CN113957439A - Al for titanium alloy2O3Mullite gradient anti-oxidation coating and preparation method thereof - Google Patents
Al for titanium alloy2O3Mullite gradient anti-oxidation coating and preparation method thereof Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 69
- 238000000576 coating method Methods 0.000 title claims abstract description 69
- 230000003064 anti-oxidating effect Effects 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 239000010936 titanium Substances 0.000 title claims abstract description 13
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 13
- 229910001069 Ti alloy Inorganic materials 0.000 claims abstract description 126
- 239000000758 substrate Substances 0.000 claims abstract description 80
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 64
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000011888 foil Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000011159 matrix material Substances 0.000 claims abstract description 23
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 23
- 230000003647 oxidation Effects 0.000 claims abstract description 22
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 18
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 18
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 17
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 17
- 238000000227 grinding Methods 0.000 claims abstract description 15
- 238000004544 sputter deposition Methods 0.000 claims abstract description 15
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 12
- 238000005498 polishing Methods 0.000 claims abstract description 10
- 238000007747 plating Methods 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 14
- 238000007605 air drying Methods 0.000 claims description 13
- 239000000956 alloy Substances 0.000 claims description 11
- 229910052782 aluminium Inorganic materials 0.000 claims description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 10
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 239000013077 target material Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 35
- 238000006243 chemical reaction Methods 0.000 description 11
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 230000004584 weight gain Effects 0.000 description 2
- 235000019786 weight gain Nutrition 0.000 description 2
- 235000015842 Hesperis Nutrition 0.000 description 1
- 235000012633 Iberis amara Nutrition 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
- C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
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Abstract
Al for titanium alloy of the invention2O3-mullite gradient anti-oxidation coating and a preparation method thereof, wherein the preparation method comprises the following steps: firstly, grinding a titanium alloy matrix, then polishing and ultrasonically cleaning; drying the cleaned titanium alloy matrix in a blast drying oven; uniformly paving a layer of Al foil on the surface of the dried titanium alloy; placing the titanium alloy substrate coated with the Al foil in a vacuum furnace, and carrying out vacuum heat treatment at high temperature to completely melt the titanium alloy substrate so as to uniformly coat the titanium alloy substrate on the surface of the titanium alloy substrate; titanium alloyOxidizing the substrate at high temperature to form a layer of Al on the surface2O3(ii) a Placing the substrate on a sample stage of a magnetron sputtering instrument, and mounting SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer; heat treating the titanium alloy substrate in air to obtain SiO2And Al2O3Reacting to obtain mullite and Al2O3-mullite gradient anti-oxidation coating. The invention can improve the oxidation resistance of the titanium alloy matrix.
Description
Technical Field
The invention belongs to the technical field of surface modification of metal materials, and particularly relates to Al for a titanium alloy2O3_A mullite gradient anti-oxidation coating and a preparation method thereof.
Background
The titanium alloy is an important structural metal, has high strength and good corrosion resistance, and is mainly used for manufacturing parts of an air compressor of an aircraft engine, structural parts of rockets, missiles and high-speed airplanes. However, various performances of the titanium alloy are sharply reduced after the titanium alloy is oxidized, so that the research on the oxidation resistance of the titanium alloy is important for the application of the titanium alloy.
Al is an active metal and is easily oxidized to form compact Al2O3The oxide layer is used as a coating material to protect the substrate from being oxidized and has good combination with the titanium alloy. But Al produced2O3The oxide layer is usually thin and has weak bonding force with the substrate, so that the single layer of Al2O3The oxidation resistant layer is difficult to meet the practical use requirements. Mullite is a high-quality high-temperature refractory material, and Al is added2O3The titanium alloy is compounded with mullite to be used as an anti-oxidation coating of a titanium alloy base material, so that the problem of poor binding force between the coating and a substrate can be solved; thereby adding Al2O3The anti-oxidation coating and mullite are prepared into a gradient structure, so that the thickness of an anti-oxidation layer can be increased, and the oxidation resistance of a metal matrix is effectively improved.
Disclosure of Invention
The invention aims to provide Al for titanium alloy2O3_Mullite gradient anti-oxidation coating and preparation thereofA method. The method comprises the steps of using a titanium alloy as a substrate, paving a layer of aluminum foil on the surface of the titanium alloy, melting the aluminum foil in a vacuum heat treatment mode, uniformly coating the aluminum foil on the surface to form a metal Al layer, and oxidizing at high temperature to obtain Al2O3A layer; reuse of SiO2As a target material, Al is added by magnetron sputtering method2O3Coating a layer of SiO on the surface of the layer2(ii) a Finally, heat-treating it at high temperature to obtain Al2O3And SiO of the surface2After the reaction, mullite (3 Al) is generated2O3·2SiO2) To obtain Al2O3_The mullite gradient anti-oxidation coating improves the anti-oxidation performance of the titanium alloy matrix.
The invention is realized by adopting the following technical scheme:
al for titanium alloy2O3_The preparation method of the mullite gradient anti-oxidation coating comprises the following steps:
step 1, firstly grinding a titanium alloy substrate, and then polishing;
step 3, drying the titanium alloy matrix obtained in the step 2 in a forced air drying oven;
step 4, uniformly paving a layer of Al foil on the surface of the titanium alloy obtained in the step 3;
step 5, placing the titanium alloy substrate coated with the Al foil in the step 4 in a vacuum furnace, and performing vacuum heat treatment at high temperature to completely melt the titanium alloy substrate so as to uniformly coat the titanium alloy substrate on the surface;
step 6, oxidizing the titanium alloy substrate obtained in the step 5 at high temperature to generate a layer of Al on the surface of the titanium alloy substrate2O3；
Step 7, placing the substrate obtained in the step 6 on a sample table of a magnetron sputtering instrument, and installing SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer;
The invention is further improved in that 500#, 1000#, 1500#, 2000# sand paper is sequentially ground in the step 1, and polishing treatment is carried out by using the grinding paste.
The further improvement of the invention is that in the step 2, the ultrasonic cleaning time is 10-15 min.
The further improvement of the invention is that in the step 3, the drying temperature of the titanium alloy substrate in the blast drying oven is 70-100 ℃, and the drying time is 40-60 min.
The further improvement of the invention is that in the step 4, the thickness of the aluminum foil paved on the surface of the titanium alloy is 30-200 μm.
The invention has the further improvement that in the step 5, the temperature for vacuum heat treatment at high temperature is 750-900 ℃ and the time is 0.5-1 h.
The further improvement of the invention is that in the step 6, the temperature for carrying out the oxidation treatment at high temperature is 450-550 ℃, and the time is 1-2 h.
A further development of the invention is that, in step 7, SiO2The purity of the target material is 99.99 percent, and the background vacuum degree is about 5 multiplied by 10-4Pa, deposition temperature of 500-600 ℃, and air pressure of the cavity of 10-3～10-2Pa, a bias voltage of 250-350V, an argon flow of 10-20 mL/min, and a continuous sputtering time of 80-200 min to obtain SiO2And (3) a layer.
The further improvement of the invention is that in step 8, the temperature of oxidation in air is 900-1100 ℃, and the time is 2-3 h, so that Al is obtained2O3_Mullite gradient anti-oxidation coating.
Al for titanium alloy2O3_The mullite gradient anti-oxidation coating is prepared by the preparation method.
The invention has at least the following beneficial technical effects:
1. the invention provides Al for titanium alloy2O3_Mullite gradient anti-oxidation coatingLayer and method for producing the same, Al being obtained by means of melt coating and oxidation2O3Coating a layer of SiO by magnetron sputtering2And finally Al after high-temperature heat treatment2O3And SiO of the surface2Al is obtained after the reaction2O3_Mullite gradient anti-oxidation coating. The preparation method skillfully utilizes the oxidability of metal Al and the method of artificially heating aluminosilicate to prepare mullite, so that the whole preparation process is simpler and more time-saving, and has wide application prospect.
2. The invention provides Al for titanium alloy2O3_The mullite gradient anti-oxidation coating and the preparation method thereof adopt a mode of combining coating infiltration, magnetron sputtering and in-situ reaction to prepare the anti-oxidation coating, have stronger bonding force with a matrix, and obtain a more compact coating.
3. Al prepared by the invention2O3_The mullite gradient anti-oxidation coating not only has obvious layered structure, but also utilizes Al2O3Dense protective layer and mullite phase (3 Al)2O3·2SiO2) The metal matrix is protected by the high temperature stability of the alloy, so that more excellent high temperature oxidation resistance is obtained. Compared with single-layer Al2O3Coating of Al2O3_The oxidation weight gain of the mullite gradient anti-oxidation coating at 800 ℃ is reduced by more than 2 times, and the oxidation resistance of the mullite gradient anti-oxidation coating is greatly improved.
Drawings
FIG. 1 shows Al prepared according to the present invention2O3_XRD pattern of mullite gradient anti-oxidation coating;
FIG. 2 shows Al prepared by the present invention2O3_SEM image of the cross section of the surface of the mullite gradient anti-oxidation coating;
FIG. 3 shows Al prepared by the present invention2O3_The oxidation weight increasing graph of the mullite gradient anti-oxidation coating at 800 ℃.
Detailed Description
The present invention will be described in detail with reference to the following embodiments,
the invention relates to Al2O3_The mullite gradient anti-oxidation coating and the preparation method thereof are implemented according to the following steps:
step 1, sequentially mechanically grinding a titanium alloy matrix by using 500#, 1000#, 1500#, 2000# abrasive paper, and polishing by using a grinding paste;
step 3, drying the titanium alloy substrate obtained in the step 2 in a forced air drying oven, wherein the drying temperature of the titanium alloy substrate in the forced air drying oven is 70-100 ℃, and the drying time is 40-60 min;
step 4, uniformly paving a layer of Al foil on the surface of the titanium alloy obtained in the step 3, wherein the thickness of the aluminum foil paved on the surface of the titanium alloy is 30-200 mu m;
step 5, placing the titanium alloy substrate coated with the Al foil in the step 4 in a vacuum furnace, performing vacuum heat treatment at high temperature to completely melt the titanium alloy substrate, uniformly coating the titanium alloy substrate on the surface of the titanium alloy substrate, and performing vacuum heat treatment at high temperature at 750-900 ℃ for 0.5-1 h;
step 6, oxidizing the titanium alloy substrate obtained in the step 5 at high temperature to generate a layer of Al on the surface of the titanium alloy substrate2O3The temperature for carrying out oxidation treatment at high temperature is 450-550 ℃, and the time is 1-2 h;
step 7, placing the substrate obtained in the step 6 on a sample table of a magnetron sputtering instrument, and installing SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer; SiO 22The purity of the target material is 99.99 percent, and the background vacuum degree is about 5 multiplied by 10-4Pa, deposition temperature of 500-600 ℃, and air pressure of the cavity of 10-3～10-2Pa, a bias voltage of 250-350V, an argon flow of 10-20 mL/min, and a continuous sputtering time of 80-200 min to obtain SiO2A layer;
Example 1
Step 1, mechanically grinding a titanium alloy matrix by using 500# abrasive paper, and polishing by using a grinding paste;
step 3, drying the titanium alloy substrate obtained in the step 2 in a forced air drying oven, wherein the drying temperature of the titanium alloy substrate in the forced air drying oven is 70 ℃, and the drying time is 40 min;
step 4, uniformly paving a layer of Al foil on the surface of the titanium alloy obtained in the step 3, wherein the thickness of the aluminum foil paved on the surface of the titanium alloy is 30 micrometers;
step 5, placing the titanium alloy substrate coated with the Al foil in the step 4 in a vacuum furnace, performing vacuum heat treatment at high temperature to completely melt the titanium alloy substrate, uniformly coating the titanium alloy substrate on the surface of the titanium alloy substrate, and performing vacuum heat treatment at high temperature at 750 ℃ for 0.5 h;
step 6, oxidizing the titanium alloy substrate obtained in the step 5 at high temperature to generate a layer of Al on the surface of the titanium alloy substrate2O3The temperature for oxidation treatment at high temperature is 450 ℃ and the time is 1 h;
step 7, placing the substrate obtained in the step 6 on a sample table of a magnetron sputtering instrument, and installing SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer; SiO 22The purity of the target material is 99.99 percent, and the background vacuum degree is about 5 multiplied by 10-4Pa, deposition temperature 500 deg.C, and chamber pressure 10 deg.C-3Pa, the bias voltage is 250V, the argon flow is 10mL/min, and the continuous sputtering time is 80min to obtain SiO2A layer;
Example 2
Step 1, mechanically grinding a titanium alloy matrix by using No. 1000 abrasive paper, and polishing by using a grinding paste;
step 3, drying the titanium alloy substrate obtained in the step 2 in a forced air drying oven, wherein the drying temperature of the titanium alloy substrate in the forced air drying oven is 80 ℃, and the drying time is 45 min;
step 4, uniformly paving a layer of Al foil on the surface of the titanium alloy obtained in the step 3, wherein the thickness of the aluminum foil paved on the surface of the titanium alloy is 90 micrometers;
step 5, placing the titanium alloy substrate coated with the Al foil in the step 4 in a vacuum furnace, performing vacuum heat treatment at high temperature to completely melt the titanium alloy substrate, uniformly coating the titanium alloy substrate on the surface of the titanium alloy substrate, and performing vacuum heat treatment at high temperature at 800 ℃ for 0.6 h;
step 6, oxidizing the titanium alloy substrate obtained in the step 5 at high temperature to generate a layer of Al on the surface of the titanium alloy substrate2O3The temperature for carrying out oxidation treatment at high temperature is 480 ℃, and the time is 1.3 h;
step 7, placing the substrate obtained in the step 6 on a sample table of a magnetron sputtering instrument, and installing SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer; SiO 22The purity of the target material is 99.99 percent, and the background vacuum degree is about 5 multiplied by 10-4Pa, deposition temperature 530 deg.C, and chamber pressure 10 deg.C-3Pa, the bias voltage is 280V, the argon flow is 13mL/min, and the continuous sputtering time is 120min to obtain SiO2A layer;
Example 3
Step 1, mechanically grinding a titanium alloy matrix by using No. 1500 sand paper, and polishing by using a grinding paste;
step 3, drying the titanium alloy substrate obtained in the step 2 in a forced air drying oven, wherein the drying temperature of the titanium alloy substrate in the forced air drying oven is 90 ℃, and the drying time is 55 min;
step 4, uniformly paving a layer of Al foil on the surface of the titanium alloy obtained in the step 3, wherein the thickness of the aluminum foil paved on the surface of the titanium alloy is 140 micrometers;
step 5, placing the titanium alloy substrate coated with the Al foil in the step 4 in a vacuum furnace, performing vacuum heat treatment at high temperature to completely melt the titanium alloy substrate, uniformly coating the titanium alloy substrate on the surface of the titanium alloy substrate, and performing vacuum heat treatment at high temperature for 0.8h at 850 ℃;
step 6, oxidizing the titanium alloy substrate obtained in the step 5 at high temperature to generate a layer of Al on the surface of the titanium alloy substrate2O3The temperature for oxidation treatment at high temperature is 520 ℃, and the time is 1.7 h;
step 7, placing the substrate obtained in the step 6 on a sample table of a magnetron sputtering instrument, and installing SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer; SiO 22The purity of the target material is 99.99 percent, and the background vacuum degree is about 5 multiplied by 10-4Pa, deposition temperature of 570 ℃, and chamber pressure of 10 DEG C-2Pa, bias voltage of 320V, argon flow of 17mL/min, and continuous sputtering time of 160min to obtain SiO2A layer;
Example 4
Step 1, mechanically grinding a titanium alloy matrix by using No. 2000 abrasive paper, and polishing by using a grinding paste;
step 3, drying the titanium alloy substrate obtained in the step 2 in a forced air drying oven, wherein the drying temperature of the titanium alloy substrate in the forced air drying oven is 100 ℃, and the drying time is 60 min;
step 4, uniformly paving a layer of Al foil on the surface of the titanium alloy obtained in the step 3, wherein the thickness of the aluminum foil paved on the surface of the titanium alloy is 200 mu m;
step 5, placing the titanium alloy substrate coated with the Al foil in the step 4 in a vacuum furnace, performing vacuum heat treatment at high temperature to completely melt the titanium alloy substrate, uniformly coating the titanium alloy substrate on the surface of the titanium alloy substrate, and performing vacuum heat treatment at high temperature for 1 hour at 900 ℃;
step 6, oxidizing the titanium alloy substrate obtained in the step 5 at high temperature to generate a layer of Al on the surface of the titanium alloy substrate2O3The temperature for oxidation treatment at high temperature is 550 ℃ for 2 h;
step 7, placing the substrate obtained in the step 6 on a sample table of a magnetron sputtering instrument, and installing SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer; SiO 22The purity of the target material is 99.99 percent, and the background vacuum degree is about 5 multiplied by 10-4Pa, deposition temperature of 600 deg.C, and chamber pressure of 10 deg.C-2Pa, bias voltage of 350V, argon flow of 20mL/min, and continuous sputtering time of 200min to obtain SiO2A layer;
The present invention providesAl for titanium alloy2O3_The mullite gradient anti-oxidation coating is prepared by combining coating infiltration, magnetron sputtering and in-situ reaction, and not only utilizes the active chemical property of Al and the formed Al2O3The oxidation resistance of the titanium alloy matrix is improved by the compact protective layer; mullite phase (3 Al) generated by in-situ reaction at the same time2O3·2SiO2) The high-temperature stability is better; and the bonding force between the coating and the substrate is stronger, and the obtained coating is more compact.
By Al2O3_The XRD pattern of the mullite gradient anti-oxidation coating can be seen that Al is removed from the coating2O3And in addition to mullite, a small amount of SiO is present2No other impurities exist, the overall reaction is complete, and the coating performance is good, as shown in fig. 1; by Al2O3_SEM picture of the cross section of the mullite gradient anti-oxidation coating can show that the coating has high melting degree, the surface of the coating is uniform and compact, no obvious defect exists, and all layers of the composite coating are tightly combined and well combined with the matrix, as shown in figure 2.
FIG. 3 shows Al prepared by the present invention2O3_The oxidation weight increase of the mullite gradient anti-oxidation coating at 800 ℃ is gradually gentle as shown in the figure. Compared with single-layer Al2O3Coating of Al2O3_The oxidation weight gain of the mullite gradient anti-oxidation coating at 800 ℃ is reduced by more than 2 times, and the oxidation resistance of the mullite gradient anti-oxidation coating is greatly improved.
Claims (10)
1. Al for titanium alloy2O3The preparation method of the mullite gradient anti-oxidation coating is characterized by comprising the following steps:
step 1, firstly grinding a titanium alloy substrate, and then polishing;
step 2, carrying out ultrasonic cleaning on the titanium alloy matrix obtained in the step 1 by sequentially using absolute ethyl alcohol and deionized water;
step 3, drying the titanium alloy matrix obtained in the step 2 in a forced air drying oven;
step 4, uniformly paving a layer of Al foil on the surface of the titanium alloy obtained in the step 3;
step 5, placing the titanium alloy substrate coated with the Al foil in the step 4 in a vacuum furnace, and performing vacuum heat treatment at high temperature to completely melt the titanium alloy substrate so as to uniformly coat the titanium alloy substrate on the surface;
step 6, oxidizing the titanium alloy substrate obtained in the step 5 at high temperature to generate a layer of Al on the surface of the titanium alloy substrate2O3；
Step 7, placing the substrate obtained in the step 6 on a sample table of a magnetron sputtering instrument, and installing SiO on a target base2Target, plating SiO on the surface of titanium alloy by DC sputtering2A layer;
step 8, carrying out heat treatment on the titanium alloy substrate obtained in the step 7 in air to obtain SiO2And Al2O3Reacting to obtain mullite and Al2O3-mullite gradient anti-oxidation coating.
2. Al for titanium alloy according to claim 12O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that the 500#, 1000#, 1500#, 2000# sand paper is sequentially polished in the step 1, and polishing treatment is carried out by using a grinding paste.
3. Al for titanium alloy according to claim 12O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that in the step 2, the ultrasonic cleaning time is 10-15 min.
4. Al for titanium alloy according to claim 12O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that in the step 3, the drying temperature of the titanium alloy substrate in a forced air drying oven is 70-100 ℃, and the drying time is 40-60 min.
5. The method of claim 1Al for titanium alloy2O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that in the step 4, the thickness of the aluminum foil paved on the surface of the titanium alloy is 30-200 mu m.
6. Al for titanium alloy according to claim 12O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that in the step 5, the temperature for vacuum heat treatment at high temperature is 750-900 ℃, and the time is 0.5-1 h.
7. Al for titanium alloy according to claim 12O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that in the step 6, the temperature for oxidation treatment at high temperature is 450-550 ℃, and the time is 1-2 hours.
8. Al for titanium alloy according to claim 12O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that in the step 7, SiO2The purity of the target material is 99.99 percent, and the background vacuum degree is about 5 multiplied by 10-4Pa, deposition temperature of 500-600 ℃, and air pressure of the cavity of 10-3～10-2Pa, a bias voltage of 250-350V, an argon flow of 10-20 mL/min, and a continuous sputtering time of 80-200 min to obtain SiO2And (3) a layer.
9. Al for titanium alloy according to claim 12O3The preparation method of the mullite gradient anti-oxidation coating is characterized in that in the step 8, the temperature of oxidation in the air is 900-1100 ℃, and the time is 2-3 h, so that Al is obtained2O3-mullite gradient anti-oxidation coating.
10. Al for titanium alloy2O3-a mullite gradient anti-oxidation coating, characterized in that it is prepared by the preparation method as claimed in any one of claims 1 to 9.
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| US5763008A (en) * | 1995-01-06 | 1998-06-09 | Trustees Of Boston University | Chemical vapor deposition of mullite coatings |
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| US20060093833A1 (en) * | 2002-03-05 | 2006-05-04 | Dirk Meyer | Components having crystalline coatings of the aluminum oxide/silicon oxide system and method for the production thereof |
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| CN102002673A (en) * | 2010-09-17 | 2011-04-06 | 陕西师范大学 | Preparation method of nanocrystalline silicon-aluminum oxide/silicon oxide thermoelectric film material |
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| US3073770A (en) * | 1961-04-24 | 1963-01-15 | Bell Telephone Labor Inc | Mullite synthesis |
| US5763008A (en) * | 1995-01-06 | 1998-06-09 | Trustees Of Boston University | Chemical vapor deposition of mullite coatings |
| US20060093833A1 (en) * | 2002-03-05 | 2006-05-04 | Dirk Meyer | Components having crystalline coatings of the aluminum oxide/silicon oxide system and method for the production thereof |
| CN1448534A (en) * | 2002-04-04 | 2003-10-15 | 西北工业大学 | Prep. of alumina---monox composite oxides film |
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