibited and the fading is prevented. (3) The color fixing agent does not contain fluorine and metal salt, the wastewater treatment is simple, and no health threat is caused to operators; the working temperature is 15-55 ℃, the dyed workpiece is subjected to high-temperature nickel-free hole sealing after color fixation, and the fading degree and the hole sealing performance after hole sealing can be comparable to those of the mainstream high-temperature nickel-containing hole sealing process in the market.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
The color fixing agent for the aluminum and aluminum alloy after anodic oxide film dyeing comprises the following components in percentage by weight of 100 percent: 10% of an aqueous polyacrylic acid solution having a molecular weight of 2000 volume fraction of 40%, 0.5% of hydroxyethylidene diphosphonic acid, 1% of ammonium dihydrogen phosphate, 2% of MOA-3P, 1% of sodium fatty alcohol-polyoxyethylene ether sulfate, 1% of fatty alcohol-polyoxyethylene ether, 2% of polyhydroxy polyamine, and the balance of deionized water.
A preparation method of a color fixing agent after aluminum and aluminum alloy anodic oxide film dyeing comprises the steps of firstly adding deionized water into a reaction kettle according to the weight percentage, then sequentially adding a polyacrylic acid aqueous solution, hydroxyl ethylidene diphosphonic acid, ammonium dihydrogen phosphate, MOA-3P, fatty alcohol polyoxyethylene ether sodium sulfate, fatty alcohol polyoxyethylene ether and polyhydroxy polyamine into the reaction kettle while stirring, and after full dissolution, adjusting the pH value of a mixed solution to 4 to prepare the color fixing agent.
A method for using a color fixing agent after dyeing of an aluminum and aluminum alloy anodic oxide film comprises the step of immersing the dyed aluminum and aluminum alloy anodic oxide film into a color fixing agent aqueous solution with the concentration of 40g/L for 5min for color fixing, wherein the color fixing temperature is 15 ℃.
Example 2
The color fixing agent for the aluminum and aluminum alloy after anodic oxide film dyeing comprises the following components in percentage by weight of 100 percent: 30% tannic acid, 2% acrylic acid-acrylate-sulfonate terpolymer, 2% sodium dihydrogen pyrophosphate, 5% MOA-9P, 1.25% surfactant sodium dodecyl benzene sulfonate, 3.75% alkylphenol polyoxyethylene, 5% ethanolamine, and the balance deionized water.
A preparation method of a color fixing agent after dyeing of an aluminum and aluminum alloy anodic oxide film comprises the steps of adding deionized water into a reaction kettle according to the weight percentage, sequentially adding tannic acid, acrylic acid-acrylate-sulfonate terpolymer, sodium dihydrogen pyrophosphate, MOA-9P, surfactant sodium dodecyl benzene sulfonate, alkylphenol polyoxyethylene ether and ethanolamine into the reaction kettle while stirring, and after full dissolution, adjusting the pH value of a mixed solution to 5 to prepare the color fixing agent.
A method for using a color fixing agent after dyeing of an aluminum and aluminum alloy anodic oxide film comprises the step of immersing the dyed aluminum and aluminum alloy anodic oxide film into a color fixing agent aqueous solution with the concentration of 60g/L for 10min for color fixing, wherein the color fixing temperature is 55 ℃.
Example 3
The color fixing agent for the dyed aluminum and aluminum alloy anode oxide film comprises the following components in percentage by weight of 100 percent: 10% polyacrylic acid aqueous solution with the molecular weight of 5000 volume percent of 40%, 5% phytic acid, 0.5% amino trimethylene phosphoric acid, 0.5% hydrolyzed polymaleic anhydride, 1% monocalcium phosphate, 0.5% sodium hexametaphosphate, 1% MOA-3P, 2% MOA-9P, 0.5% fatty alcohol polyoxyethylene ether sulfur, 0.5% sodium dodecyl diphenyl ether disulfonate, 2% fatty acid polyoxyethylene ether, 1% diethylamine, 2% tetrahydroxyethylenediamine and the balance of deionized water.
A preparation method of a color fixing agent after aluminum and aluminum alloy anodic oxide film dyeing comprises the steps of adding deionized water into a reaction kettle according to the weight percentage, then sequentially adding polyacrylic acid aqueous solution, phytic acid, amino trimethylene phosphoric acid, hydrolyzed polymaleic anhydride, monocalcium phosphate, sodium hexametaphosphate, MOA-3P, MOA-9P, fatty alcohol polyoxyethylene ether sulfur, sodium dodecyl diphenyl ether disulfonate, fatty acid polyoxyethylene ether, diethylamine and tetrahydroxy ethylenediamine into the reaction kettle while stirring, and after full dissolution, adjusting the pH of a mixed solution to 4.5 to prepare the color fixing agent.
A method for using a color fixing agent after dyeing of an aluminum and aluminum alloy anodic oxide film comprises the step of immersing the dyed aluminum and aluminum alloy anodic oxide film into a color fixing agent aqueous solution with the concentration of 45g/L for 6min for color fixing, wherein the color fixing temperature is 25 ℃.
Example 4
The color fixing agent for the aluminum and aluminum alloy after anodic oxide film dyeing comprises the following components in percentage by weight of 100 percent: 10% tannic acid, 10% phytic acid, 0.5% sodium salt of a 2-naphthalenesulfonic acid formaldehyde condensate, 1% phosphonocarboxylic acid copolymer, 1.5% ammonium dihydrogen phosphate, 4% MOA-3P, 2% sodium fatty alcohol polyoxyethylene ether sulfate, 2% alkylphenol polyoxyethylene ether, 1% polyhydroxy polyamine, 4% ethanolamine, and the balance deionized water.
A preparation method of a color fixing agent after aluminum and aluminum alloy anodic oxide film dyeing comprises the steps of adding deionized water into a reaction kettle according to the weight percentage, then sequentially adding tannic acid, phytic acid, 2-naphthalene sulfonic acid formaldehyde condensation product sodium salt, phosphono carboxylic acid copolymer, ammonium dihydrogen phosphate, MOA-3P, fatty alcohol-polyoxyethylene ether sodium sulfate, alkylphenol ethoxylates, polyhydroxy polyamine and ethanolamine into the reaction kettle, stirring while adding, and after full dissolution, adjusting the pH value of a mixed solution to 4 to prepare the color fixing agent.
A use method of a color fixing agent after dyeing of aluminum and aluminum alloy anodic oxide films comprises the steps of immersing the dyed aluminum and aluminum alloy anodic oxide films into a color fixing agent aqueous solution with the concentration of 50g/L for 7min for color fixing, wherein the color fixing temperature is 30 ℃.
Example 5
The color fixing agent for the dyed aluminum and aluminum alloy anode oxide film comprises the following components in percentage by weight of 100 percent: 15% polyacrylic acid aqueous solution with molecular weight of 3000 volume percent being 40%, 10% tannic acid, 1% hydroxyethylidene diphosphonic acid, 0.6% acrylic acid-acrylate-sulfonate terpolymer, 1% calcium dihydrogen phosphate, 1% sodium hexametaphosphate, 5% MOA-9P, 1% fatty alcohol polyoxyethylene ether ammonium sulfate, 3% fatty acid polyoxyethylene ether, 5% tetrahydroxyethylenediamine and the balance being deionized water.
A preparation method of a color fixing agent after aluminum and aluminum alloy anodic oxide film dyeing comprises the steps of adding deionized water into a reaction kettle according to the weight percentage, sequentially adding polyacrylic acid aqueous solution, tannic acid, hydroxyethylidene diphosphonic acid, acrylic acid-acrylate-sulfonate terpolymer, calcium dihydrogen phosphate, sodium hexametaphosphate, MOA-9P, fatty alcohol polyoxyethylene ether ammonium sulfate, fatty acid polyoxyethylene ether and tetrahydroxy ethylenediamine into the reaction kettle, stirring while adding, and after full dissolution, adjusting the pH value of a mixed solution to 5 to prepare the color fixing agent.
A method for using a color fixing agent after dyeing of an aluminum and aluminum alloy anodic oxide film comprises the step of immersing the dyed aluminum and aluminum alloy anodic oxide film into a color fixing agent aqueous solution with the concentration of 55g/L for 8min for color fixing, wherein the color fixing temperature is 40 ℃.
Examples 1-5 color fixing agent and high temperature nickel-free sealer formulation:
s1, placing an anodized aluminum or aluminum alloy workpiece in oxidizing solution such as concentrated sulfuric acid after oil removal, water washing, alkali etching, water washing, chemical polishing, water washing, ash removal and water washing, electrifying to carry out anodic oxidation, and washing to obtain a workpiece with an anodic oxide film on the surface;
s2, dyeing: the above-mentioned work piece having the anodic oxide film is dipped in organic dyes or inorganic dyes of different colors for dyeing, the dyeing colors being black (L: 30.4a: -0.20b: -0.58), blue L:43.50a: -12.15b: -45.82), red (L: 51.1a.
S3, color fixation: and immersing the dyed aluminum and aluminum alloy anodic oxide films into a color fixing agent aqueous solution with the concentration of 40-60g/L for 5-10min for color fixing, wherein the color fixing temperature is 15-55 ℃.
S4, hole sealing: high temperature nickel-free sealant Phoenix Seal 130, concentration: the 10g/L time is 20min, and the hole sealing temperature is 95 ℃.
Comparative example 1 process:
the method takes the direct sealing of the high-temperature nickel-free sealing agent as a comparative example 1 without using a color fixing agent after the aluminum and aluminum alloy anodic oxide film is dyed.
S1, subjecting an anodized aluminum or aluminum alloy workpiece to oil removal, water washing, alkaline etching, water washing, chemical polishing, water washing, ash removal and water washing, then placing the workpiece in oxidizing solutions such as concentrated sulfuric acid and the like, electrifying for anodizing, and washing to obtain a workpiece with an anodized film on the surface;
s2, dyeing: the workpiece with the anodic oxide film is dipped in organic dyes or inorganic dyes with different colors for dyeing, wherein the dyeing colors are black (L: 30.4a: -0.20b: -0.58), blue L:43.50a: -12.15b: -45.82), red (L: 51.1a.
S3, hole sealing: high temperature nickel-free sealant Phoenix Seal 130, concentration: the 10g/L time is 20min, and the hole sealing temperature is 95 ℃.
Comparative example 2 process:
the color fixing agent is not used after the aluminum and aluminum alloy anodic oxide film is dyed, and the high-temperature nickel-containing sealant hole sealing is adopted as the comparative example 2.
S1, placing an anodized aluminum or aluminum alloy workpiece in oxidizing solution such as concentrated sulfuric acid after oil removal, water washing, alkali etching, water washing, chemical polishing, water washing, ash removal and water washing, electrifying to carry out anodic oxidation, and washing to obtain a workpiece with an anodic oxide film on the surface;
s2, dyeing: the workpiece with the anodic oxide film is dipped in organic dyes or inorganic dyes with different colors for dyeing, wherein the dyeing colors are black (L: 30.4a: -0.20b: -0.58), blue L:43.50a: -12.15b: -45.82), red (L: 51.1a.
S3, hole sealing: high-temperature nickel-containing sealant: japanese DX500, concentration: the time of 10g/L is 20min, and the hole sealing temperature is 94 ℃.
Comparative example 3
Example 1 without inhibitor was used as the fixing agent of comparative example 3, and the use process was as follows: after the aluminum and aluminum alloy anodic oxide films are dyed, the color fixing agent of the comparative example 3 is adopted for color fixing, and the hole sealing is carried out by adopting a high-temperature nickel-free hole sealing agent.
TABLE 1 comparison of color change before and after plugging
As can be seen from the results in Table 1, in examples 1 to 5, the color difference Delta E after sealing is obviously reduced compared with comparative example 1 and comparative example 3, which shows that the inhibitor pair can prevent discoloration and achieve the effect of inhibiting yellow films. Examples 1-5, the color difference Δ E was not significantly different relative to comparative example 2. The result shows that the color fixing agent can make up the defect of nickel-free high-temperature sealing in dyeing sealing hole fading property, and has obvious promotion effect on sealing hole color fixing.
The weight loss test of the phosphorus chromic acid refers to the evaluation method of the quality of the anodic oxidation hole sealing of GB/T8753.1-2005 aluminum and aluminum alloy.
TABLE 2 weight loss of phosphorus chromic acid test results
The weightlessness test data will become smaller after aging, and the weightlessness test is arranged to measure the data on the same day after hole sealing. As can be seen from the results in Table 2, the weight loss data for the phosphochromic acids for examples 1-5 are significantly reduced relative to comparative example 1. Examples 1-5, the weight loss data was close to or even slightly superior to comparative example 2. Compared with comparative example 3, the inhibitor in the color fixing agent of the invention has obvious effect of reducing the weight loss of phosphorus chromic acid. The color fixing agent has a certain pre-sealing effect, is combined with a nickel-free high-temperature sealing agent, has excellent color fixing and phosphorus chromic acid weight loss reducing effects, and can be replaced for nickel-containing high-temperature sealing.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (4)
1. The color fixing agent for dyed aluminum and aluminum alloy anode oxide films is characterized in that: calculated according to the weight percentage of 100 percent, comprises the following components: 10-30% organic acid, 0.5-2% inhibitor, 1-2% accelerator, 2-5% protectant, 2-5% surfactant, 2-5% pH regulator, and the balance deionized water;
the workpiece dyed by the aluminum and aluminum alloy anodic oxide film is subjected to color fixation by the color fixing agent and then subjected to high-temperature nickel-free hole sealing;
the organic acid is one or a combination of more of polyacrylic acid, polymethacrylic acid, tannic acid and phytic acid;
the inhibitor is one or more of hydroxyethylidene diphosphonic acid, amino trimethylene phosphoric acid, hydrolyzed polymaleic anhydride, acrylic acid-acrylate-sulfonate terpolymer, 2-naphthalene sulfonic acid formaldehyde condensate sodium salt and phosphono carboxylic acid copolymer;
the accelerator is one or more of ammonium dihydrogen phosphate, calcium dihydrogen phosphate, sodium dihydrogen pyrophosphate and sodium hexametaphosphate;
the protective agent is fatty alcohol ether phosphate selected from one or two of MOA-3P and MOA-9P;
the surfactant is composed of an anionic surfactant and a nonionic surfactant, wherein the ratio of the anionic surfactant: the mass ratio of the nonionic surfactant is 1 (1-3); the anionic surfactant is one or a combination of more of fatty alcohol-polyoxyethylene ether sodium sulfate, fatty alcohol-polyoxyethylene ether ammonium sulfate, sodium dodecyl benzene sulfonate and sodium dodecyl diphenyl ether disulfonate; the nonionic surfactant is one or a combination of more of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether and fatty acid polyoxyethylene ether;
the pH regulator is one or a combination of more of polyhydroxy polyamine, ethanolamine, diethanolamine, triethanolamine, diethylamine, triethylamine and tetrahydroxy ethylenediamine.
2. The color fixing agent for aluminum and aluminum alloy anodic oxide film after dyeing according to claim 1, wherein: the polyacrylic acid is polyacrylic acid aqueous solution with the volume fraction of 40%, and the molecular weight is 2000-5000.
3. The method for preparing the color fixing agent used after the anodic oxide film of aluminum and aluminum alloy is dyed according to any one of claims 1-2, which is characterized in that: adding deionized water into a reaction kettle, then sequentially adding an organic acid, an inhibitor, an accelerator, a protective agent, a surfactant and a pH regulator into the reaction kettle, stirring while adding, and after the organic acid, the inhibitor, the accelerator, the protective agent, the surfactant and the pH regulator are fully dissolved, adjusting the pH of the mixed solution to 4-5 to prepare the color fixing agent.
4. The use method of the color fixing agent for aluminum and aluminum alloy after anodic oxide film dyeing according to any one of claims 1-2, characterized by comprising the following steps: and immersing the dyed aluminum and aluminum alloy anodic oxide films into a color fixing agent aqueous solution with the concentration of 40-60g/L for 5-10min for color fixing, wherein the color fixing temperature is 15-55 ℃.
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