CN112210808A - Preparation method of black film - Google Patents
Preparation method of black film Download PDFInfo
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- CN112210808A CN112210808A CN202011054995.1A CN202011054995A CN112210808A CN 112210808 A CN112210808 A CN 112210808A CN 202011054995 A CN202011054995 A CN 202011054995A CN 112210808 A CN112210808 A CN 112210808A
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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
- 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
- C23F3/00—Brightening metals by chemical means
- C23F3/02—Light metals
- C23F3/03—Light metals with acidic solutions
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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
- 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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- 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
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- Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a preparation method of a black film, which comprises the steps of carrying out periodic and repeated mechanical polishing and chemical polishing on an aluminum alloy workpiece, anodizing, dyeing by using a black dye solution containing 50-80g/L of acidic hair dye ATT, 5-8g/L of acidic lake blue and 8-20g/L of carbon-containing additive, sealing and washing. The black film obtained by the method disclosed by the invention through the process of combining the mechanical polishing, the chemical polishing and the carbon-containing black dye solution which are periodically repeated has high glossiness and hardness, has excellent black appearance and wear resistance, and is suitable for application.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a preparation method of a black film.
Background
With the popularity of black industrial wind worldwide, none of them is subjected to black decoration, as small as bolts, as large as home electric products, automobiles, etc. In the household industry, black aluminum alloy products are also visible everywhere, such as black aluminum alloy shower room frames, black aluminum alloy towel racks and the like. For example, patent CN108707942A discloses a process for black anodic oxidation electrophoresis of aluminum alloy, wherein the process comprises the steps of anodizing the aluminum alloy, adding black electrolytic coloring, and then performing electrophoresis to obtain an anodized appearance with smooth, smooth and impact-resistant capability, and can meet the test requirements of high alkali resistance, long-period salt spray and condensed water.
However, most of the existing aluminum alloy products are oxidized into black films or sprayed with black paint and black powder, and the problems of poor glossiness (such as black oxide, and the glossiness is less than 50), low hardness (such as pencil hardness of 2H) and the like exist on the surfaces of samples.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of a black film with high glossiness and high hardness.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the preparation method of the black film comprises the following steps:
1) polishing of
Performing periodic repeated mechanical polishing and chemical polishing on the surface of the aluminum alloy workpiece, wherein the mechanical polishing is multi-step polishing with increased rotating speed and polishing time gradient, the chemical polishing is to put the aluminum alloy workpiece after the mechanical polishing into polishing solution containing 10-20 wt% of sulfuric acid, 65-70 wt% of phosphoric acid and 1-5 wt% of additives for chemical polishing, the temperature is 80-100 ℃, and the polishing time is 10-30 min;
2) anodic oxidation
Putting the polished aluminum alloy workpiece into an anodic oxidation solution for oxidation, wherein the voltage is 10-20V, and the current is 1.0-3.0A/dm2The temperature is 15-20 ℃, and the oxidation time is 10-30 min;
3) dyeing process
Placing the anodized aluminum alloy workpiece into a black dye solution for dyeing at the temperature of 35-45 ℃ and the pH value of 3-5 for 15-30 min; the black dye solution contains 50-80g/L of acidic hair dye ATT, 5-8g/L of acidic lake blue and 8-20g/L of carbon-containing additive; after dyeing, putting the workpiece into pure water for cleaning for 5-20 min;
4) sealing of
Placing the dyed aluminum alloy workpiece into a hole sealing agent solution for hole sealing treatment at the temperature of 75-85 ℃ for 40-80 min;
5) washing with water
Cleaning the aluminum alloy workpiece after hole sealing with normal-temperature ultrapure water for 10-20 min; then cleaning with ultrapure water of 60-90 ℃ for 10-30 min.
Optionally, the multi-step polishing comprises at least two steps, and the rotation speed of each step is increased by 500-1500r/min and the polishing time is increased by 3-8 min.
Optionally, the multi-step polishing is a three-step polishing; the rotation speed of the first step of polishing is 500-; the rotation speed of the second step of polishing is 1500-; the rotation speed of the third step of polishing is 2500-.
Optionally, the chemical polishing additive includes at least one of nickel sulfate, polydithio-dipropyl sulfonate, thio-benzimidazole, ethylene thiourea, sulfamic acid and wetting agent.
Optionally, the polishing cycle is 2-5.
Optionally, the step of degreasing, alkali washing and neutralizing the aluminum alloy workpiece is further included between the mechanical polishing and the chemical polishing.
Optionally, the aluminum alloy workpiece after mechanical polishing is placed into a 5-10% sulfuric acid solution for degreasing treatment, and is taken out after 5-15min and is placed into pure water for cleaning for 5-20 min; then, putting the aluminum alloy workpiece into a NaOH solution with the concentration of 45-55g/L for alkali washing, wherein the solution temperature is 45-55 ℃, the alkali washing time is 2-5min, and after the alkali washing, putting the aluminum alloy workpiece into pure water for washing for 5-20 min; and (3) putting the aluminum alloy workpiece subjected to alkali washing into a nitric acid solution with the concentration of 140-150g/L for neutralization treatment, and then putting the aluminum alloy workpiece into pure water for washing for 5-20 min.
Optionally, the anodizing solution contains 5-10g/L of Al3+And 15-25 wt% H2SO4。
Optionally, the carbon-containing additive is granular carbon powder with the particle size of 10-100 μm.
Optionally, the thickness of the black film is more than or equal to 10 μm.
The invention has the beneficial effects that:
the black film obtained by the process of combining the mechanical polishing, the chemical polishing and the carbon-containing black dye solution which are periodically repeated has high glossiness and hardness, has excellent black appearance and wear resistance and is suitable for application.
Drawings
FIG. 1 is a real object diagram of an aluminum alloy workpiece coated with a black film obtained in example 4;
FIG. 2 is a surface SEM photograph of the black film obtained in example 4.
Detailed Description
The invention is further explained below with reference to the figures and the specific embodiments.
Example 1
The method for preparing the black film of example 1 includes the following steps:
1. rotational velocity gradient mechanical polishing
Firstly, performing low-speed mechanical polishing on the surface of an aluminum alloy blank workpiece at the rotating speed of 1000r/min for 5 min;
secondly, mechanically polishing the workpiece polished at low speed at a medium speed of 2000r/min for 10 min;
thirdly, performing high-speed mechanical polishing on the workpiece subjected to the medium-speed polishing at a rotating speed of 3000r/min for 15 min;
through the arrangement of gradient mechanical polishing, the flaws on the surface of the base material can be uniformly removed from the change from low rotating speed to high rotating speed, and then the surface with certain brightness is obtained.
2. Degreasing treatment
Putting the aluminum alloy workpiece subjected to high-speed mechanical polishing into 8% sulfuric acid solution for degreasing treatment, taking out after 10min, and putting into pure water for cleaning for 10 min;
3. alkali washing treatment
Putting the polished aluminum alloy workpiece into NaOH solution for alkali washing, wherein the process conditions are as follows: the concentration of NaOH is 45-55g/L, the temperature of the solution is 45-55 ℃, and the alkali washing time is 3 min; after the polishing workpiece is washed with alkali, putting the polishing workpiece into pure water for washing for 10 min;
4. neutralization treatment
Putting the aluminum alloy workpiece subjected to alkali washing into a nitric acid solution with the concentration of 140-150g/L for neutralization treatment; after the polishing workpiece is neutralized, putting the workpiece into pure water for cleaning for 10 min;
5. two-acid environment-friendly chemical polishing treatment
Firstly, putting the cleaned aluminum alloy workpiece into polishing solution containing 15% of sulfuric acid, 70% of phosphoric acid and 3% of additives for chemical polishing, wherein the chemical polishing additives mainly comprise nickel sulfate, polydithio-dipropyl sulfonate, sulfenyl benzimidazole, ethylene thiourea, sulfamic acid, wetting agent and the like. And (3) a chemical polishing process: the temperature is 100 ℃, and the polishing time is 20 min; washing after chemical polishing;
the chemical polishing adopts sulfuric acid and phosphoric acid, does not adopt waste water such as nitric acid and the like to treat complicated acid which causes great pollution to the environment, is more environment-friendly and has good polishing effect;
6. repeating steps 1-5
The mechanical polishing and the chemical polishing are repeated, so that the part with uneven surface reaction after the first chemical polishing can be further ground to obtain a bright and flat surface, and a black film obtained by subsequent anodic oxidation and dyeing is more uniform in film forming and good in dyeing effect.
7. Anodic oxidation treatment
Putting the washed aluminum alloy workpiece into an anodic oxidation solution for oxidation, wherein Al in the solution3+Has a concentration of 8g/L, H2SO4The concentration of (2) is 20%; and (3) an oxidation process: the voltage is 15V and the current is 2.0A/dm2The temperature is 15-20 ℃, and the oxidation time is 20 min;
8. treatment for dyeing black
And putting the anodized aluminum alloy workpiece into a chemical black dye solution for dyeing black. Black fuel solution composition: acid hair dye ATT 50-80g/L, acid lake blue 5-8g/L, carbon-containing additive 8 g/L; the dyeing process comprises the following steps: the temperature is 35-45 deg.C, pH value is 3-5, and time is 15-30 min; after dyeing, putting the workpiece into pure water for cleaning for 10 min; the carbonaceous additive used in this example was a particulate carbon powder having a particle size of 10-100 μm.
9. Hole sealing treatment
Placing the aluminum alloy workpiece after being colored black into a hole sealing agent solution for hole sealing treatment, wherein the pH value of the hole sealing agent solution is 5.5-6.5, the temperature is 75-85 ℃, and the time is 60 min; the pore sealing agent solution comprises 75g/L nickel acetate, 2g/L benzoic acid, 1.5g/L sodium benzoate, 18g/L naphthalene sulfonate, 2g/L sodium dodecyl sulfate and 1g/L organic silicon defoamer;
10. washing treatment
Cleaning the aluminum alloy workpiece after hole sealing for 15min by using normal-temperature ultrapure water; then, the mixture is cleaned for 20min by ultrapure water at 75 ℃.
The thickness of the resulting black film was about 10 μm.
Example 2
The black film of example 2 was prepared in substantially the same manner as in example 1, except that the content of the carbon-containing additive was changed to 12g/L in the black-coloring treatment.
Example 3
The black film of example 3 was prepared in substantially the same manner as in example 1, except that the content of the carbon-containing additive was changed to 16g/L in the black-coloring treatment.
Example 4
The black film of example 4 was prepared in substantially the same manner as in example 1, except that the content of the carbon-containing additive was changed to 20g/L in the black-coloring treatment.
The black film substance obtained in example 4 and SEM images are shown in FIGS. 1 and 2, and as can be seen from FIG. 1, a black film having a bright and flat mirror surface effect is obtained; as can be seen from FIG. 2, the obtained black film is uniform and compact, and the carbon particles are uniformly dispersed in the film, so that the effects of obviously improving hardness and resisting wear are achieved.
Comparative example 1
The black thin film of comparative example 1 was prepared in substantially the same manner as in example 1, except that the carbon-containing additive was not added in the black dyeing treatment.
Comparative example 2
The black film of comparative example 2 was prepared in substantially the same manner as in example 1, except that the content of the carbonaceous additive was changed to 4g/L in the black dyeing treatment.
Comparative example 3
The black thin film of comparative example 3 was prepared by a method different from that of example 1 in that one mechanical polishing + one chemical polishing was used for polishing, and the mechanical polishing was performed at a rotational speed of 2000r/min for 30 min.
The black films obtained in examples 1 to 4 and comparative examples 1 to 3 were subjected to the performance test, and the results are shown in the following table:
it can be seen from the examples and comparative examples that the product obtained by the present invention realizes the preparation of a black thin film with high glossiness and high hardness by combining the polishing process of periodically repeating mechanical polishing and chemical polishing with a carbon-containing coloring agent, and with the increase and compatibility of the content of the carbon additive, the whole thin film has stronger coloring ability, and the color is blacker, the glossiness is further improved, and the hardness is further improved.
The above examples are only for further illustrating the method of preparing the black thin film of the present invention, but the present invention is not limited to the examples, and any simple modification, equivalent change and modification made to the above examples according to the technical spirit of the present invention fall within the scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a black film is characterized by comprising the following steps:
1) polishing of
Performing periodic repeated mechanical polishing and chemical polishing on the surface of the aluminum alloy workpiece, wherein the mechanical polishing is multi-step polishing with increased rotating speed and polishing time gradient, the chemical polishing is to put the aluminum alloy workpiece after the mechanical polishing into polishing solution containing 10-20 wt% of sulfuric acid, 65-70 wt% of phosphoric acid and 1-5 wt% of additives for chemical polishing, the temperature is 80-100 ℃, and the polishing time is 10-30 min;
2) anodic oxidation
Putting the polished aluminum alloy workpiece into an anodic oxidation solution for oxidation, wherein the voltage is 10-20V, and the current is 1.0-3.0A/dm2The temperature is 15-20 ℃, and the oxidation time is 10-30 min;
3) dyeing process
Placing the anodized aluminum alloy workpiece into a black dye solution for dyeing at the temperature of 35-45 ℃ and the pH value of 3-5 for 15-30 min; the black dye solution contains 50-80g/L of acidic hair dye ATT, 5-8g/L of acidic lake blue and 8-20g/L of carbon-containing additive; after dyeing, putting the workpiece into pure water for cleaning for 5-20 min;
4) sealing of
Placing the dyed aluminum alloy workpiece into a hole sealing agent solution for hole sealing treatment at the temperature of 75-85 ℃ for 40-80 min;
5) washing with water
Cleaning the aluminum alloy workpiece after hole sealing with normal-temperature ultrapure water for 10-20 min; then cleaning with ultrapure water of 60-90 ℃ for 10-30 min.
2. The method for producing a black thin film according to claim 1, wherein: the multi-step polishing comprises at least two steps, the rotating speed of each step is increased by 500-1500r/min compared with the previous step, and the polishing time is increased by 3-8min compared with the previous step.
3. The method for producing a black thin film according to claim 2, wherein: the multi-step polishing is three-step polishing; the rotation speed of the first step of polishing is 500-; the rotation speed of the second step of polishing is 1500-; the rotation speed of the third step of polishing is 2500-.
4. The method for producing a black thin film according to claim 1, wherein: the chemical polishing additive comprises at least one of nickel sulfate, polydithio-dipropyl sulfonate, thio-benzimidazole, ethylene thiourea, sulfamic acid and wetting agent.
5. The method for producing a black thin film according to claim 1, wherein: the polishing period is 2-5.
6. The method for producing a black thin film according to claim 1, wherein: the mechanical polishing and the chemical polishing also comprise the steps of degreasing, alkali washing and neutralizing treatment of the aluminum alloy workpiece.
7. The method for producing a black thin film according to claim 6, wherein: putting the mechanically polished aluminum alloy workpiece into a 5-10% sulfuric acid solution for degreasing treatment, taking out after 5-15min, and putting the aluminum alloy workpiece into pure water for cleaning for 5-20 min; then, putting the aluminum alloy workpiece into a NaOH solution with the concentration of 45-55g/L for alkali washing, wherein the solution temperature is 45-55 ℃, the alkali washing time is 2-5min, and after the alkali washing, putting the aluminum alloy workpiece into pure water for washing for 5-20 min; and (3) putting the aluminum alloy workpiece subjected to alkali washing into a nitric acid solution with the concentration of 140-150g/L for neutralization treatment, and then putting the aluminum alloy workpiece into pure water for washing for 5-20 min.
8. The method for producing a black thin film according to claim 1, wherein: the anodic oxidation solution contains 5-10g/L of Al3+And 15-25 wt% H2SO4。
9. The method for producing a black thin film according to claim 1, wherein: the carbon-containing additive is granular carbon powder with the grain diameter of 10-100 mu m.
10. The method for producing a black thin film according to claim 1, wherein: the thickness of the black film is more than or equal to 10 mu m.
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Cited By (1)
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CN114517319A (en) * | 2022-03-01 | 2022-05-20 | 九牧厨卫股份有限公司 | Gray golden sterilization film, gray golden sterilization product and preparation method of gray golden sterilization film |
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CN114517319A (en) * | 2022-03-01 | 2022-05-20 | 九牧厨卫股份有限公司 | Gray golden sterilization film, gray golden sterilization product and preparation method of gray golden sterilization film |
CN114517319B (en) * | 2022-03-01 | 2024-03-29 | 九牧厨卫股份有限公司 | Gray-gold sterilizing film, gray-gold sterilizing product and preparation method of gray-gold sterilizing film |
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