CN110184600B - Preparation method of low-stress high-temperature oxidation-resistant coating on titanium alloy surface - Google Patents
Preparation method of low-stress high-temperature oxidation-resistant coating on titanium alloy surface Download PDFInfo
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- CN110184600B CN110184600B CN201910536706.2A CN201910536706A CN110184600B CN 110184600 B CN110184600 B CN 110184600B CN 201910536706 A CN201910536706 A CN 201910536706A CN 110184600 B CN110184600 B CN 110184600B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
- C23C24/103—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
Abstract
The invention discloses a preparation method of a low-stress high-temperature anti-oxidation coating on the surface of a titanium alloy, which is characterized in that an Al/Ti/TiBCN coating material is paved on the surface of the titanium alloy, laser scanning cladding is carried out to obtain a high-temperature anti-oxidation coating, and laser scanning processing is carried out again to obtain a remelting high-temperature anti-oxidation coating, so that the coating structure is refined, and uniform surface residual stress is obtained; and then carrying out vacuum diffusion heat treatment and HCPEB secondary remelting treatment on the remelted high-temperature oxidation-resistant coating to reduce the internal stress of the coating and obtain the low-stress high-temperature oxidation-resistant Al/Ti/TiBCN composite coating.
Description
Technical Field
The invention relates to a preparation method of a high-temperature oxidation-resistant coating, in particular to a method for preparing a low-stress high-temperature oxidation-resistant coating on the surface of a titanium alloy based on laser cladding and HCPEB composite technology.
Background
The titanium alloy material has high specific strength, excellent corrosion resistance and good high-temperature mechanical property, and is a preferable structural and functional material in the industries of aerospace, weaponry, chemical engineering, medical treatment and the like. The method is mainly used for reducing the structural mass and improving the thrust-weight ratio in the aerospace industry.
However, under high temperature conditions, the oxide film formed on the surface of the titanium alloy is mainly porous TiO2Mainly, the oxygen invasion cannot be effectively blocked; in addition, the titanium alloy can be combusted under certain ambient temperature, pressure and airflow speed, for example, the titanium fire spreading speed on a gas turbine engine is very high, and only 4-20 s is left from the beginning to the end of combustion. Therefore, research on the titanium alloy high-temperature protection technology is actively carried out at home and abroad, and the oxidation behavior of the surface of the titanium alloy is changed by controlling the alloy components and the structure.The laser cladding technology is an effective means for obtaining the optimal mechanical property and surface protection at the same time.
As a novel surface modification technology, the laser cladding technology has the advantages of high heating speed, high instant heating temperature, high cooling speed, small heat influence on a workpiece, controllable cladding layer components and dilution, high metallurgical bonding strength between the cladding layer and a substrate and the like. However, under the optimal process parameters, more stress still exists in the high-temperature oxidation-resistant coating prepared by laser cladding, so that the interior of the coating is loose and porous, and the high-temperature service performance of the coating is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a low-stress high-temperature oxidation resistant coating on the surface of a titanium alloy, aiming at the problems of insufficient oxidation resistance of the titanium alloy under a high-temperature condition and more internal stress of a laser cladding coating.
The preparation method of the low-stress high-temperature oxidation-resistant coating on the surface of the titanium alloy comprises the following treatment processes in sequence:
1) paving an Al/Ti/TiBCN coating material on the surface of the titanium alloy, and carrying out laser scanning cladding on the coating material at the laser power of 600-1400W to obtain a high-temperature oxidation-resistant coating;
2) scanning the high-temperature oxidation-resistant coating again by using the laser with the laser power of 50-85% in the step 1), and carrying out laser remelting treatment on the high-temperature oxidation-resistant coating to obtain a remelted high-temperature oxidation-resistant coating;
3) carrying out vacuum diffusion heat treatment on the remelting high-temperature oxidation-resistant coating;
4) and carrying out secondary remelting treatment on the surface of the remelted high-temperature oxidation-resistant coating by using an HCPEB technology to obtain the low-stress high-temperature oxidation-resistant Al/Ti/TiBCN composite coating.
The Al/Ti/TiBCN coating material is obtained by mixing and drying 3-10 wt% of high-purity Al powder, 10-40 wt% of Ti powder and 50-80 wt% of TiBCN powder.
Further, the high-purity Al powder, Ti powder and TiBCN powder are preferably 80-150 mesh raw materials.
Further, the technological conditions for preparing the high-temperature oxidation-resistant coating through laser scanning cladding are that the laser power is 600-1400W, the diameter of a light spot is 4mm, the flow of protective gas is 5-15L/min, the laser scanning speed is 3-9 mm/s, and the scanning overlap ratio is 30-50%.
Furthermore, the Al/Ti/TiBCN coating material is paved on the surface of the titanium alloy through a coaxial carrier gas powder feeding device.
Preferably, the thickness of the high-temperature oxidation-resistant coating formed on the surface of the titanium alloy is 3-5 mm.
Furthermore, when the high-temperature oxidation-resistant coating is subjected to laser remelting treatment, sand paper is firstly used for treating the surface of the high-temperature oxidation-resistant coating, so that the roughness of the high-temperature oxidation-resistant coating reaches 5-20 Ra.
Specifically, the vacuum diffusion heat treatment conditions of the present invention are 1X 10 in vacuum degree-3～1×10-1Carrying out vacuum diffusion heat treatment for 5-7 h in an environment with Pa and a temperature of 600-900 ℃.
Furthermore, the process conditions of the HCPEB technology of the invention are 4 multiplied by 10 under vacuum degree-3～7×10-3Under Pa, with an energy of 10 to 35KeV and an energy density of 3 to 8J/cm2The electron beam bombards the surface of the remelting high-temperature oxidation-resistant coating.
Preferably, the electron beam is arranged 8-35 cm away from the surface of the remelting high-temperature oxidation-resistant coating for bombardment treatment, and the bombardment times are 1-100.
The preparation method also comprises the steps of pretreating the surface of the titanium alloy, including the step of cleaning the surface of the titanium alloy by using a solvent to remove all dirt on the surface, such as oxide skin, oil stain, paint and other dirt, particularly the surface and the grease permeated into the surface; and preheating the titanium alloy.
Specifically, the preheating is to place the titanium alloy in a vacuum furnace, and preheat the titanium alloy to 100 ℃ so as to reduce the cracking of the coating caused by the stress caused by the thermal expansion difference between the surface of the titanium alloy and the coating material.
The invention adopts the combination of the laser cladding technology and the HCPEB technology to prepare the low-stress high-temperature oxidation-resistant coating on the surface of the titanium alloy substrate. The high-temperature oxidation-resistant coating which is compact in structure, uniform in surface residual stress and high in bonding strength with a matrix is prepared by two times of treatment through a laser cladding technology, and then a layer of reinforced remelting coating is formed on the surface of the laser cladding coating after the treatment through an HCPEB technology, so that the porosity of the coating is effectively reduced, coating particles are refined, the distribution of coating elements is optimized, the internal stress of the coating is effectively reduced, and the high-temperature oxidation resistance of the coating is improved.
Drawings
FIG. 1 is a graph comparing the distribution of residual stress on the surface of a remelted high temperature oxidation-resistant coating with that of a high temperature oxidation-resistant coating.
FIG. 2 is a cross-sectional SEM topography comparison of a composite technology process coating and a high temperature oxidation resistant coating.
FIG. 3 is a graph comparing the results of internal stress testing of a composite technology process coating and a high temperature oxidation resistant coating.
FIG. 4 is a comparison graph of the morphology of the composite technology treatment coating and the high-temperature oxidation-resistant coating after isothermal oxidation for 72 h.
Detailed Description
The following examples are only preferred embodiments of the present invention and are not intended to limit the present invention in any way. Various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Example 1.
Respectively screening high-purity Al powder, Ti powder and TiBCN powder of 80-150 meshes by using a mechanical screen, mixing the high-purity Al powder, the Ti powder and the TiBCN powder in a ball mill for 3 hours according to the proportion of 8wt% of the high-purity Al powder, 32wt% of the high-purity Ti powder and 60wt% of the TiBCN powder, drying the uniformly mixed powder for 1 hour in vacuum at 100 ℃, and naturally cooling to obtain the coating material.
The method comprises the steps of taking a TC4 titanium alloy base material with the specification of 20mm multiplied by 15mm as a test sample, carrying out coarse grinding treatment on the surface of the test sample by using 100-mesh metallographic abrasive paper, and then cleaning the surface of the test sample by using acetone to remove all dirt on the surface of the test sample, including oxide scales, oil stains, paint and other dirt, and the key is the surface of the test sample and grease permeated into the surface of the test sample. Wiping, wiping with alcohol, blow-drying, placing in a vacuum heating furnace, heating to 100 deg.C as pretreatment substrate to reduce coating cracking caused by stress due to thermal expansion difference between the substrate and the coating material.
By utilizing the laser cladding process technology, the laser power is 1200W, the diameter of a light spot is 4mm, the flow of protective gas Ar is 15L/min, the laser scanning speed is 7mm/s, and the scanning lap joint rate is 50%. And (3) coating the coating material on the surface of the pretreated substrate through a coaxial carrier gas powder feeding device, and carrying out laser cladding simultaneously to obtain a sample cladded with the high-temperature antioxidant coating.
And removing granular impurities on the surface of the high-temperature oxidation-resistant coating by using sand paper to ensure that the surface roughness of the coating reaches 10 Ra. The method comprises the steps of adopting a laser cladding process technology, carrying out laser remelting treatment on the surface of the high-temperature oxidation-resistant coating according to the process conditions of 800W of laser power, 5mm/s of laser scanning speed, 4mm of spot diameter, 15L/min of protective gas Ar gas flow, longitudinal 25% of scanning lap joint rate and transverse 56.5% of scanning lap joint rate, and removing impurities on the surface of the remelted high-temperature oxidation-resistant coating by using 500-mesh fine sand paper.
And (3) measuring the surface residual stress of the remelting high-temperature oxidation-resistant coating on the sample by using a PSF-2M type X-ray residual stress tester, and interpolating and fitting by using MATLAB to obtain a remelting high-temperature oxidation-resistant coating surface residual stress distribution diagram shown in figure 1 (a).
The surface residual stress of the high-temperature oxidation-resistant coating which is not subjected to the remelting treatment was measured in the same manner, and the surface residual stress distribution diagram of the high-temperature oxidation-resistant coating shown in fig. 1(b) was obtained.
As is apparent from fig. 1(a) and (b), the residual stress distribution on the surface of the remelted high-temperature oxidation-resistant coating in (a) is relatively flat, and the residual stress distribution on the surface of the high-temperature oxidation-resistant coating in (b) is uneven, which shows that the residual stress distribution on the surface of the sample coating can be uniform by the laser remelting treatment.
In order to make the distribution of the elements on the surface of the remelting high-temperature oxidation-resistant coating more uniform, the sample is placed in a vacuum degree of 1 multiplied by 10-3And (3) heating to 660 ℃ at the heating rate of 5 ℃/min in a Pa vacuum heat treatment furnace, and carrying out vacuum diffusion heat treatment for 5 h.
Finally, the HCPEB technology is used, and the process conditions are set as follows: degree of vacuum of 5X 10-3Pa, electron beam energy 20KeV, energy density 6J/cm2And the working distance is 25cm, the bombardment time is 60 times, secondary remelting treatment is carried out on the surface of the remelted high-temperature oxidation-resistant coating, and finally the low-stress secondary remelting high-temperature oxidation-resistant Al/Ti/TiBCN composite coating is obtained.
In fig. 2, (a) and (b) are sectional SEM topography images of the twice-remelted high-temperature oxidation-resistant Al/Ti/TiBCN composite coating treated by the above-mentioned composite technique and the high-temperature oxidation-resistant coating not treated by the composite technique, respectively. The comparison shows that (a) after laser remelting treatment and HCPEB technology secondary remelting treatment, the coating surface is smooth and compact, and the crystal grains are obviously refined.
And then a YJ-31 static resistance strain gauge is adopted, semiconductor silicon (the sensitive grid length is 7mm, the micro strain is 11/DEG C) is used as a residual stress strain gauge, a circuit adopts a full-bridge wiring method, the internal stress of the coating is measured by an ohmmeter, and data is recorded.
FIG. 3 shows a comparison graph of the internal stress test results of the secondary remelting high-temperature oxidation resistant Al/Ti/TiBCN composite coating and the high-temperature oxidation resistant coating. The result shows that the internal stress of the composite technology processing coating is obviously lower than that of the high-temperature oxidation-resistant coating.
And placing the secondary remelting high-temperature oxidation resistant Al/Ti/TiBCN composite coating sample and the high-temperature oxidation resistant coating sample in a heating furnace at 1100 ℃, carrying out isothermal oxidation for 72h, and observing the oxidation SEM morphology of the coating section again.
FIGS. 4(a) and (b) are respectively the 72h isothermal oxidation morphology of the twice-remelted high-temperature oxidation-resistant Al/Ti/TiBCN composite coating and the high-temperature oxidation-resistant coating. It can be obviously seen that the oxidation film of the coating treated by the composite technology is compact, and the oxidation resistance of the coating is stronger than that of the high-temperature oxidation-resistant coating.
Example 2.
Respectively screening high-purity Al powder, Ti powder and TiBCN powder of 80-150 meshes by using a mechanical screen, mixing the high-purity Al powder, the Ti powder and the TiBCN powder in a ball mill for 3 hours according to the proportion of 5wt% of the high-purity Al powder, 25wt% of the high-purity Ti powder and 70wt% of the TiBCN powder, drying the uniformly mixed powder for 1 hour in vacuum at 100 ℃, and naturally cooling to obtain the coating material.
The surface of a TC4 titanium alloy base material (20 mm multiplied by 15 mm) is roughly ground by 100-mesh metallographic abrasive paper, then is cleaned by acetone, wiped clean, wiped and dried by alcohol, and is placed in a vacuum heating furnace to be heated to 100 ℃ to serve as a pretreated base material.
By utilizing the laser cladding process technology, the laser power is set to be 1000W, the diameter of a light spot is 4mm, the flow of protective gas Ar is 15L/min, the laser scanning speed is 5mm/s, and the scanning lap joint rate is 40%. And (3) coating the coating material on the surface of the pretreated substrate through a coaxial carrier gas powder feeding device, and carrying out laser cladding simultaneously to obtain a sample cladded with the high-temperature antioxidant coating.
And removing granular impurities on the surface of the high-temperature oxidation-resistant coating by using sand paper to ensure that the surface roughness of the coating reaches 10 Ra. The method comprises the steps of adopting a laser cladding process technology, carrying out laser remelting treatment on the surface of the high-temperature oxidation-resistant coating according to the process conditions of laser power of 600W, laser scanning speed of 4mm/s, spot diameter of 4mm, protective gas Ar gas flow of 15L/min, scanning lap joint rate of 25% in the longitudinal direction and 56.5% in the transverse direction, and removing impurities on the surface of the remelted high-temperature oxidation-resistant coating by using 500-mesh fine sand paper.
In order to make the elements on the surface of the coating uniformly distributed, the sample is placed in a vacuum degree of 1X 10-2And (3) heating to 660 ℃ at the heating rate of 5 ℃/min in a Pa vacuum heat treatment furnace, and carrying out vacuum diffusion heat treatment for 4 h.
Finally, the HCPEB technology is used, and the process conditions are set as follows: degree of vacuum of 6X 10-3Pa, electron beam energy 30KeV, energy density 5J/cm2And the working distance is 20cm, the bombardment time is 40 times, secondary remelting treatment is carried out on the surface of the remelted high-temperature oxidation-resistant coating, and finally the low-stress secondary remelting high-temperature oxidation-resistant Al/Ti/TiBCN composite coating is obtained.
The test sample is tested according to the method of the embodiment 1, and the result shows that compared with the high-temperature oxidation-resistant coating, the residual stress distribution on the surface of the coating treated by the composite technology is more uniform, the internal stress of the coating is smaller, and after the coating is subjected to oxidation treatment, the structure is compact, the crystal grains are fine, and the oxidation resistance is excellent.
Example 3.
Respectively screening high-purity Al powder, Ti powder and TiBCN powder of 80-150 meshes by using a mechanical screen, mixing the high-purity Al powder, the Ti powder and the TiBCN powder in a ball mill for 3 hours according to the proportion of 3wt% of the high-purity Al powder, 17wt% of the high-purity Ti powder and 80wt% of the TiBCN powder, drying the uniformly mixed powder for 1 hour in vacuum at 100 ℃, and naturally cooling to obtain the coating material.
The surface of a TC4 titanium alloy base material (20 mm multiplied by 15 mm) is roughly ground by 100-mesh metallographic abrasive paper, then is cleaned by acetone, wiped clean, wiped and dried by alcohol, and is placed in a vacuum heating furnace to be heated to 100 ℃ to serve as a pretreated base material.
By utilizing the laser cladding process technology, the laser power is set to be 800W, the diameter of a light spot is 4mm, the flow of protective gas Ar is 15L/min, the laser scanning speed is 3mm/s, and the scanning lap joint rate is 30%. And (3) coating the coating material on the surface of the pretreated substrate through a coaxial carrier gas powder feeding device, and carrying out laser cladding simultaneously to obtain a sample cladded with the high-temperature antioxidant coating.
And removing granular impurities on the surface of the high-temperature oxidation-resistant coating by using sand paper to ensure that the surface roughness of the coating reaches 10 Ra. The method comprises the steps of adopting a laser cladding process technology, carrying out laser remelting treatment on the surface of the high-temperature oxidation-resistant coating according to the process conditions of 400W of laser power, 3mm/s of laser scanning speed, 4mm of spot diameter, 15L/min of protective gas Ar gas flow, longitudinal 25% of scanning lap joint rate and transverse 56.5% of scanning lap joint rate, and removing impurities on the surface of the remelted high-temperature oxidation-resistant coating by using 500-mesh fine sand paper.
In order to make the elements on the surface of the coating uniformly distributed, the sample is placed in a vacuum degree of 1X 10-1And (3) heating to 660 ℃ at the heating rate of 5 ℃/min in a Pa vacuum heat treatment furnace, and carrying out vacuum diffusion heat treatment for 7 h.
Finally, the HCPEB technology is used, and the process conditions are set as follows: degree of vacuum of 7X 10-3Pa, electron beam energy 35KeV, energy density 8J/cm2And the working distance is 35cm, the bombardment time is 100 times, secondary remelting treatment is carried out on the surface of the remelted high-temperature oxidation-resistant coating, and finally the low-stress secondary remelting high-temperature oxidation-resistant Al/Ti/TiBCN composite coating is obtained.
The test sample is tested according to the method of the embodiment 1, and the result shows that compared with the high-temperature oxidation-resistant coating, the residual stress distribution on the surface of the coating treated by the composite technology is more uniform, the internal stress of the coating is smaller, and after the coating is subjected to oxidation treatment, the structure is compact, the crystal grains are fine, and the oxidation resistance is excellent.
Claims (10)
1. A preparation method of a low-stress high-temperature oxidation-resistant coating on the surface of a titanium alloy comprises the following treatment processes in sequence:
1) paving an Al/Ti/TiBCN coating material on the surface of the titanium alloy, and carrying out laser scanning cladding on the coating material at the laser power of 600-1400W to obtain a high-temperature oxidation-resistant coating;
2) scanning the high-temperature oxidation-resistant coating again by using the laser with the laser power of 50-85% in the step 1), and carrying out laser remelting treatment on the high-temperature oxidation-resistant coating to obtain a remelted high-temperature oxidation-resistant coating;
3) carrying out vacuum diffusion heat treatment on the remelting high-temperature oxidation-resistant coating;
4) and carrying out secondary remelting treatment on the surface of the remelted high-temperature oxidation-resistant coating by using an HCPEB technology to obtain the low-stress high-temperature oxidation-resistant Al/Ti/TiBCN composite coating.
2. The preparation method of claim 1, wherein the Al/Ti/TiBCN coating material is prepared by mixing and drying 3-10 wt% of high-purity Al powder, 10-40 wt% of Ti powder and 50-80 wt% of TiBCN powder.
3. The preparation method of claim 1, wherein the process conditions for preparing the high-temperature oxidation-resistant coating by laser scanning cladding are as follows: the laser power is 600-1400W, the diameter of a light spot is 4mm, the flow of protective gas is 5-15L/min, the laser scanning speed is 3-9 mm/s, and the scanning overlap ratio is 30-50%.
4. The preparation method of claim 1, wherein the Al/Ti/TiBCN coating material is coated on the surface of the titanium alloy by a coaxial carrier gas powder feeding device.
5. The method according to claim 4, wherein the high temperature oxidation resistant coating formed on the surface of the titanium alloy has a thickness of 3 to 5 mm.
6. The method according to claim 1, wherein the surface roughness of the high-temperature oxidation-resistant coating is treated to 5 to 20Ra before laser remelting treatment.
7. The method according to claim 1, wherein the vacuum diffusion heat treatment is carried out under a vacuum of 1X 10-3～1×10-1Carrying out vacuum diffusion heat treatment for 5-7 h in an environment with Pa and a temperature of 600-900 ℃.
8. The method of claim 1, wherein the HCPEB technique is performed under a vacuum of 4X 10%-3～7×10-3Under Pa, with an energy of 10 to 35KeV and an energy density of 3 to 8J/cm2The electron beam bombards the surface of the remelting high-temperature oxidation-resistant coating.
9. The preparation method according to claim 8, wherein the electron beam is arranged 8-35 cm away from the surface of the remelted high-temperature oxidation-resistant coating for bombardment treatment, and the bombardment times are 1-100.
10. The method according to claim 1, wherein the method further comprises pretreating the surface of the titanium alloy, including solvent cleaning the surface of the titanium alloy and preheating the titanium alloy to 100 ℃.
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