CN113089047A - Aluminum alloy component and preparation method and application thereof - Google Patents
Aluminum alloy component and preparation method and application thereof Download PDFInfo
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- CN113089047A CN113089047A CN202110390355.6A CN202110390355A CN113089047A CN 113089047 A CN113089047 A CN 113089047A CN 202110390355 A CN202110390355 A CN 202110390355A CN 113089047 A CN113089047 A CN 113089047A
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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
- C25D11/026—Anodisation with spark discharge
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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
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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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Abstract
The invention discloses an aluminum alloy member and a preparation method and application thereof, wherein the preparation method comprises the following steps: s1, generating an aluminum oxide ceramic membrane on the surface of the aluminum alloy by adopting a micro-arc oxidation technology; and S2, coating a hydrophilic layer on the surface of the alumina ceramic membrane. According to the invention, the aluminum oxide ceramic membrane is generated on the surface of the aluminum alloy by adopting the micro-arc oxidation technology, so that the mechanical strength of the surface of the aluminum alloy is enhanced, the obtained enhanced surface is a rough structure containing a pore channel, the structure is beneficial to coating an organic or inorganic coating on the surface, and the surface hydrophilic layer plays a role in filling the pore channel generated by micro-arc oxidation on the surface, so that the pore channel position is protected to prevent the pore channel from being corroded by the environment firstly, and meanwhile, the binding force between the membrane layer and the surface is enhanced.
Description
Technical Field
The invention relates to the field of surface treatment of aluminum and aluminum alloy, in particular to an aluminum alloy member and a preparation method and application thereof.
Background
The aluminum and the aluminum alloy have the advantages of light weight, strong impact absorbability, no magnetism, easy processing and forming, weldability and the like. The material can be well processed into bars, plates, sections and the like with various styles and sizes, is widely applied in the fields of spaceflight, aviation, automobiles, war industry and the like, and is a second engineering material which is second only to steel.
However, aluminum and its alloys also have significant disadvantages such as low hardness, poor wear resistance, lack of corrosion resistance in certain media, etc., which limit their range of use. For example, aluminum alloy fins used in air conditioners can generate a "white powder" phenomenon in an alternate dry and wet environment, that is, a corrosion phenomenon such as cracking and falling of an aluminum oxide thin layer on the surface; because the surface hydrophilicity is poor, a 'water bridge' phenomenon can be generated on the air-conditioning fins which are arranged densely; the product can generate 'water rust' and 'peculiar smell' after long-term use; the marine aluminum alloy structure product is in a high-humidity, high-heat and high-salt-spray environment at sea and on the coast for a long time and is washed by seawater, and the seawater can gradually permeate to the surface of the material aluminum alloy through micropores, so that corrosion problems such as water bridges, water rust and the like are caused; (ii) a The conventional improvement is to perform acid or alkali etching on the surface of aluminum or aluminum alloy to obtain a rough surface to achieve super-hydrophilic effect, so that the water contact angle of the surface is small. Finally, the purpose of reducing the water bridge phenomenon is achieved. The disadvantages of this technique are that the mechanical strength of the aluminum surface is not high, the long-term service life is not high, and the generation of "scale" and "odor" cannot be avoided.
Disclosure of Invention
The invention aims to provide a preparation method of an aluminum alloy member, which improves the hardness, hydrophilicity and corrosion resistance of the aluminum alloy member.
The invention is realized by the following technical scheme:
a method of making an aluminum alloy component, comprising the steps of:
s1, generating an aluminum oxide ceramic membrane on the surface of the aluminum alloy by adopting a micro-arc oxidation technology;
and S2, coating a hydrophilic layer on the surface of the alumina ceramic membrane.
The micro-arc oxidation technology (MAO), also known as spark discharge anodic oxidation, Anodic Spark Deposition (ASD) or micro-plasma oxidation (MPO), is a new technology developed in recent decades for in-situ growth of oxide ceramic membranes on the surfaces of nonferrous metals. The technology is that valve metal such as aluminum, magnesium, titanium and the like is used as an anode and is placed in electrolyte, a working area of voltage is introduced into a high-voltage discharge area from a common anode oxidation Faraday area, plasma spark discharge is generated on the surface of the valve metal, and a dense oxide film which has metal characteristics and ceramic characteristics and is metallurgically bonded with a substrate is formed by utilizing instantaneous high temperature and high pressure generated in a micro area along with the generation of a plurality of complicated chemical, electrochemical, physical and chemical reactions and the like.
According to the invention, the aluminum oxide ceramic membrane is generated on the surface of the aluminum alloy by adopting the micro-arc oxidation technology, so that the mechanical strength of the surface of the aluminum alloy is enhanced, the obtained enhanced surface is a rough structure containing a pore channel, the structure is beneficial to coating an organic or inorganic coating on the surface, and the surface hydrophilic layer plays a role in filling the pore channel generated by micro-arc oxidation on the surface, so that the pore channel position is protected to prevent the pore channel from being corroded by the environment firstly, and meanwhile, the binding force between the membrane layer and the surface is enhanced.
Further, a transition layer is applied prior to the application of the hydrophilic layer.
Further, the transition layer is polymethacrylate, and the film thickness is 0.5-25 g/m2The drying temperature for coating the transition layer is 245-250 ℃, and the drying time is 20-25 s.
Further, in step S1, the micro-arc oxidation technology adopts a silicate electrolyte system, a constant current power supply or a pulse direct current power supply, and the oxidation time is 10-60 min.
Further, the hydrophilic layer has a film thickness of 0.2 to 1.5g/m2。
Further, the hydrophilic layer comprises a water-soluble fiber resin hydrophilic layer, a silicon dioxide hydrophilic layer and SiO2/TiO2Hydrophilic layer or inorganic binder AP/TiO2A hydrophilic layer.
Further, SiO2/TiO2The preparation of the hydrophilic layer comprises the following steps:
1) preparation of TiO2Sol: dropwise adding tetrabutyl titanate into absolute ethyl alcohol and acetylacetone, and uniformly mixing;
2) preparation of SiO2Sol: slowly adding TEOS into absolute ethyl alcohol, then adding hydrochloric acid, and stirring;
3)、TiO2sol and SiO2Mixing sol, adding hydrochloric acid, and stirring to obtain a mixed sol solution;
4) preparing TiO on a sample by adopting a soaking and pulling method2-SiO2Film formation: and putting the micro-arc oxidized sample into the mixed sol solution, and then taking out.
Further, an inorganic binder AP/TiO2The preparation of the hydrophilic layer comprises the following steps:
A) and preparing an inorganic binder: h3PO4Diluting with deionized water, adding Al (OH)3Stirring to obtain an inorganic binder AP;
B) dissolving the inorganic binder AP in deionized water, and stirring to obtain an AP solution;
C) adding nano TiO2Adding the powder into alcohol or deionized water, and stirring to obtain TiO2A solution;
D) adding AP solution to TiO2Stirring the solution, adding the flatting agent, and uniformly stirring and mixing;
E) and D, placing the micro-arc oxidized sample into the solution obtained in the step D, and standing.
An aluminum alloy member prepared by the above preparation method.
The application of the aluminum alloy member in a corrosive medium and dry-wet alternate environment.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention adopts the micro-arc oxidation technology to effectively enhance the surface strength of the aluminum and the aluminum alloy and prolong the service life of the aluminum and the aluminum alloy.
2. The microstructure formed on the surface of the aluminum alloy through micro-arc oxidation enhances the adhesive force of the hydrophilic film on the surface and simultaneously improves the hydrophilic capability of the film layer; the hydrophilic coating on the surface plays a role in filling the pore channel generated by micro-arc oxidation, so that the position of the pore channel is protected, the pore channel is prevented from being corroded by the environment firstly, and meanwhile, the binding force between the film layer and the surface is enhanced.
3. The good hydrophilic performance of the invention can effectively reduce or even eliminate the occurrence of 'water bridge' phenomenon in application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1:
a method of making an aluminum alloy component, comprising the steps of:
s1, micro-arc oxidation: this experiment uses the electrolyte system that commonly used silicate is main, adopts the deionized water configuration, and the composition is: 20g/L Na2SO3·9H2O，5g/L(NaPO3)61g/L KOH; adopting a constant current power supply: selecting only positive pulse with current density of 10A/dm2Duty ratio of 60%, frequency of 200HZ, treatment temperature controlled below 40 deg.C, and oxidation time of 60 min; taking out the sample after micro-arc oxidation, washing the sample with deionized water, and blow-drying the sample;
s2, coating a transition layer: the thickness of the coating film is 0.5 to 25g/m2Drying the polymethacrylate ester at 250 ℃ for 20 s;
s3, coating a hydrophilic layer: a water-soluble fiber resin was coated on a polymethacrylate film to a thickness of 1.5g/m2And drying at 250 ℃ for 20 s.
6063 aluminum alloy has been treated as described above and tested to have a water contact angle of about 10 degrees and a microhardness of 1490 HV.
Example 2:
a method of making an aluminum alloy component, comprising the steps of:
s1, micro-arc oxidation: a pulse direct current power supply is adopted, the frequency is 500Hz, and the duty ratio is 15% -20%; the voltage is 300V-400V; the reaction time is 10min to 30min, and silicate electrolyte, 2g/L NaOH and 8g/L Na are selected2SiO3；
S2, preparing a hydrophilic membrane stock solution: 5g of silica dissolved in 120ml of H2O and 180ml of alcohol; stirring for 30min, ultrasonically oscillating for 15min, stirring for a long time, finally adding 2ml of polyurethane solution, and continuing stirring;
s3, coating a hydrophilic layer: pouring the silicon dioxide solution on a sample for several timesThen hung and blown dry by an air gun to dry residual liquid with the film thickness of 1.5g/m2And finally drying for 2 hours at 70 ℃.
6063 aluminum alloy has been treated as described above and tested to have a water contact angle of about 18 degrees and a microhardness of 1600 HV. After 100 hours of soaking in 3.5 wt% NaCl water solution, the surface has no obvious corrosion.
Example 3:
a method of making an aluminum alloy component, comprising the steps of:
s1, micro-arc oxidation: a pulse direct current power supply is adopted, the electrical parameters are selected to be 300V-600V of voltage, 500Hz of frequency, 12-18% of duty ratio, and the reaction time is 10 min-30 min. The electrolyte mainly contains Na2SiO3And (NaPO)3)6In which Na2SiO3Has a concentration of 8g/L (NaPO)3)6The concentration of (A) is 7.5 g/L;
s2 preparation and SiO coating2/TiO2Hydrophilic layer:
1) preparation of TiO2Sol: 20.5g (0.06mol) of tetrabutyl titanate (TBOT) was added dropwise to 100g of absolute ethanol and 60.3g of acetylacetone, and stirred for 1 hour;
2) preparation of SiO2Sol: slowly adding 8.3g (0.04mol) of TEOS into 36.9g of absolute ethyl alcohol, then adding 0.65ml of HCl, and stirring for 1 h;
3)、TiO2sol and SiO2Mixing the sol, adding 1.8ml of HCl, and stirring for 1h to obtain a mixed sol solution;
4) preparing TiO on a sample by adopting a soaking and pulling method2-SiO2Film formation: placing the micro-arc oxidized sample into the mixed sol solution for 5min, and taking out the sample to obtain a film with a thickness of 1.5g/m2；
5) Drying the sample at 200 ℃ for 30min, then heating to 550 ℃ in a muffle furnace at the heating rate of 2 ℃/min, preserving the heat for 1 hour, and naturally cooling.
6063 aluminum alloy has a water contact angle of about 10 degrees and a microhardness of 1800HV as measured by the above treatment. After 100 hours of soaking in 3.5 wt% NaCl water solution, the surface has no obvious corrosion.
Example 4:
a method of making an aluminum alloy component, comprising the steps of:
s1, micro-arc oxidation: the electrolyte consists of 9g/L of Na2SiO3And 2g/L of Na OH, with a positive/negative current density of 8/4A dm-2The pulse frequency was 200Hz, the duty ratio was 20%, and the ratio of the positive/negative pulse number in a single period was 1. The oxidation time is 15min to 45 min;
s2, preparation and coating of a hydrophilic layer:
A) and preparing an inorganic binder: 90g of 85% H are taken3PO437.5g of deionized water was added, diluted to 60% and stirred at 100 ℃ to obtain 20.3g of Al (OH) in a molar ratio of 3:13Addition of H3PO4Continuously stirring the solution for 3 hours to obtain an inorganic binder AP;
B) dissolving 80g of AP in 200ml of deionized water, and stirring to obtain an AP solution;
C) about 0.5-2 g of nano TiO is taken2Adding the powder into 15ml of alcohol/deionized water, stirring for 30min, and then performing ultrasonic oscillation for 15min to obtain TiO2A solution;
D) adding AP solution to TiO2Stirring the solution for 10min, and then ultrasonically oscillating the solution for 15 min; finally, 2 drops of BKY leveling agent is added, and the mixture is continuously stirred and evenly mixed;
E) putting the micro-arc oxidized sample into the solution obtained in the step D, standing, and finally blowing off the redundant solution by an air gun to obtain a film with the thickness of 1.5g/m2；
F) Drying the sample after standing, airing and spraying for 2 hours at the temperature of 120 ℃; then heated at 240 ℃ for 1 hour.
6063 aluminum alloy has been treated as described above and tested to have a water contact angle of about 10 degrees and a microhardness of 1690 HV. After 100 hours of soaking in 3.5 wt% NaCl water solution, the surface has no obvious corrosion.
Comparative example 1:
this comparative example is based on example 1 and differs from example 1 in that only the micro-arc oxidation treatment is performed.
6063 aluminum alloy has been treated as described above and tested to have a water contact angle of about 23 degrees and a microhardness of 1510 HV.
Comparative example 2:
this comparative example is based on example 2 and differs from example 2 in that the micro-arc oxidation treatment is not performed.
6063 aluminum alloy has been treated as described above and tested to have a water contact angle of about 25 degrees and a microhardness of 100 HV. After 10 hours of immersion in 3.5 wt% NaCl aqueous solution, the surface hydrophilic layer was peeled off and severe pitting corrosion was observed.
Comparative example 3:
this comparative example is based on example 3 and differs from example 3 in that the micro-arc oxidation treatment is not performed.
6063 aluminum alloy has been treated as described above and tested to have a water contact angle of about 25 degrees and a microhardness of 110 HV. After immersion in 3.5 wt% NaCl aqueous solution for 10 hours, the hydrophilic layer on the surface was partially peeled off, and pitting was observed.
Comparative example 4:
this comparative example is based on example 4 and differs from example 4 in that the micro-arc oxidation treatment is not performed.
6063 aluminum alloy has been treated as described above and tested to have a water contact angle of about 25 degrees and a microhardness of 103 HV. After 100 hours of immersion in 3.5 wt% NaCl aqueous solution, the surface hydrophilic layer was peeled off and severe pitting corrosion was observed.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method of making an aluminum alloy component, comprising the steps of:
s1, generating an aluminum oxide ceramic membrane on the surface of the aluminum alloy by adopting a micro-arc oxidation technology;
and S2, coating a hydrophilic layer on the surface of the alumina ceramic membrane.
2. A method of manufacturing an aluminium alloy member according to claim 1, wherein the transition layer is applied before the hydrophilic layer.
3. The method for manufacturing an aluminum alloy member according to claim 2, wherein the transition layer is polymethacrylate, and the thickness of the film is 0.5-25 g/m2The coating temperature of the transition layer is 245-250 ℃ and the time is 20-25 s.
4. The method of claim 1, wherein the micro-arc oxidation technique in step S1 uses a silicate electrolyte system, and uses a constant current power supply or a pulse DC power supply, and the oxidation time is 10-60 min.
5. The method of claim 1, wherein the hydrophilic layer has a film thickness of 0.2-1.5 g/m2。
6. The method of claim 1, wherein the hydrophilic layer comprises a water-soluble fiber resin hydrophilic layer, a silica hydrophilic layer, SiO2/TiO2Hydrophilic layer or inorganic binder AP/TiO2A hydrophilic layer.
7. The method of claim 6, wherein the SiO is in the form of a film2/TiO2The preparation of the hydrophilic layer comprises the following steps:
1) preparation of TiO2Sol: dropwise adding tetrabutyl titanate into absolute ethyl alcohol and acetylacetone, and uniformly mixing;
2) preparation of SiO2Sol: slowly adding TEOS into absolute ethyl alcohol, then adding hydrochloric acid, and stirring;
3)、TiO2sol and SiO2Mixing the sol, adding hydrochloric acid, and stirringStirring to obtain a mixed sol solution;
4) preparing TiO on a sample by adopting a soaking and pulling method2-SiO2Film formation: and putting the micro-arc oxidized sample into the mixed sol solution, and then taking out.
8. The method of claim 6, wherein the inorganic binder AP/TiO is selected from the group consisting of2The preparation of the hydrophilic layer comprises the following steps:
A) and preparing an inorganic binder: h3PO4Diluting with deionized water, adding Al (OH)3Stirring to obtain an inorganic binder AP;
B) dissolving the inorganic binder AP in deionized water, and stirring to obtain an AP solution;
C) adding nano TiO2Adding the powder into alcohol or deionized water, and stirring to obtain TiO2A solution;
D) adding AP solution to TiO2Stirring the solution, adding the flatting agent, and uniformly stirring and mixing;
E) and D, placing the micro-arc oxidized sample into the solution obtained in the step D, and standing.
9. An aluminum alloy structural member produced by the method for producing an aluminum alloy structural member according to any one of claims 1 to 8.
10. Use of the aluminum alloy member of claim 9 in a corrosive medium, wet and dry alternating environment.
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