CN116351685B - Preparation process of aluminum alloy hub surface coating - Google Patents
Preparation process of aluminum alloy hub surface coating Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 239000011248 coating agent Substances 0.000 title claims abstract description 63
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 27
- 238000005507 spraying Methods 0.000 claims abstract description 17
- 230000007704 transition Effects 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000003980 solgel method Methods 0.000 claims abstract description 9
- 239000007921 spray Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 17
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 16
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 11
- 230000007062 hydrolysis Effects 0.000 claims description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 9
- 238000005728 strengthening Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 8
- 238000004519 manufacturing process Methods 0.000 claims 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 102
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 44
- 229910052593 corundum Inorganic materials 0.000 abstract description 32
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 32
- 238000002156 mixing Methods 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 4
- 239000000499 gel Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000000197 pyrolysis Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 1
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/002—Pretreatement
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0209—Multistage baking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
- B05D3/0272—After-treatment with ovens
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/20—Metallic substrate based on light metals
- B05D2202/25—Metallic substrate based on light metals based on Al
Abstract
The invention relates to the technical field of coatings, in particular to a preparation process of an aluminum alloy hub surface coating. A preparation process of an aluminum alloy hub surface coating comprises the following steps: spraying the modified transition layer by adopting a sol-gel method, and fully mixing ZrO2 sol and A12O3 sol in a molar ratio of 1:5 to prepare ZrO2/Al2O3 composite sol serving as a coating; evenly spraying on the surface of the hub by a spray gun, and drying and curing to form an even coating. Firstly, utilizing laser beams to generate high-energy density instant impact on the surface of an aluminum alloy hub so as to destroy the oxide film and the grain structure, lead the surface to be micro-deformed, generate densely distributed pits and increase the roughness of the surface; so as to form a modified transition layer on the surface of the hub and improve the binding force between the surface of the matrix and the coating.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a preparation process of an aluminum alloy hub surface coating.
Background
The surface coating process of the aluminum alloy hub mainly comprises spraying, electroplating and various sol-gel coatings; the sol-gel coating has the advantages of low cost, environmental friendliness, strong adjustability and the like, and is a novel coating technology with development prospect. The preparation method of the alcohol-based aluminum alloy hub paint disclosed in patent document CN105860833B adopts the particle nanocrystallization effect of the silicon-titanium composite sol to improve the mechanical properties of the coating material and realize the reinforcement and toughening of the final coating material.
Alumina is a ceramic material with high hardness, wear resistance and corrosion resistance, and the jelly alumina sol of the alumina has the characteristics of high adhesiveness, thixotropy, easy dispersibility and the like, and can be applied to surface coating materials to improve the wear resistance and corrosion resistance of the surface of a substrate; but due to the high expansion coefficient of the alumina sol (15.3X10 -6 ) Causing microcracks to easily appear in the heat treatment process, and leading corrosive solution to enter the matrix layerA convenient passage for the portion. The zirconia sol has the advantages of low expansion coefficient, high fracture toughness, high stability and the like; meanwhile, the zirconium dioxide sol has good optical transparency and refractive index adjustability, and can improve the aesthetic degree and decorative effect of the coating.
However, no research on preparing the surface coating of the metal matrix by compounding two sol has been disclosed in the prior literature at home and abroad, because the synergistic strengthening and toughening effects are still not obvious, and the specific process is still to be optimized and explored.
Disclosure of Invention
In order to overcome the defects that microcracks are easy to occur in the heat treatment process due to the high expansion coefficient of the alumina sol, and the synergistic strengthening and toughening effects of the ZrO2/A12O3F composite sol are still to be optimized, the technical problem of the invention is that: provides a preparation process of an aluminum alloy hub surface coating of ZrO2/Al2O3F composite sol.
A preparation process of an aluminum alloy hub surface coating comprises the following steps: spraying the modified transition layer by adopting a sol-gel method, and fully mixing ZrO2 sol and A12O3 sol in a molar ratio of 1:5 to prepare ZrO2 and A12O3 composite sol as a coating; evenly spraying on the surface of the hub by a spray gun, and drying and curing to form an even coating.
(1) Performing laser shock peening on the surface of the aluminum alloy hub by using an SGR-Extra-10 laser, wherein the output parameters of the laser are set as follows: the laser wavelength is 1024-1064nm, the pulse energy is 15-20J, the frequency is 0.1-0.2Hz, the spot diameter of the laser beam in the strengthening area is 4-4.25mm, the lap rate is 20-25%, and the impact frequency is not more than 2 times.
(2) Spraying the modified transition layer by adopting a sol-gel method, and fully mixing ZrO2 sol and Al2O3 sol according to a molar ratio of 1:5 to prepare ZrO2 and Al2O3 composite sol as a coating; uniformly spraying on the surface of the hub by a spray gun, and drying and curing to form a uniform coating; the method comprises the following specific steps:
s1) preparation of ZrO2 sol:
s101, putting zirconium oxychloride (ZrOCl 2.8H2O) into a water bath, adding dilute hydrochloric acid to adjust the pH value to 1.5-2.0, fully dissolving, heating the water bath to 80-90 ℃, and evaporating and concentrating at constant temperature;
s102, cooling the solution to room temperature, adding a proper amount of ethanol, and uniformly stirring to obtain zirconium oxychloride sol;
s103, putting the zirconium oxychloride sol into an oven, and pyrolyzing the zirconium oxychloride sol at 120-150 ℃ for 4-6H to decompose the zirconium oxychloride into ZrO2;
s104, treating the pyrolyzed sol by ultrasonic waves for 10-20min to uniformly disperse ZrO2 particles, thereby obtaining ZrO2 sol;
s2) preparation of alumina sol:
s201, dissolving aluminum isopropoxide (Zr (OC 4H 9) 4) in isopropanol, stirring at room temperature for 0.5H, and adding acetylacetone and aluminum isopropoxide into the mixed solution according to a molar ratio of 1:1;
s202, heating the mixed solution to 80 ℃ under stirring, keeping the temperature unchanged, and continuously stirring for 30 minutes to completely dissolve the aluminum isopropoxide.
S203, adding 1% dilute nitric acid for hydrolysis for 10 minutes, and continuously stirring in the hydrolysis process; cooling to room temperature after hydrolysis to obtain clear and transparent alumina sol;
s3) mixing ZrO2 sol and A12O3 sol according to a molar ratio of 1:5, and fully stirring for 20min by using a magnetic stirrer to uniformly mix the nano particles to prepare the composite sol.
(3) Drying the sprayed hub in a drying box at 100-110 ℃ for 15min to volatilize the solvent in the sol film, and carrying out polymerization reaction among sol particles to form a layer of compact gel coating;
(4) And then the hub is placed in a high-temperature tubular electric furnace at 250-300 ℃ for heat treatment for 2 hours, and the hub is heated to a certain temperature and kept for a certain time, so that organic substances in the gel coating are decomposed to generate an oxide network structure, and the hardness and the adhesive force of the coating are improved.
Further, the particle size of the colloidal particles of the Al2O3 sol is 50-60 nm; the particle size of colloidal particles of the Zr O2 sol is 6-10 nm.
The invention has the following advantages: 1. the laser beam is utilized to generate high-energy density instant impact on the surface of the aluminum alloy hub, so that the oxide film and the grain structure are damaged, the surface is slightly deformed, dense pits are generated, the surface roughness is increased, a modified transition layer is formed on the surface of the hub, and the binding force between the surface of a substrate and a coating is improved.
2. The nano-scale zirconium dioxide sol is obtained by a zirconium oxychloride pyrolysis method. The method fully dissolves zirconium hydroxide by hydrochloric acid, improves the stability and uniformity of sol, and then further purifies the sol by thermal decomposition, so that the size and shape of particles can be effectively refined, and the particle size is controlled below 10nm.
3. The purpose of preparing the composite sol is to utilize the synergistic effect of two different materials, most ZrO2 grains are inserted between grain boundaries of Al2O3 grains, the expansion of the Al2O3 grains in the heat treatment process is limited to a certain extent, the stress deformation caused by ZrO2 phase change also inhibits the growth of primary microcracks, and the hardness and crack resistance of the coating are improved.
Drawings
FIG. 1 is a diagram showing an exemplary calculation of diameter values for simulated geometric figures in accordance with the present invention.
FIG. 2 is an SEM image of the microstructure of a ZrO2/Al2O3 composite coating as shown in examples 1-3 according to the invention.
Detailed Description
The present invention now will be described more fully hereinafter with reference to the accompanying drawings, in which currently preferred embodiments of the invention are shown. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
A preparation process of an aluminum alloy hub surface coating comprises the following steps:
(1) Performing laser impact modification on the surface of the aluminum alloy hub by using an SGR-Extra-10 laser strengthening device, so as to form a modified transition layer on the surface of the hub; wherein the laser output parameters are set as: the laser wavelength is 1024-1064nm, the pulse energy is 15-20J, the frequency is 0.1-0.2Hz, the spot diameter of the laser beam in the strengthening area is 4-4.25mm, the lap joint rate is 20-25%, and the impact frequency is not more than 2 times;
laser impact modification: the laser impact modification is characterized in that a laser beam is utilized to generate instantaneous impact with high energy density on the surface of the aluminum alloy, so that compressive stress is generated on the surface, thereby damaging an oxide film and a grain structure, micro-deforming the surface, generating densely distributed pits and increasing the roughness of the surface; thereby forming a modified transition layer on the surface of the hub and improving the binding force between the surface of the matrix and the coating.
In the invention, a sol-gel method is adopted to prepare the composite coating; firstly, aluminum isopropoxide is taken as a precursor, dissolved with an alcohol agent of the aluminum isopropoxide, and then subjected to hydrolysis polycondensation reaction to form stable and transparent nanoscale alumina sol;
and secondly, obtaining the nano-scale zirconium dioxide sol by a zirconium oxychloride pyrolysis method. The method fully dissolves zirconium hydroxide by hydrochloric acid, improves the stability and uniformity of sol, and then further purifies the sol by thermal decomposition, so that the size and shape of particles can be effectively refined, and the particle size is controlled below 10nm.
(2) Spraying the modified transition layer by adopting a sol-gel method, and fully mixing ZrO2 sol and Al2O3 sol according to a molar ratio of 1:5 to prepare ZrO2/Al2O3 composite sol serving as a coating; uniformly spraying on the surface of the hub by a spray gun, and drying and curing to form a uniform coating; the method comprises the following specific steps:
s1) preparation of ZrO2 sol:
s101, putting zirconium oxychloride (ZrOC 12-8H 2O) into a water bath, adding dilute hydrochloric acid to adjust the pH value to 1.5-2.0, fully dissolving, heating the water bath to 80-90 ℃, and evaporating and concentrating at constant temperature;
s102, cooling the solution to room temperature, adding a proper amount of ethanol, and uniformly stirring to obtain zirconium oxychloride sol;
s103, putting the zirconium oxychloride sol into an oven, and pyrolyzing the zirconium oxychloride sol at 120-150 ℃ for 4-6H to decompose the zirconium oxychloride into ZrO2;
s104, treating the pyrolyzed sol by ultrasonic waves for 10-20min to uniformly disperse ZrO2 particles, thereby obtaining ZrO2 sol;
s2) preparation of alumina sol:
s201, dissolving aluminum isopropoxide (Zr (OC 4H 9) 4) in isopropanol, stirring at room temperature for 0.5H, and adding acetylacetone and aluminum isopropoxide into the mixed solution according to a molar ratio of 1:1;
s202, heating the mixed solution to 80 ℃ under stirring, keeping the temperature unchanged, and continuously stirring for 30 minutes to completely dissolve the aluminum isopropoxide.
S203, adding 1% dilute nitric acid for hydrolysis for 10 minutes, and continuously stirring in the hydrolysis process; cooling to room temperature after hydrolysis to obtain clear and transparent alumina sol;
s3) mixing ZrO2 sol and Al2O3 sol according to a molar ratio of 1:5, and fully stirring for 20min by using a magnetic stirrer to uniformly mix the nano particles to prepare the composite sol.
(3) Drying the sprayed hub in a drying box at 100-110 ℃ for 15min to volatilize the solvent in the sol film, and carrying out polymerization reaction among sol particles to form a layer of compact gel coating;
(4) And then the hub is placed in a high-temperature tubular electric furnace at 250-300 ℃ for heat treatment for 2 hours, and the hub is heated to a certain temperature and kept for a certain time, so that organic substances in the gel coating are decomposed to generate an oxide network structure, and the hardness and the adhesive force of the coating are improved.
Further, the particle size of the colloidal particles of the Al2O3 sol is 50-60 nm; the particle size of colloidal particles of the Zr O2 sol is 6-10 nm. The ZrO2/Al2O3 composite sol prepared by the process utilizes the synergistic effect of two different materials, and the alumina has high hardness and wear resistance; zirconium dioxide has the function of phase change toughening, and can resist crack growth; the grain size of the ZrO2 sol can be effectively controlled by a pyrolysis method, so that the mutual interpenetration effect of grains with different sizes on a physical microcosmic level can be realized, a compact ZrO2/Al2O3 composite grain network structure is generated, and the hardness and the crack resistance of the coating are improved.
According to the existing ZrO2 preparation process, the grain sizes of ZrO2 formed by the subsequent heat treatment in different preparation processes are different. The ZrO2 sol is prepared first by a pyrolysis method by referring to the prior researches (hydrolysis method, high-temperature calcination method and the like are also available).
In addition, as shown in FIG. 1, the particle size of ZrO2 sol obtained by the pyrolysis method was very well adapted to the particle size of Al2O3 sol by calculation of the diameter of the simulated geometric figure. The side surface of the catalyst reveals that the ZrO2 sol and the Al2O3 sol prepared by the pyrolysis method selected in the step (2) have optimal suitability.
Example 1
A preparation process of an aluminum alloy hub surface coating comprises the following steps: (1) Performing laser impact modification on the surface of the aluminum alloy hub by using an SGR-Extra-10 laser, so as to form a modified transition layer on the surface of the hub; wherein the laser output parameters are set as: the laser wavelength is 1064nm, the pulse energy is 20J, the frequency is 0.2Hz, the spot diameter of the laser beam in the strengthening area is 4.25mm, the lap rate is 25%, and the impact times are 2 times;
(2) Spraying a modified transition layer on the surface of the hub by adopting a sol-gel method, wherein the mol ratio of ZrO2 sol to Al2O3 sol is 1:8, fully mixing to prepare ZrO2/Al2O3 composite sol serving as a coating; uniformly spraying on the surface of the hub through a spray gun to form a uniform coating;
(3) Drying the sprayed hub in a drying box at 110 ℃ for 15min to volatilize the solvent in the sol film, and carrying out polymerization reaction among sol particles to form a layer of compact gel coating;
(4) And then placing the hub in a 300 ℃ high-temperature tubular electric furnace for heat treatment for 2 hours, heating to a certain temperature and keeping for a certain time, and discharging to finish the preparation of the ZrO2/Al2O3 composite coating on the surface of the hub.
Example 2
A preparation process of an aluminum alloy hub surface coating comprises the following steps: (1) Performing laser impact modification on the surface of the aluminum alloy hub by using an SGR-Extra-10 laser, so as to form a modified transition layer on the surface of the hub; wherein the laser output parameters are set as: the laser wavelength is 1064nm, the pulse energy is 20J, the frequency is 0.2Hz, the spot diameter of the laser beam in the strengthening area is 4.25mm, the lap rate is 25%, and the impact times are 2 times;
(2) Spraying a modified transition layer on the surface of the hub by adopting a sol-gel method, wherein the mol ratio of ZrO2 sol to Al2O3 sol is 1:6, fully mixing to prepare ZrO2/Al2O3 composite sol serving as a coating; uniformly spraying on the surface of the hub through a spray gun to form a uniform coating;
(3) Drying the sprayed hub in a drying box at 110 ℃ for 15min to volatilize the solvent in the sol film, and carrying out polymerization reaction among sol particles to form a layer of compact gel coating;
(4) And then placing the hub in a 300 ℃ high-temperature tubular electric furnace for heat treatment for 2 hours, heating to a certain temperature and keeping for a certain time, and discharging to finish the preparation of the ZrO2/Al2O3 composite coating on the surface of the hub.
Example 3
A preparation process of an aluminum alloy hub surface coating comprises the following steps: (1) Performing laser impact modification on the surface of the aluminum alloy hub by using an SGR-Extra-10 laser, so as to form a modified transition layer on the surface of the hub; wherein the laser output parameters are set as: the laser wavelength is 1064nm, the pulse energy is 20J, the frequency is 0.2Hz, the spot diameter of the laser beam in the strengthening area is 4.25mm, the lap rate is 25%, and the impact times are 2 times;
(2) Spraying a modified transition layer on the surface of the hub by adopting a sol-gel method, wherein the mol ratio of ZrO2 sol to Al2O3 sol is 1:4, fully mixing to prepare ZrO2/Al2O3 composite sol serving as a coating; uniformly spraying on the surface of the hub through a spray gun to form a uniform coating;
(3) Drying the sprayed hub in a drying box at 110 ℃ for 15min to volatilize the solvent in the sol film, and carrying out polymerization reaction among sol particles to form a layer of compact gel coating;
(4) And then placing the hub in a 300 ℃ high-temperature tubular electric furnace for heat treatment for 2 hours, heating to a certain temperature and keeping for a certain time, and discharging to finish the preparation of the ZrO2/Al2O3 composite coating on the surface of the hub.
Test:
test 1: electron Microscope (SEM) scanning was performed on the surface microstructure of the sample coating (ZrO 2/Al2O3 composite coating on the surface of the aluminum alloy hub) of the same aluminum alloy material under the same environment of each example, to obtain an image as shown in fig. 2.
In addition, in the observation of the electron microscope scanning image of each example, the number of microcracks per unit area was also counted and evaluated simply, and the data shown in table 3 below were obtained.
Table 3: grain density and microcrack count statistics for different ZrO2/Al2O3 mole ratios in three examples
| Examples | ZrO2/Al2O3 molar ratio | Density (g/cm 3) | Number of microcracks (/ μm) |
| Example 1 | 1:8 | 2.08 | 0.43 |
| Example 2 | 1:6 | 2.46 | 0.18 |
| EXAMPLE 3 | 1:4 | 2.82 | 0.01 |
As can be seen from the SEM micrographs of FIG. 2, examples 1 (a), 2 (b) and 3 (c) show that the ZrO2/Al2O3 grain structure gradually becomes full, and FIG. 2 (c) shows a small amount of ZrO2 agglomerates, which indicates the network structure density of the interpenetration of different grains to reach a saturated state; related studies have also shown that when agglomerates exceed a certain critical size, microscopic defects can be created in the composite material, which can significantly reduce the strength and crack resistance of the composite material.
On the other hand, as is clear from FIG. 2- (c), most of ZrO2 grains are intercalated between grain boundaries of A12O3 grains, expansion of Al2O3 grains during heat treatment is limited to a certain extent, and stress deformation caused by ZrO2 phase transition also inhibits growth of primary microcracks. The effect is also shown in Table 3 of observation statistics in a plurality of scanning electron microscope pictures, wherein the ZrO2/Al2O3 grains are dense, and the data in the microcrack number statistics table are mutually verified. Test 2:
test for sample coatings (ZrO 2/Al2O3 composite coatings on aluminum alloy hub surfaces) of the same aluminum alloy materials under the same environment of each example, the hardness performance-Vickers hardness tested by a 2kg load was: 2600.+ -.160 HV. The results show that the hardness of the composite coating is also much higher than the level of the relevant Al2O3 coating.
In summary, in step (2) in any embodiment, the ZrO2 sol and the a12O3 sol are uniformly mixed in a molar ratio of 1:5 to achieve the best effect, and the combination of the two has the characteristics of high hardness, high strength and high toughness of the alumina, and also achieves the crack resistance, further improves the corrosion resistance, and makes up the defect of easy crack occurrence of a single coating.
While the present disclosure has been shown and described with reference to certain exemplary embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present disclosure as defined by the appended claims and their equivalents. The scope of the disclosure should, therefore, not be limited to the above-described embodiments, but should be determined not only by the following claims, but also by the equivalents of the following claims.
Claims (3)
1. A preparation process of an aluminum alloy hub surface coating comprises the following steps:
(1) Performing laser impact modification on the surface of the aluminum alloy hub by using a laser, so as to form a modified transition layer on the surface of the hub;
(2) Spraying a modified transition layer on the surface of the hub by adopting a sol-gel method, and using ZrO 2 Sol and Al 2 O 3 The sol is fully mixed in a certain molar ratio to prepare ZrO 2 /Al 2 O 3 The composite sol is used as a coating; uniformly spraying on the surface of the hub through a spray gun to form a uniform coating;
(3) Drying the sprayed hub in a drying box at 100-110 ℃ for 15min to volatilize the solvent in the sol film, and carrying out polymerization reaction among sol particles to form a layer of compact gel coating;
(4) Then placing the hub in a high-temperature tubular electric furnace at 250-300 ℃ for heat treatment for 2h, heating to a certain temperature and maintaining for a certain time, and discharging the aluminum alloy hub to finish ZrO on the surface of the aluminum alloy hub 2 /Al 2 O 3 Preparing a composite coating;
the specific process flow of the step (2) is as follows:
S1)ZrO 2 preparation of sol:
s101, zirconium oxychloride ZrOCl 2 ·8H 2 Placing O in a water bath, adding dilute hydrochloric acid to adjust the pH value to 1.5-2.0, fully dissolving, heating the water bath to 80-90 ℃, and evaporating and concentrating at constant temperature;
s102, cooling the solution to room temperature, adding a proper amount of ethanol, and uniformly stirring to obtain zirconium oxychloride sol;
s103, putting the zirconium oxychloride sol into an oven, and pyrolyzing for 4-6 hours at the temperature of 120-150 ℃ to decompose the zirconium oxychloride into ZrO 2 ；
S104, treating the pyrolyzed sol by ultrasonic waves for 10-20min to enable ZrO 2 Uniformly dispersing the particles to obtain ZrO 2 Sol;
S2) Al 2 O 3 preparation of sol:
s201, dissolving aluminum isopropoxide in isopropanol, stirring at room temperature for 0.5h, and adding acetylacetone and aluminum isopropoxide into the mixed solution according to a molar ratio of 1:1;
s202, heating the mixed solution to 80 ℃ under stirring, keeping the temperature unchanged, and continuously stirring for 30 minutes to completely dissolve aluminum isopropoxide;
s203, adding 1% dilute nitric acid for hydrolysis for 10 minutes, and continuously stirring in the hydrolysis process; cooling to room temperature after hydrolysis to obtain clear and transparent Al 2 O 3 Sol;
s3) ZrO is reacted with 2 Sol and Al 2 O 3 The sol is uniformly mixed according to the mol ratio of 1:4-1:6, and is fully stirred for 20min by a magnetic stirrer, so that the nano particles are uniformly mixed, and the ZrO is prepared 2 /Al 2 O 3 Compounding sol;
the Al is 2 O 3 The particle size of colloidal particles of the sol is 50-60 nm; the ZrO 2 The particle size of colloidal particles of the sol is 6-10 nm.
2. The process for preparing the aluminum alloy hub surface coating according to claim 1, which is characterized in that: the output parameters of the laser in the step (1) are set as follows: the laser wavelength is 1024-1064nm, the pulse energy is 20-30J, the frequency is 0.1-0.2Hz, the spot diameter of the laser beam in the strengthening area is 4-4.25mm, the lap rate is 20-25%, and the impact frequency is not more than 2 times.
3. The process for preparing the aluminum alloy hub surface coating according to claim 1, which is characterized in that: zrO in the step S3) 2 Sol and Al 2 O 3 The sol was homogeneously mixed in a molar ratio of 1:5.
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| CN115637398A (en) * | 2022-10-10 | 2023-01-24 | 集美大学 | Aluminum alloy hub and surface layer high-energy composite modification method thereof |
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