CN112195491A - SiC-Al based on micro-arc oxidation2O3Method for producing a coating - Google Patents
SiC-Al based on micro-arc oxidation2O3Method for producing a coating Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 93
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 72
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- 238000002360 preparation method Methods 0.000 claims abstract description 68
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 20
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 12
- 239000005011 phenolic resin Substances 0.000 claims abstract description 12
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 12
- 229910020350 Na2WO4 Inorganic materials 0.000 claims abstract description 11
- 239000010935 stainless steel Substances 0.000 claims description 25
- 229910001220 stainless steel Inorganic materials 0.000 claims description 25
- 238000004140 cleaning Methods 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 19
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- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
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- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 5
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 238000002161 passivation Methods 0.000 description 7
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- 229910052814 silicon oxide Inorganic materials 0.000 description 3
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
Abstract
The invention provides SiC-Al based on micro-arc oxidation2O3The preparation method of the coating comprises the steps of matrix pretreatment, solution preparation, composite ceramic coating preparation and ceramic layer post-treatment, and the inner layer obtained by the method is Al2O3Ceramic layer, SiC-Al with SiC ceramic layer as outer layer2O3A composite layer, wherein the thickness of the composite layer is 30-400 μm; wherein, KOH-Na is adopted in the solution preparation2SiO3‑(NaPO3)6‑Na2WO4Deionized water solution as main component and mixed solution of alkaline silica sol solution, water soluble phenolic resin and nanometer SiC grains. The method of the invention prepares the two-layer composite on the surface of the aluminum alloy workpiece by a one-step micro-arc oxidation processThe ceramic layer has high preparation efficiency, low production energy consumption and low preparation cost, and saves preparation time; meanwhile, the method does not need hole sealing treatment, the bonding strength between the ceramic layer and between the ceramic layer and the substrate is high, the compactness of the composite ceramic coating is good, and the overall wear resistance, corrosion resistance, heat insulation and ablation resistance of the aluminum alloy workpiece are excellent.
Description
Technical Field
The invention relates to the technical field of surface treatment, in particular to SiC-Al based on micro-arc oxidation2O3A method for preparing the coating.
Background
Aluminum alloy, an alloy based on aluminum with a certain amount of other alloying elements added, is one of light metal materials. In addition to the general characteristics of aluminum, aluminum alloys have certain alloy specific characteristics due to the variety and amount of alloying elements added. The aluminum alloy has a density of 2.63-2.85 g/cm and a high strength (delta)b110-650 MPa), the strength of the alloy is close to that of high alloy steel, the rigidity of the alloy is higher than that of common steel, the alloy has good casting performance and plastic processing performance, good electric conduction and heat conduction performance, good corrosion resistance and weldability, and can be used as a structural material, so that the aluminum alloy has wide application in aerospace, aviation, transportation, construction, electromechanics, lightening and daily necessities. However, the aluminum alloy has the defects of low melting point, quick heat transfer, easy oxidation at high temperature, no wear resistance and the like, so that when the aluminum alloy is applied to severe conditions of high temperature and high wear, such as aerospace, weaponry and the like, the internal structure of the aluminum alloy is extremely easy to damage, and the application range of the aluminum alloy is greatly restricted.
Micro-arc oxidation, also known as Plasma Electrolytic Oxidation (PEO), has evolved from the technology of anodic oxidation, with the resulting coatings being superior to anodic oxidation. The micro-arc oxidation process mainly depends on matching and adjustment of electrolyte and electrical parameters, and under the action of instantaneous high temperature and high pressure generated by arc discharge, a modified ceramic coating which mainly comprises matrix metal oxide and is supplemented with electrolyte components grows on the surfaces of valve metals such as aluminum, magnesium, titanium and the like and alloys thereof, and the corrosion resistance and the wear resistance of the modified ceramic coating are obviously superior to those of the traditional anodic oxidation coating, so that the micro-arc oxidation process is widely concerned in application to marine ships and aviation components. However, in the micro-arc oxidation process, a large amount of gas can be discharged from the workpiece due to the high-temperature sintering effect, and the gas generates pores when passing through the micro-arc oxidation film, so that the micro-arc oxidation film has low compactness, and the corrosion resistance and the wear resistance of the micro-arc oxidation film are closely related to the subsequent hole sealing technology; meanwhile, the single micro-arc oxidation film is thin and large in brittleness, and the abrasion resistance of the single micro-arc oxidation film cannot completely meet the requirements of weaponry and aerospace due to repeated, repeated and high-strength friction of most of equipment in aerospace and weaponry.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide SiC-Al based on micro-arc oxidation2O3The preparation method of the coating comprises the steps of preparing an inner layer of Al on the surface of an aluminum alloy workpiece by a one-step micro-arc oxidation process2O3The ceramic layer and the outer layer are the two-layer composite coating of the SiC ceramic layer, so that the preparation efficiency is greatly improved, and the energy consumption and the cost in the production process are reduced; meanwhile, the method does not need hole sealing treatment, and Al2O3The ceramic layer and the SiC ceramic layer have high bonding strength, the composite coating has good compactness and excellent wear resistance, corrosion resistance, heat insulation and ablation resistance.
The purpose of the invention is realized by the following technical scheme:
SiC-Al based on micro-arc oxidation2O3The preparation method of the coating is characterized by comprising the following steps: the method comprises the steps of matrix pretreatment, solution preparation, composite ceramic coating preparation and ceramic layer post-treatment, and the inner layer obtained by the method is Al2O3Ceramic layer, SiC-Al with SiC ceramic layer as outer layer2O3The composite ceramic layer has a thickness of 30～400μm；
Specifically, the method comprises the following steps:
the solution is prepared by the following steps: firstly, KOH-Na is added into a stainless steel solution tank2SiO3-(NaPO3)6- Na2WO4Adding an alkaline silica sol solution, water-soluble phenolic resin and nano SiC particles into deionized water solution serving as a main component, and continuously stirring to fully dissolve all the components into the deionized water to finally obtain mixed preparation liquid;
the composite ceramic coating is prepared by the following steps: designing a special tool according to the structural characteristics of an aluminum alloy element, clamping the aluminum alloy element on an anode of a high-voltage direct-current pulse power supply, placing the aluminum alloy element on the special tool in a stainless steel solution tank, immersing the special tool in a mixed preparation solution, connecting the stainless steel solution tank with a cathode of the high-voltage direct-current pulse power supply, and finally adjusting the parameters of the high-voltage direct-current pulse power supply to perform SiC-Al2O3The preparation of the composite ceramic coating needs to add positive and negative voltages simultaneously in the preparation process of the coating, and finally the SiC-Al is obtained2O3And compounding a ceramic layer.
As known by the technical personnel in the field, SiC has poor water solubility, and if the SiC is directly prepared on the surface of the aluminum alloy, high-temperature ablation is needed, and the high temperature can cause the melting of the aluminum alloy, so that the deformation of an aluminum alloy workpiece is caused; meanwhile, due to the crystal and chemical bond characteristics of SiC, SiC is difficult to adsorb on the alumina film, if the SiC ceramic layer and Al are directly carried out2O3The compounding of the ceramic layer can lead to the combination of the SiC ceramic layer and the Al2O3The ceramic layers have low bonding force and are easy to peel off, even Al2O3And a case where the SiC ceramic layer cannot be formed at all on the surface of the ceramic layer. The invention adopts KOH-Na2SiO3-(NaPO3)6- Na2WO4Mixing deionized water solution as main component, alkaline silica sol solution, water soluble phenolic resin and nano SiC particles as solvent, and firstly carrying out micro-arc oxidation on an aluminum alloy workpiece to generate Al by controlling parameters of a high-voltage direct-current pulse power supply2O3Ceramic layer, and then adsorbed on Al by positive polarity action of silicon oxide2O3On the ceramic layer, silicon oxide is carbonized to generate SiC (silicon oxide absorbs a small amount of SiC particles and a carbon source in water-soluble phenolic resin and the absorbed SiC particles enhance the compactness of the SiC ceramic layer generated by carbonization) due to arc ablation in micro-arc oxidation, and Al is filled in the ceramic layer during silicon oxide absorption2O3Micropores in the ceramic layer, SiC after carbonization, are also filled with Al in situ2O3The micropores in the ceramic layer can be sealed, so ensuring the formation of Al2O3The compact SiC ceramic layer with high bonding strength is generated at the micropores and on the surface of the ceramic layer, so that the peeling and falling off of the SiC ceramic layer are avoided. And, due to Al2O3The ceramic layer is generated in situ on the aluminum alloy workpiece, so that the composite ceramic layer has high bonding strength with the aluminum alloy workpiece.
The invention prepares SiC-Al2O3Composite ceramic coating (i.e. inner layer of Al)2O3The ceramic layer and the outer layer are SiC ceramic layers) are prepared into two ceramic layers with high bonding strength by adopting a one-step micro-arc oxidation process, subsequent treatment processes are not needed for treatment, the preparation efficiency is high, the speed is high, the preparation time is greatly saved, and the energy consumption and the cost in the preparation are reduced.
Further optimization, the matrix pretreatment specifically comprises the following steps: an ultrasonic cleaning instrument is adopted to carry out dust removal, oil removal and cleaning on the aluminum alloy element, an oxidation film is removed, deionized water or distilled water is used for cleaning after treatment, and then alkali cleaning is carried out;
further optimization, the step of removing the oxidation film specifically comprises: by means of H3PO4And Al (OH)3And (3) reacting to obtain an aqueous solution treatment solution of the aluminum dihydrogen phosphate sol, and immersing the aluminum alloy element cleaned by the ultrasonic cleaner into the solution for 2-3 min to remove oxide skin on the surface of the aluminum alloy.
Further optimizing, the alkali washing step specifically comprises: and (3) carrying out surface alkaline washing and passivation on the aluminum alloy subjected to oxide film removal and deionized water cleaning by using a NaOH solution with the invasion concentration of 10-20 g/L, wherein the invasion time is 3-10 min.
For further optimization, the KOH and the Na are2SiO3、(NaPO3)6、Na2WO4The concentration of the water-soluble organic compound is 3-8 g/L, 8-16 g/L, 5-12 g/L and 6-15 g/L.
Further optimizing, wherein the concentration of the alkaline silica sol solution is 30-90 ml/L; the pH value of the alkaline silica sol solution is 7-10.
Further optimizing, the alkaline silica sol solution contains SiO with the content of 30 percent or more and the grain diameter of less than 20 nm2And (3) granules.
Further optimizing, the concentration of the water-soluble phenolic resin is 10-50 g/L.
Further optimizing, the concentration of the nano SiC particles is 5-30 g/L.
Further optimizing, the water quality of the deionized water in the solution preparation process is 10M omega-cm @25 ℃ or above.
For further optimization, the deionized water in the solution preparation process can be replaced by high-purity distilled water, and the high-purity distilled water is water obtained by three times of distillation or more.
Further optimization, the stainless steel solution tank is made of conductive stainless steel, has sufficient cooling capacity, and can ensure that the temperature of the solution is kept below 30 ℃ in the preparation process.
The high-voltage direct-current pulse power supply is a special high-voltage direct-current pulse power supply with adjustable positive and negative voltages, adjustable positive and negative pulse ratios, adjustable positive and negative pulse widths and adjustable frequency; and the positive and negative voltages of the high-voltage direct-current pulse power supply are both above 700V.
Further optimizing, the technological parameters of the high-voltage direct-current pulse power supply in the preparation process of the composite ceramic coating are as follows: the current density is 3-8A/dm2(ii) a The frequency is 700-1200 Hz; the pulse width of the positive pulse is 10-80%, and the ratio of the positive pulse to the negative pulse is 1:1 or 1:2 or 2: 1; the positive voltage and the negative voltage are both 10-700V, the ratio of the positive voltage to the negative voltage is 3:1, and the processing time is 10-30 min.
Preferably, the pulse width of the positive pulse is 20% to 50%.
Further optimization, the ceramic layer post-treatment specifically comprises the following steps: and (3) washing the aluminum alloy element obtained after the preparation process of the composite ceramic coating by using deionized water or distilled water, and then drying by using a hair drier.
The invention has the following technical effects:
the invention prepares the inner layer of Al on the surface of the aluminum alloy element by a one-step micro-arc oxidation process2O3Ceramic layer, two-layer composite coating with SiC ceramic layer as outer layer, i.e. SiC-Al2O3The composite ceramic coating does not need to be subjected to special hole sealing treatment in the later period, so that the process steps are greatly saved, the production time is saved, the preparation efficiency and the production efficiency are improved, the energy consumption required by production is saved, and the production cost is reduced. Meanwhile, the two composite coatings prepared by the method have high bonding strength, good compactness, good wear resistance of the whole composite ceramic layer, and good corrosion resistance, heat insulation and ablation resistance, and cannot be peeled or shed.
The composite coating prepared by the method can effectively improve the performances of wear resistance, corrosion resistance, heat insulation, ablation resistance and the like of the aluminum alloy workpiece, so that the aluminum alloy workpiece can meet the requirements of the worst conditions in the fields of weaponry, aerospace and the like, and the application range is wide.
Drawings
FIG. 1 shows SiC-Al prepared in examples of the present invention2O3The surface micro-morphology of the composite ceramic coating.
FIG. 2 shows SiC-Al prepared in an example of the present invention2O3The microscopic appearance of the cross section of the composite ceramic coating.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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 derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
SiC-Al based on micro-arc oxidation2O3The preparation method of the coating is characterized by comprising the following steps: the method comprises the steps of matrix pretreatment, solution preparation, composite ceramic coating preparation and ceramic layer post-treatment, and the inner layer obtained by the method is Al2O3Ceramic layer, SiC-Al with SiC ceramic layer as outer layer2O3The ceramic layer is compounded, and the thickness of the ceramic layer is 60 mu m;
the method specifically comprises the following steps:
a. matrix pretreatment:
firstly, an ultrasonic cleaner is adopted to carry out dust removal and oil removal cleaning on an aluminum alloy element in deionized water; then using H3PO4And Al (OH)3Reacting to obtain an aqueous solution treatment solution of aluminum dihydrogen phosphate sol, immersing the aluminum alloy element cleaned by an ultrasonic cleaner into the solution for 2min to remove oxide skin on the surface of the aluminum alloy, and cleaning the aluminum alloy element by deionized water after treatment; finally, performing surface alkaline washing and passivation on the aluminum alloy workpiece immersed in NaOH solution with the concentration of 10g/L for 3 min; because the pH value of the solution formula for preparing the coating is about 9, in order to keep the solution characteristics, the aluminum alloy workpiece needs to be subjected to alkali cleaning and passivation.
b. Solution preparation:
KOH-Na is added into a stainless steel solution tank2SiO3- (NaPO3)6- Na2WO4Adding an alkaline silica sol solution, water-soluble phenolic resin and nano SiC particles into deionized water solution serving as a main component, and continuously stirring to fully dissolve all the components into the deionized water; wherein, KOH and Na2SiO3、(NaPO3)6、Na2WO4The concentration of (b) is 3g/L, 8g/L, 5g/L and 6g/L respectively; the concentration of the alkaline silica sol solution is 30ml/L, the pH value of the alkaline silica sol solution is 7, and the alkaline silica sol solution contains SiO2 particles with the content of 30 percent or more and the particle size of less than 20 nm; the concentration of the water-soluble phenolic resin is 10 g/L; the concentration of the nano SiC particles is 5 g/L; the deionized water has a water quality of 10M omega cm @25 ℃ or above.
Analytical pure reagents are adopted for each chemical component in the solution.
The stainless steel solution tank is made of conductive stainless steel, has sufficient cooling capacity, and can ensure that the temperature of the solution is kept below 30 ℃ in the preparation process.
c. Preparing a composite ceramic coating:
designing a special tool according to the structural characteristics of an aluminum alloy element (namely designing a clamping tool which can be suitable for micro-arc oxidation according to the specific shape of an aluminum alloy workpiece), clamping the aluminum alloy element on the anode of a high-voltage direct-current pulse power supply, placing the aluminum alloy element on the special tool in a stainless steel solution tank, and connecting the stainless steel solution tank with the cathode of a power supply, wherein the high-voltage direct-current pulse power supply is a special high-voltage direct-current pulse power supply with adjustable positive and negative voltages, adjustable positive and negative pulse ratios, adjustable positive and negative pulse widths and adjustable frequency; and the positive and negative voltages of the high-voltage direct-current pulse power supply are both above 700V.
Adjusting parameters of high-voltage direct-current pulse power supply and carrying out SiC-Al2O3The preparation of the composite ceramic coating needs to add positive and negative voltages simultaneously in the coating preparation process; the parameters of the high-voltage direct-current pulse power supply are as follows: the current density is 3A/dm2(ii) a The frequency is 700 Hz; the pulse width of the positive pulse is 20%, and the ratio of the positive pulse to the negative pulse is 1: 1; the positive voltage and the negative voltage are both between 100V, the ratio of the positive voltage to the negative voltage is 3:1, and the processing time is 11 min.
d. Ceramic layer post-treatment:
the SiC-Al obtained in the step c2O3Cleaning the aluminum alloy element compounded with the ceramic layer by using deionized water, and then drying by using a hair dryer; finally obtaining the SiC-Al2O3An aluminum alloy workpiece compounded with a ceramic layer.
Example 2:
SiC-Al based on micro-arc oxidation2O3The preparation method of the coating is characterized by comprising the following steps: the method comprises the steps of matrix pretreatment, solution preparation, composite ceramic coating preparation and ceramic layer post-treatment, and the inner layer obtained by the method is Al2O3Ceramic layer and SiC ceramic layer as outer layerSiC-Al of the layer2O3The composite ceramic layer is 260 mu m thick;
the method specifically comprises the following steps:
a. matrix pretreatment:
firstly, an ultrasonic cleaner is adopted to carry out dust removal and oil removal cleaning on an aluminum alloy element in distilled water; then using H3PO4And Al (OH)3Reacting to obtain an aqueous solution treatment solution of aluminum dihydrogen phosphate sol, immersing the aluminum alloy element cleaned by an ultrasonic cleaner into the solution for 2min to remove oxide skin on the surface of the aluminum alloy, and cleaning the aluminum alloy element with distilled water after treatment; finally, performing surface alkaline washing and passivation on the aluminum alloy workpiece by soaking in NaOH solution with the concentration of 15g/L for 6 min; because the pH value of the solution formula for preparing the coating is about 9, in order to keep the solution characteristics, the aluminum alloy workpiece needs to be subjected to alkali cleaning and passivation.
b. Solution preparation:
KOH-Na is added into a stainless steel solution tank2SiO3- (NaPO3)6- Na2WO4Adding alkaline silica sol solution, water-soluble phenolic resin and nano SiC particles into distilled water solution which is the main component, and continuously stirring to fully dissolve all the components into the distilled water; wherein, KOH and Na2SiO3、(NaPO3)6、Na2WO4The concentration of (b) is respectively 7g/L, 11g/L, 8g/L and 10 g/L; the concentration of the alkaline silica sol solution is 60ml/L, the pH value of the alkaline silica sol solution is 8, and the alkaline silica sol solution contains SiO2 particles with the content of 30 percent or more and the particle size of less than 20 nm; the concentration of the water-soluble phenolic resin is 30 g/L; the concentration of the nano SiC particles is 20 g/L; distilled water high purity distilled water, i.e., water obtained by tertiary distillation or more.
Analytical pure reagents are adopted for each chemical component in the solution.
The stainless steel solution tank is made of conductive stainless steel, has sufficient cooling capacity, and can ensure that the temperature of the solution is kept below 30 ℃ in the preparation process.
c. Preparing a composite ceramic coating:
designing a special tool according to the structural characteristics of an aluminum alloy element (namely designing a clamping tool which can be suitable for micro-arc oxidation according to the specific shape of an aluminum alloy workpiece), clamping the aluminum alloy element on the anode of a high-voltage direct-current pulse power supply, placing the aluminum alloy element on the special tool in a stainless steel solution tank, and connecting the stainless steel solution tank with the cathode of a power supply, wherein the high-voltage direct-current pulse power supply is a special high-voltage direct-current pulse power supply with adjustable positive and negative voltages, adjustable positive and negative pulse ratios, adjustable positive and negative pulse widths and adjustable frequency; and the positive and negative voltages of the high-voltage direct-current pulse power supply are both above 700V.
Adjusting parameters of high-voltage direct-current pulse power supply and carrying out SiC-Al2O3The preparation of the composite ceramic coating needs to add positive and negative voltages simultaneously in the coating preparation process; the parameters of the high-voltage direct-current pulse power supply are as follows: the current density is 6A/dm2(ii) a The frequency is 1000 Hz; the pulse width of the positive pulse is 35%, and the ratio of the positive pulse to the negative pulse is 1: 2; the positive voltage and the negative voltage are both 400V, the ratio of the positive voltage to the negative voltage is 3:1, and the processing time is 21 min.
d. Ceramic layer post-treatment:
the SiC-Al obtained in the step c2O3Cleaning the aluminum alloy element compounded with the ceramic layer by using distilled water, and then drying by using a hair drier; finally obtaining the SiC-Al2O3An aluminum alloy workpiece compounded with a ceramic layer.
Example 3:
SiC-Al based on micro-arc oxidation2O3The preparation method of the coating is characterized by comprising the following steps: the method comprises the steps of matrix pretreatment, solution preparation, composite ceramic coating preparation and ceramic layer post-treatment, and the inner layer obtained by the method is Al2O3Ceramic layer, SiC-Al with SiC ceramic layer as outer layer2O3The composite ceramic layer is 400 microns thick;
the method specifically comprises the following steps:
a. matrix pretreatment:
firstly, an ultrasonic cleaner is adopted to carry out dust removal and oil removal cleaning on an aluminum alloy element in deionized water; then using H3PO4And Al (OH)3Reacting to obtain an aqueous solution treatment solution of aluminum dihydrogen phosphate sol, immersing the aluminum alloy element cleaned by an ultrasonic cleaner into the solution for 3min to remove oxide skin on the surface of the aluminum alloy, and cleaning the aluminum alloy element by deionized water after treatment; finally, performing surface alkaline washing and passivation on the aluminum alloy workpiece by soaking the aluminum alloy workpiece into NaOH solution with the concentration of 20g/L for 10 min; because the pH value of the solution formula for preparing the coating is about 9, in order to keep the solution characteristics, the aluminum alloy workpiece needs to be subjected to alkali cleaning and passivation.
b. Solution preparation:
KOH-Na is added into a stainless steel solution tank2SiO3- (NaPO3)6- Na2WO4Adding an alkaline silica sol solution, water-soluble phenolic resin and nano SiC particles into deionized water solution serving as a main component, and continuously stirring to fully dissolve all the components into the deionized water; wherein, KOH and Na2SiO3、(NaPO3)6、Na2WO4The concentration of (b) is respectively 8g/L, 16g/L, 12g/L and 15 g/L; the concentration of the alkaline silica sol solution is 90ml/L, the pH value of the alkaline silica sol solution is 10, and the alkaline silica sol solution contains SiO2 particles with the content of 30 percent or more and the particle size of less than 20 nm; the concentration of the water-soluble phenolic resin is 50 g/L; the concentration of the nano SiC particles is 30 g/L; the deionized water has a water quality of 10M omega cm @25 ℃ or above.
Analytical pure reagents are adopted for each chemical component in the solution.
The stainless steel solution tank is made of conductive stainless steel, has sufficient cooling capacity, and can ensure that the temperature of the solution is kept below 30 ℃ in the preparation process.
c. Preparing a composite ceramic coating:
designing a special tool according to the structural characteristics of an aluminum alloy element (namely designing a clamping tool which can be suitable for micro-arc oxidation according to the specific shape of an aluminum alloy workpiece), clamping the aluminum alloy element on the anode of a high-voltage direct-current pulse power supply, placing the aluminum alloy element on the special tool in a stainless steel solution tank, and connecting the stainless steel solution tank with the cathode of a power supply, wherein the high-voltage direct-current pulse power supply is a special high-voltage direct-current pulse power supply with adjustable positive and negative voltages, adjustable positive and negative pulse ratios, adjustable positive and negative pulse widths and adjustable frequency; and the positive and negative voltages of the high-voltage direct-current pulse power supply are both above 700V.
Adjusting parameters of high-voltage direct-current pulse power supply and carrying out SiC-Al2O3The preparation of the composite ceramic coating needs to add positive and negative voltages simultaneously in the coating preparation process; the parameters of the high-voltage direct-current pulse power supply are as follows: the current density is 8A/dm2(ii) a The frequency is 1200 Hz; the pulse width of the positive pulse is 50%, and the ratio of the positive pulse to the negative pulse is 2: 1; the positive voltage and the negative voltage are both between 700V, the ratio of the positive voltage to the negative voltage is 3:1, and the processing time is 30 min.
d. Ceramic layer post-treatment:
the SiC-Al obtained in the step c2O3Cleaning the aluminum alloy element compounded with the ceramic layer by using deionized water or distilled water, and then drying by using a hair dryer; finally obtaining the SiC-Al2O3An aluminum alloy workpiece compounded with a ceramic layer.
The composite coating prepared by the invention has high density (as shown in figure 1), high bonding strength between the ceramic layers, difficult falling, peeling and the like, good abrasion resistance, good corrosion resistance, heat insulation and ablation resistance; meanwhile, the invention only prepares two ceramic layers by a micro-arc oxidation process, thereby having high preparation efficiency and greatly saving preparation time and preparation cost.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. SiC-Al based on micro-arc oxidation2O3The preparation method of the coating is characterized by comprising the following steps: the method comprises the steps of matrix pretreatment, solution preparation, composite ceramic coating preparation and ceramic layer post-treatment, and the inner layer obtained by the method is Al2O3Ceramic layer, SiC-Al with SiC ceramic layer as outer layer2O3The ceramic layer is compounded, and the thickness of the ceramic layer is 30-400 mu m;
specifically, the method comprises the following steps:
the solution is prepared by the following steps: firstly, KOH-Na is added into a stainless steel solution tank2SiO3-(NaPO3)6- Na2WO4Adding an alkaline silica sol solution, water-soluble phenolic resin and nano SiC particles into deionized water solution serving as a main component, and continuously stirring to fully dissolve all the components into the deionized water to finally obtain mixed preparation liquid;
the composite ceramic coating is prepared by the following steps: designing a special tool according to the structural characteristics of an aluminum alloy element, clamping the aluminum alloy element on an anode of a high-voltage direct-current pulse power supply, placing the aluminum alloy element on the special tool in a stainless steel solution tank, immersing the special tool in a mixed preparation solution, connecting the stainless steel solution tank with a cathode of the high-voltage direct-current pulse power supply, and finally adjusting the parameters of the high-voltage direct-current pulse power supply to perform SiC-Al2O3The preparation of the composite ceramic coating needs to add positive and negative voltages simultaneously in the preparation process of the coating, and finally the SiC-Al is obtained2O3And compounding a ceramic layer.
2. The micro-arc oxidation-based SiC-Al according to claim 12O3The preparation method of the coating is characterized by comprising the following steps: the matrix pretreatment specifically comprises the following steps: and (3) carrying out dust removal, oil removal and cleaning on the aluminum alloy element by adopting an ultrasonic cleaning instrument, removing an oxide film, cleaning by using deionized water or distilled water after treatment, and then carrying out alkali cleaning.
3. The micro-arc oxidation-based SiC-Al according to claim 22O3The preparation method of the coating is characterized by comprising the following steps: the step of removing the oxidation film specifically comprises the following steps: can adopt H3PO4And Al (OH)3And (3) reacting to obtain an aqueous solution treatment solution of the aluminum dihydrogen phosphate sol, and immersing the aluminum alloy element cleaned by the ultrasonic cleaner into the solution for 2-3 min to remove oxide skin on the surface of the aluminum alloy.
4. The micro-arc oxidation-based SiC-Al according to claim 12O3The preparation method of the coating is characterized by comprising the following steps: the alkaline silica sol solution contains SiO with the content of 30 percent or more and the grain diameter of less than 20 nm2And (3) granules.
5. The micro-arc oxidation-based SiC-Al according to claim 12O3The preparation method of the coating is characterized by comprising the following steps: the concentration of the nano SiC particles can be 5-30 g/L.
6. The micro-arc oxidation-based SiC-Al according to claim 12O3The preparation method of the coating is characterized by comprising the following steps: the deionized water in the solution preparation process can be replaced by high-purity distilled water, and the high-purity distilled water is water obtained by three times of distillation or more.
7. The micro-arc oxidation-based SiC-Al according to claim 12O3The preparation method of the coating is characterized by comprising the following steps: the stainless steel solution tank is made of conductive stainless steel, has sufficient cooling capacity, and can ensure that the temperature of the solution is kept below 30 ℃ in the preparation process.
8. The micro-arc oxidation-based SiC-Al according to claim 12O3The preparation method of the coating is characterized by comprising the following steps: the technological parameters of the high-voltage direct-current pulse power supply in the preparation process of the composite ceramic coating are as follows: the current density can be 3-8A/dm2(ii) a The frequency can be 700-1200 Hz; the pulse width of the positive pulse can be 10-80%, and the ratio of the positive pulse to the negative pulse is 1:1 or 1:2 or 2: 1; the positive voltage and the negative voltage are both between 10V and 700V, the ratio of the positive voltage to the negative voltage is 3:1, and the processing time can be 10min to 30 min.
9. The micro-arc oxidation-based SiC-Al according to claim 12O3The preparation method of the coating is characterized in that: the ceramic layer post-treatment specifically comprises the following steps: and (3) washing the aluminum alloy element obtained after the preparation process of the composite ceramic coating by using deionized water or distilled water, and then drying by using a hair drier.
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