CN111960830A - SiC/HfB on graphite matrix2-SiC-La2O3SiC superhigh temperature oxidation resistant composite coating - Google Patents
SiC/HfB on graphite matrix2-SiC-La2O3SiC superhigh temperature oxidation resistant composite coating Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 77
- 238000000576 coating method Methods 0.000 title claims abstract description 77
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 59
- 239000010439 graphite Substances 0.000 title claims abstract description 59
- 230000003647 oxidation Effects 0.000 title claims abstract description 52
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 153
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000000034 method Methods 0.000 claims abstract description 44
- 238000002360 preparation method Methods 0.000 claims abstract description 33
- 239000002002 slurry Substances 0.000 claims abstract description 30
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 239000011159 matrix material Substances 0.000 claims abstract description 20
- 230000001680 brushing effect Effects 0.000 claims abstract description 7
- 239000011863 silicon-based powder Substances 0.000 claims description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 229910052593 corundum Inorganic materials 0.000 claims description 21
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 20
- 239000011812 mixed powder Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 5
- 238000007581 slurry coating method Methods 0.000 claims description 5
- 238000010422 painting Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 230000007547 defect Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 239000011253 protective coating Substances 0.000 abstract description 2
- 230000035876 healing Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 73
- 229910003862 HfB2 Inorganic materials 0.000 description 7
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 230000006698 induction Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000002679 ablation Methods 0.000 description 3
- 230000003064 anti-oxidating effect Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000005524 ceramic coating Methods 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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Abstract
The invention relates to the field of ultrahigh-temperature oxidation protective coatings, in particular to SiC/HfB on a graphite substrate2‑SiC‑La2O3a/SiC superhigh temperature oxidation resistant composite coating and a preparation method thereof. The design and preparation of the coating comprise: preparing a SiC bottom layer with a thickness of 100-150 μm by a powder embedding method, and preparing HfB with a thickness of 60-70 μm by a slurry brushing method2‑SiC‑La2O3The intermediate layer and the subsequent embedding method are used for preparing the SiC outer layer with the thickness of 70-80 mu m. Wherein the SiC underlayer can mitigate HfB2‑SiC‑La2O3Coefficient of thermal expansion mismatch between the intermediate layer and the graphite substrate, HfB2‑SiC‑La2O3The middle layer provides good ultrahigh temperature oxidation resistance and structural stability for the graphite matrix. The SiC outer layer is effective in healing surface defects generated by oxidation processes. The method has the advantages of high material utilization rate, simple and easy preparation process and short preparation period, and can effectively reduce the preparation cost of the coating and improve the uniformity and controllability of the components of the prepared coating. The coating prepared by the invention has the capacity of resisting ultrahigh temperature oxidation at 1700 ℃ for 1800 seconds.
Description
The technical field is as follows:
the invention relates to the field of ultrahigh-temperature oxidation protective coatings, in particular to SiC/HfB on a graphite substrate2-SiC-La2O3Design of a/SiC superhigh temperature oxidation resistant composite coating and a preparation method thereof.
Background art:
carbon and its composite material are high-temperature structural materials with excellent performance, and have the advantages of low density, low thermal expansion coefficient, ideal high-temperature mechanical property and the like. However, the defect of insufficient oxidation resistance severely restricts the wide application of the anti-oxidation coating, and the oxidation resistance and the ablation performance of the high-temperature strip can be effectively improved by applying the anti-oxidation coating on the surface.
At present, silicon-based compounds such as SiC are mostly selected as an anti-oxidation coating system of a carbon material, so that effective protection can be realized at medium and high temperature, but the protection performance is poor under the condition of ultrahigh temperature (1600 ℃ and above). With HfB2The typical ultrahigh-temperature ceramic has high melting point, good mechanical property and ultrahigh-temperature ablation resistance, and the introduction of the ultrahigh-temperature ceramic phase into a coating system is one of effective ways for improving the ultrahigh-temperature protective property of the coating. HfB2the-SiC is an ultrahigh-temperature composite ceramic material system with excellent comprehensive performance and is also a coating candidate material with wide attention. However, the ultra-high temperature ceramic coating is usually prepared by a plasma spraying method and an in-situ reaction method, the required equipment is expensive, the material utilization rate is low, the uniformity and controllability of the prepared coating components are poor, and the internal defects exist, so that the application of the coating is greatly limited.
The invention content is as follows:
the invention aims to provide SiC/HfB on a graphite matrix2-SiC-La2O3The invention relates to a design of a/SiC superhigh temperature oxidation resistant composite coating and a preparation method thereof, and the implementation of the invention can effectively solve the existing preparation technology of an oxidation resistant coatingThe problems of high cost, complex process, long preparation period, low material utilization rate, poor uniformity and controllability of coating components and the like in the process. In particular, the coating prepared by the invention has the performance of resisting ultrahigh temperature oxidation at 1700 ℃ for 1800 seconds.
The technical scheme of the invention is as follows:
SiC/HfB on graphite matrix2-SiC-La2O3The SiC superhigh temperature oxidation resistant composite coating comprises a SiC layer with the thickness of 100-150 mu m as a bottom layer and HfB with the thickness of 60-70 mu m as an intermediate layer2-SiC-La2O3The outer layer is a SiC layer with the thickness of 70-80 mu m.
SiC/HfB on the graphite substrate2-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating comprises the steps of preparing a SiC bottom layer by adopting a powder embedding method, and preparing HfB2-SiC-La2O3The intermediate layer is prepared by a slurry brushing method, and the SiC outer layer is prepared by an embedding method.
SiC/HfB on the graphite substrate2-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating comprises the following steps of preparing a SiC bottom layer by adopting an embedding method, wherein the embedding powder comprises the following components in percentage by mass: 60-65% of Si powder, 15-20% of C powder and Al2O315-20% of powder; raw powders Si powder, C powder and Al2O3The powder is dry-mixed for 3-5 h at the rotating speed of 550-650 r/min to obtain embedded powder; completely embedding the graphite matrix into the embedded powder, heating to 1550-1650 ℃ at a speed of 10-15 ℃/min, keeping the temperature for 1.5-2.5 hours in a flowing argon environment, cooling to 900-1100 ℃ at a speed of 5-10 ℃/min, and furnace-cooling to room temperature to obtain the SiC bottom layer.
SiC/HfB on the graphite substrate2-SiC-La2O3Preparation method of/SiC superhigh temperature oxidation resistant composite coating HfB2-SiC-La2O3The intermediate layer is prepared by slurry coating method, and the original powder is HfB in percentage by mass260-70% of powder, 20-30% of SiC powder and La2O3Mixing 10-15% of the powder, performing wet ball milling for 6-10 h by taking absolute ethyl alcohol as a medium to obtain mixed powder,drying the mixed powder, mixing the dried mixed powder with polyvinyl butyral and absolute ethyl alcohol in a mass ratio of 10:0.1: 15-25 to prepare slurry, directly painting the slurry on the outer surface of the SiC bottom layer, and drying the coated slurry in a drying oven at 50-70 ℃ to obtain HfB2-SiC-La2O3An intermediate layer.
SiC/HfB on the graphite substrate2-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating comprises the following steps of preparing an SiC outer layer by adopting an embedding method, wherein the embedded powder comprises the following components in percentage by mass: 60-65% of Si powder, 15-20% of C powder and Al2O315-20% of powder; raw powders Si powder, C powder and Al2O3The powder is dry-mixed for 3-5 h at the rotating speed of 550-650 r/min to obtain embedded powder; preparing SiC bottom layer and HfB2-SiC-La2O3And completely embedding the graphite matrix of the middle layer into the embedding powder, heating to 1480-1520 ℃ at a speed of 10-15 ℃/min, preserving the heat in a flowing argon environment for 50-70 minutes, cooling to 900-1100 ℃ at a speed of 5-10 ℃/min, and cooling to room temperature along with the furnace to obtain the SiC outer layer.
SiC/HfB on the graphite substrate2-SiC-La2O3According to the preparation method of the/SiC ultrahigh temperature oxidation resistant composite coating, the purity of the original powder of the embedded powder is more than 99 wt%, and the granularity of the original powder of the embedded powder is 200-400 meshes.
SiC/HfB on the graphite substrate2-SiC-La2O3Preparation method of/SiC superhigh temperature oxidation resistant composite coating, and preparation method of HfB by slurry brushing method2-SiC-La2O3In the middle layer process, the single-time painting thickness is 5-10 mu m; the purity of the original powder of the mixed powder required for preparing the slurry is more than 99.9 wt%, and the particle size range is 1-2 mu m.
The design idea of the invention is as follows:
the structure of the ultrahigh temperature oxidation resistant composite coating is designed as follows: the bottom layer is a SiC layer, and the middle layer is HfB2-SiC-La2O3The outer layer is a SiC layer. Because of good chemical and physical compatibility with the graphite substrate, the SiC is selected as the bottom layer, so that the heat between the middle layer and the graphite substrate can be effectively relievedThe coefficient of expansion is not matched, and the thermal stress generated in the preparation and application processes of the coating is reduced. Mixing ultra-high temperature ceramic HfB2The structure stability and the phase stability of the coating under the condition of ultrahigh temperature can be obviously improved by applying the antioxidant coating. La2O3Can be used as a sintering aid to improve HfB2The sintering properties of the SiC coating, making the intermediate layer denser; meanwhile, the intermediate layer is dissolved in the oxide layer after being oxidized, so that the diffusion speed of oxygen is reduced. SiC as an outer layer can generate molten SiO in the oxidation process2Filling surface defects and effectively inhibiting oxygen from diffusing inwards.
The invention has the advantages and beneficial effects that:
1. the invention introduces the HfB of the ultra-high temperature ceramic phase into the coating system2While introducing rare earth oxide La2O3Effectively reduces the sintering temperature of the coating and improves the sintering performance of the coating, so that HfB2-SiC-La2O3The middle layer is more compact, and provides good ultrahigh temperature oxidation resistance and structural stability for the graphite matrix. After oxidation of the intermediate layer, La2O3Can be dissolved in the oxide layer to reduce the diffusion speed of oxygen in the oxide layer.
2. In the invention, SiC is selected as an outer layer, and a glass phase generated after oxidation can effectively heal surface defects generated in the oxidation process, so that a complete and compact oxygen diffusion barrier layer is formed, and the oxidation of an inner coating is delayed.
3. The invention adopts a slurry brushing method combined with a subsequent embedding method to prepare the compact HfB2-SiC-La2O3An intermediate layer. Compared with the common preparation method of the ultrahigh-temperature ceramic coating, the preparation method comprises the following steps: the method has the advantages of high material utilization rate, simple preparation equipment, simple and easy preparation process, short preparation period, capability of effectively reducing the preparation cost of the coating, and strong uniformity and controllability of the components of the prepared coating.
4. SiC/HfB designed and prepared on graphite substrate by adopting method of the invention2-SiC-La2O3the/SiC superhigh temperature oxidation resistant composite coating has a multilayer structure and an interlayer interface junctionThe coating has good performance, and can effectively inhibit the inward diffusion of surface cracks, thereby improving the integrity and compactness of the coating.
5. SiC/HfB prepared on graphite matrix by adopting method of the invention2-SiC-La2O3the/SiC superhigh temperature oxidation resistant composite coating has good superhigh temperature oxidation resistance. Can realize the effective protection of oxidizing 1800s in the ultra-high temperature induction heating device at 1700 ℃.
Description of the drawings:
FIG. 1: the embodiment of the invention prepares the surface appearance of the coating.
FIG. 2: the embodiment of the invention prepares the cross-sectional morphology of the coating.
FIG. 3: the surface appearance of the coating prepared by the embodiment of the invention is oxidized at 1700 ℃ for 1800 s.
FIG. 4: the cross-sectional morphology of the coating prepared by the embodiment of the invention is after being oxidized for 1800s at 1700 ℃.
The specific implementation mode is as follows:
in the specific implementation process, the SiC/HfB on the graphite matrix of the invention2-SiC-La2O3The design and preparation of the/SiC superhigh temperature oxidation resistant composite coating structure comprise the following steps: preparing a SiC bottom layer with a thickness of 100-150 μm by a powder embedding method, and preparing HfB with a thickness of 60-70 μm by a slurry brushing method2-SiC-La2O3The intermediate layer and the subsequent embedding method are used for preparing the SiC outer layer with the thickness of 70-80 mu m. The SiC bottom layer comprises, by mass, 60-65% of Si powder, 15-20% of C powder and Al powder2O315-20% of powder and HfB2-SiC-La2O3The intermediate layer adopts HfB as the original powder260-70% of powder, 20-30% of SiC powder and La2O310-15% of powder, wherein the original powder adopted by the SiC outer layer is 60-65% of Si powder, 15-20% of C powder and Al2O315-20% of powder. Wherein the SiC underlayer can mitigate HfB2-SiC-La2O3Coefficient of thermal expansion mismatch between the intermediate layer and the graphite substrate, HfB2-SiC-La2O3The middle layer provides good ultrahigh temperature oxidation resistance and structural stability for the graphite matrix. The SiC outer layer can effectively heal the oxide generatedSurface defects. Further, the coating prepared by the invention is verified to have the capacity of resisting the ultrahigh temperature oxidation at 1700 ℃ for 1800 seconds by examples.
The present invention will be explained in further detail below by way of examples and figures.
Example 1
In this example, SiC/HfB on graphite substrate2-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating comprises the following steps:
(1) the density is 1.78g/cm2The graphite block of (2) was cut into a graphite sample of 10mm × 10mm × 5mm, and surface cutting marks were polished and chamfered using 1000 # water abrasive paper. And ultrasonically cleaning the polished graphite block in absolute ethyl alcohol for 20min, and then drying the graphite block in an oven at 60 ℃ for later use.
(2) The SiC bottom layer is prepared by a powder embedding method, and the embedded powder comprises the following components in percentage by weight: 65% of Si powder, 20% of C powder and Al2O315 percent of powder (mass percentage), the purity of the original powder of the embedded powder is more than 99 weight percent, and the granularity of the original powder of the embedded powder is 300 meshes; mixing the original powders Si powder, C powder and Al2O3The powder is dry-mixed for 4 hours at the rotating speed of 600r/min to obtain embedded powder; completely embedding the graphite matrix into the embedding powder, heating to 1600 ℃ at a speed of 10 ℃/min, preserving the temperature for 2 hours in a flowing argon environment, cooling to 1000 ℃ at a speed of 5 ℃/min, and furnace-cooling to room temperature to obtain a SiC bottom layer with the thickness of 120 mu m.
(3)HfB2-SiC-La2O3The intermediate layer is prepared by slurry coating method, and the original powder is HfB270% of powder, 20% of SiC powder and La2O3Mixing 10% of powder (mass percentage), wherein the purity of the original powder of the mixed powder required by preparing slurry is more than 99.9 wt%, and the granularity range is 1-2 mu m; ball-milling for 8 hours by a wet method by taking absolute ethyl alcohol as a medium to obtain mixed powder, drying the mixed powder, mixing the dried mixed powder with polyvinyl butyral and absolute ethyl alcohol in a mass ratio of 10:0.1:20 to prepare slurry, directly coating the slurry on the outer surface of the SiC inner layer, coating the slurry with the thickness of 5-10 microns in one time, and drying the coated slurry in a 60 ℃ drying oven to obtain HfB with the thickness of 70 microns2-SiC-La2O3An intermediate layer.
(4) The SiC outer layer is prepared by an embedding method, and the composition and the content of embedded powder are as follows: 65% of Si powder, 20% of C powder and Al2O315 percent of powder (mass percentage), the purity of the original powder of the embedded powder is more than 99 weight percent, and the granularity of the original powder of the embedded powder is 300 meshes; mixing the original powders Si powder, C powder and Al2O3The powder is dry-mixed for 4 hours at the rotating speed of 600r/min to obtain embedded powder; preparing SiC bottom layer and HfB2-SiC-La2O3And completely embedding the graphite matrix of the middle layer into the embedding powder, heating to 1500 ℃ at a speed of 10 ℃/min, preserving the heat in a flowing argon environment for 60 minutes, cooling to 1000 ℃ at a speed of 5 ℃/min, and furnace-cooling to room temperature to obtain an SiC outer layer with the thickness of 80 mu m.
In this example, a SiC/HfB on graphite substrate2-SiC-La2O3No defects such as holes, cracks and the like are found on the surface of the/SiC superhigh temperature oxidation resistant composite coating, and the defects are shown in figure 1. The cross section of the coating is of a typical multilayer structure, the bonding between layers is good, and no penetrating crack exists, as shown in figure 2. After being oxidized for 1800s at 1700 ℃ in an ultra-high temperature induction heating furnace, the weight per unit area is increased by 4.60mg/cm2. The surface of the oxide film is uniform and compact, and no obvious cracks or holes are seen on the surface, which is shown in figure 3. As shown in FIG. 4, the oxidized coating and the graphite matrix are well combined, no penetrating crack is seen, and the graphite matrix is kept intact, which indicates that the coating has good ultrahigh temperature oxidation resistance.
Example 2
In this example, SiC/HfB on graphite substrate2-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating comprises the following steps:
(1) the density is 1.78g/cm2The graphite block of (2) was cut into a graphite sample of 10mm × 10mm × 5mm, and surface cutting marks were polished and chamfered using 1000 # water abrasive paper. And ultrasonically cleaning the polished graphite block in absolute ethyl alcohol for 20min, and then drying the graphite block in an oven at 60 ℃ for later use.
(2) The SiC bottom layer is prepared by a powder embedding method, and the embedded powder comprises the following components in percentage by weight: 62% of Si powder, 20% of C powder and Al2O318 percent of powder (mass percentage) and embedding powderThe purity of the original powder of the material is more than 99 wt%, and the granularity of the original powder of the embedded powder is 300 meshes; mixing the original powders Si powder, C powder and Al2O3The powder is dry-mixed for 3.5 hours at the rotating speed of 650r/min to obtain embedded powder; completely embedding the graphite matrix into the embedding powder, heating to 1550 ℃ at a speed of 15 ℃/min, preserving the temperature in a flowing argon environment for 2.5 hours, cooling to 950 ℃ at a speed of 10 ℃/min, and furnace-cooling to room temperature to obtain a SiC bottom layer with the thickness of 100 mu m.
(3)HfB2-SiC-La2O3The intermediate layer is prepared by slurry coating method, and the original powder is HfB265% of powder, 20% of SiC powder and La2O3Mixing 15% of powder (mass percentage), wherein the purity of the original powder of the mixed powder required by preparing slurry is more than 99.9 wt%, and the granularity range is 1-2 mu m; ball-milling for 10 hours by a wet method by taking absolute ethyl alcohol as a medium to obtain mixed powder, drying the mixed powder, mixing the dried mixed powder with polyvinyl butyral and absolute ethyl alcohol in a mass ratio of 10:0.1:15 to prepare slurry, directly coating the slurry on the outer surface of the SiC inner layer, coating the slurry with the thickness of 5-10 microns in one time, and drying the coated slurry in a 50 ℃ drying oven to obtain HfB with the thickness of 70 microns2-SiC-La2O3An intermediate layer.
(4) The SiC outer layer is prepared by an embedding method, and the composition and the content of embedded powder are as follows: 62% of Si powder, 20% of C powder and Al2O318 percent of powder (mass percentage), the purity of the original powder of the embedded powder is more than 99 weight percent, and the granularity of the original powder of the embedded powder is 300 meshes; mixing the original powders Si powder, C powder and Al2O3The powder is dry-mixed for 3.5 hours at the rotating speed of 650r/min to obtain embedded powder; preparing SiC bottom layer and HfB2-SiC-La2O3And completely embedding the graphite matrix of the middle layer into the embedding powder, heating to 1480 ℃ at a speed of 15 ℃/min, preserving the heat in a flowing argon environment for 70 minutes, cooling to 950 ℃ at a speed of 10 ℃/min, and cooling to room temperature along with the furnace to obtain a SiC outer layer with a thickness of 70 microns.
In this example, a SiC/HfB on graphite substrate2-SiC-La2O3After the/SiC superhigh temperature oxidation resistant composite coating is oxidized for 1800 seconds at 1700 ℃ in a superhigh temperature induction heating furnace, the weight of the unit area is increased by 4.38mg/cm2Watch, watchThe bright coating has good ultrahigh temperature oxidation resistance.
Example 3
In this example, SiC/HfB on graphite substrate2-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating comprises the following steps:
(1) the density is 1.78g/cm2The graphite block of (2) was cut into a graphite sample of 10mm × 10mm × 5mm, and surface cutting marks were polished and chamfered using 1000 # water abrasive paper. And ultrasonically cleaning the polished graphite block in absolute ethyl alcohol for 20min, and then drying the graphite block in an oven at 60 ℃ for later use.
(2) The SiC bottom layer is prepared by a powder embedding method, and the embedded powder comprises the following components in percentage by weight: 65% of Si powder, 18% of C powder and Al2O317 percent of powder (mass percentage), the purity of the original powder of the embedded powder is more than 99 weight percent, and the granularity of the original powder of the embedded powder is 300 meshes; mixing the original powders Si powder, C powder and Al2O3The powder is dry-mixed for 5 hours at the rotating speed of 550r/min to obtain embedded powder; completely embedding the graphite matrix into the embedding powder, heating to 1650 ℃ at a speed of 12 ℃/min, keeping the temperature for 1.5 hours in a flowing argon environment, cooling to 1050 ℃ at a speed of 8 ℃/min, and furnace-cooling to room temperature to obtain a SiC bottom layer with the thickness of 150 mu m.
(3)HfB2-SiC-La2O3The intermediate layer is prepared by slurry coating method, and the original powder is HfB260% of powder, 30% of SiC powder and La2O3Mixing 10% of powder (mass percentage), wherein the purity of the original powder of the mixed powder required by preparing slurry is more than 99.9 wt%, and the granularity range is 1-2 mu m; ball-milling for 6 hours by a wet method by taking absolute ethyl alcohol as a medium to obtain mixed powder, drying the mixed powder, mixing the dried mixed powder with polyvinyl butyral and absolute ethyl alcohol in a mass ratio of 10:0.1:25 to prepare slurry, directly coating the slurry on the outer surface of the SiC inner layer, coating the slurry with the thickness of 5-10 microns in one time, and drying the coated slurry in a 70 ℃ drying oven to obtain HfB with the thickness of 60 microns2-SiC-La2O3An intermediate layer.
(4) The SiC outer layer is prepared by an embedding method, and the composition and the content of embedded powder are as follows: 65% of Si powder, 18% of C powder and Al2O317 percent of powder (mass percentage)The percentage ratio) of the raw powder of the embedded powder is higher than 99 wt%, and the granularity of the raw powder of the embedded powder is 300 meshes; mixing the original powders Si powder, C powder and Al2O3The powder is dry-mixed for 5 hours at the rotating speed of 550r/min to obtain embedded powder; preparing SiC bottom layer and HfB2-SiC-La2O3And completely embedding the graphite matrix of the middle layer into the embedding powder, heating to 1520 ℃ at a speed of 12 ℃/min, preserving the heat in a flowing argon environment for 50 minutes, cooling to 1050 ℃ at a speed of 8 ℃/min, and furnace-cooling to room temperature to obtain an SiC outer layer with the thickness of 80 mu m.
In this example, a SiC/HfB on graphite substrate2-SiC-La2O3After the/SiC superhigh temperature oxidation resistant composite coating is oxidized for 1800 seconds at 1700 ℃ in a superhigh temperature induction heating furnace, the weight of the unit area is increased by 4.53mg/cm2The result shows that the coating has good ultrahigh temperature oxidation resistance.
The embodiment result shows that the coating has the characteristics of simple and easy operation, adjustable and controllable coating components and the like, and can quickly and effectively prepare the ultrahigh temperature oxidation resistant composite coating. The coating prepared in the embodiment shows good oxidation ablation resistance in air at 1700 ℃.
Claims (7)
1. SiC/HfB on graphite matrix2-SiC-La2O3the/SiC superhigh temperature oxidation resistant composite coating is characterized in that the bottom layer is a SiC layer with the thickness of 100-150 mu m, and the middle layer is HfB with the thickness of 60-70 mu m2-SiC-La2O3The outer layer is a SiC layer with the thickness of 70-80 mu m.
2. The SiC/HfB on graphite substrate of claim 12-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating is characterized in that the SiC bottom layer is prepared by adopting a powder embedding method, HfB2-SiC-La2O3The intermediate layer is prepared by a slurry brushing method, and the SiC outer layer is prepared by an embedding method.
3. SiC/H on graphite substrate according to claim 2fB2-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating is characterized in that the SiC bottom layer is prepared by an embedding method, and the composition and the content of embedded powder are as follows by mass percent: 60-65% of Si powder, 15-20% of C powder and Al2O315-20% of powder; raw powders Si powder, C powder and Al2O3The powder is dry-mixed for 3-5 h at the rotating speed of 550-650 r/min to obtain embedded powder; completely embedding the graphite matrix into the embedded powder, heating to 1550-1650 ℃ at a speed of 10-15 ℃/min, keeping the temperature for 1.5-2.5 hours in a flowing argon environment, cooling to 900-1100 ℃ at a speed of 5-10 ℃/min, and furnace-cooling to room temperature to obtain the SiC bottom layer.
4. The SiC on graphite substrate/HfB of claim 22-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating is characterized in that HfB2-SiC-La2O3The intermediate layer is prepared by slurry coating method, and the original powder is HfB in percentage by mass260-70% of powder, 20-30% of SiC powder and La2O3Mixing 10-15% of powder, performing wet ball milling for 6-10 hours by taking absolute ethyl alcohol as a medium to obtain mixed powder, drying the mixed powder, mixing the dried mixed powder with polyvinyl butyral and absolute ethyl alcohol in a mass ratio of 10:0.1: 15-25 to prepare slurry, directly coating the slurry on the outer surface of a SiC bottom layer, and drying the slurry in a drying oven at 50-70 ℃ after coating to obtain HfB2-SiC-La2O3An intermediate layer.
5. The SiC on graphite substrate/HfB of claim 22-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating is characterized in that the SiC outer layer is prepared by an embedding method, and the composition and the content of embedded powder are as follows by mass percent: 60-65% of Si powder, 15-20% of C powder and Al2O315-20% of powder; raw powders Si powder, C powder and Al2O3The powder is dry-mixed for 3-5 h at the rotating speed of 550-650 r/min to obtain embedded powder; preparing SiC bottom layer and HfB2-SiC-La2O3Of intermediate layersAnd completely embedding the graphite matrix into the embedded powder, heating to 1480-1520 ℃ at a speed of 10-15 ℃/min, preserving heat in a flowing argon environment for 50-70 minutes, cooling to 900-1100 ℃ at a speed of 5-10 ℃/min, and furnace-cooling to room temperature to obtain the SiC outer layer.
6. SiC/HfB on graphite substrate according to claim 3 or 52-SiC-La2O3The preparation method of the/SiC ultrahigh temperature oxidation resistant composite coating is characterized in that the purity of the original powder of the embedded powder is more than 99 wt%, and the granularity of the original powder of the embedded powder is 200-400 meshes.
7. The SiC on graphite substrate/HfB of claim 42-SiC-La2O3The preparation method of the/SiC superhigh temperature oxidation resistant composite coating is characterized in that the slurry brushing method is used for preparing HfB2-SiC-La2O3In the middle layer process, the single-time painting thickness is 5-10 mu m; the purity of the original powder of the mixed powder required for preparing the slurry is more than 99.9 wt%, and the particle size range is 1-2 mu m.
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