CN107673762B - Anti-oxidation ZrSi on surface of C/C composite material2-Y2O3/SiC composite coating and preparation method thereof - Google Patents
Anti-oxidation ZrSi on surface of C/C composite material2-Y2O3/SiC composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a long-time oxidation-resistant ZrSi on the surface of a C/C composite material2‑Y2O3The preparation method of the/SiC composite coating comprises the steps of preparing a SiC inner coating and ZrSi by an embedding method and a SAPS two-step method2‑Y2O3And (3) coating the composite ceramic outer layer. Preparing SiC inner coating and ZrSi by embedding and supersonic plasma spraying (SAPS) two-step method2‑Y2O3And (4) compounding an outer coating. The paint is characterized in that the outer coating comprises the following components in percentage by mass: 70 to 95 percent of ZrSi2,5%~30%Y2O3. The prepared oxidation resistant coating is ZrSi at 1500 DEG C2Produced SiO2The mobile glassy phase is capable of healing coating microcracks, and Y is added2O3Then with ZrO2React to form a solid solution and slow down SiO2And (3) volatilizing the glass phase, so that the prepared coating has good compactness, and the coating keeps weight gain after static oxidation at 1500 ℃ for 150-280 h.
Description
Technical Field
The invention belongs to a coating preparation technology, and relates to a long-time oxidation-resistant ZrSi on the surface of a C/C composite material2-Y2O3a/SiC composite coating and a preparation method thereof.
Background
The C/C composite material has excellent mechanical property and is the most ideal high-temperature thermal structure material, but the application range of the C/C composite material is limited by the problem that the C/C composite material is easy to oxidize in a high-temperature aerobic environment, and the C/C composite material is the most effective method by adopting an external coating technology. SAPS technology is one of the methods for efficiently preparing coatings developed in recent years, the plasma arc temperature of the SAPS technology can reach 10000 ℃, and ultrahigh and high melting point can be preparedThe ceramic coating and the prepared coating have high interfacial bonding force, but the prepared coating has a small amount of cracks and pores. The external coating is mainly glass phase SiO generated by silicon-based phase ceramic oxidation at high temperature2Capable of healing coating microcracks and micropores to improve oxidation performance, but glassy phase SiO2Volatilization occurs at 1500 ℃, and cracks in the coating can propagate at high temperature to produce SiO2The glass phase is limited and does not heal all of the microcracks and pores of the coating, thereby providing a pathway for oxygen, ultimately leading to failure of the coating's oxidative properties. The oxidation resistance of the oxidation resistant coating prepared by the SAPS method at present is still not ideal at 1500 ℃.
The document 1 "A ZrB 2-SiC/SiC oxidation protective double-layer coating for carbon/carbon composites, Shanbao Zhou, Yushi Qi, Peng Wang, Yehong Cheng and Wenbo Han, Advances in Applied Ceramics,2017: 1-6" indicates that the ZrB2-SiC coating has an oxidation time of 18h at 1500 ℃ and that the coating loses 1.8% weight, and the oxidation product SiO generated in the coating is SiO2One part is volatilized, the other part and an oxidation product ZrO2React to generate ZrSiO4,ZrSiO4Can effectively improve the oxidation resistance of the coating, but because of the SiO of the coating2The content is continuously reduced, and cracks and pores generated in the final coating are difficult to heal, so that the coating fails.
Document 2 "Oxidation resistance of a La-Mo-Si-O-C coating prepared by Supersonic atomic Plasma Spraying on the Surface of SiC-coated C/C compositions, Xiaohong Shi, Changcong Wang, Hongjiao Lin, Caixia Huo, Xiuxiu Jin, Guoge Shi, Kaiyan Dong, Surface & Coatings Technology,2016,300: 10-18" indicates that the coating Oxidation system prepared by the SAPA method has a certain Oxidation resistance, static Oxidation 85h at 1500 ℃ is 5.12%, and the failure reason is mainly due to the fact that the non-healing cracks and pores in the coating provide channels for oxygen, resulting in a shorter Oxidation time.
Therefore, the preparation of the C/C composite material oxidation resistant coating by the SAPS method for a long time is a problem which is difficult to break through.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides the ZrSi with long-time oxidation resistance on the surface of the C/C composite material2-Y2O3the/SiC composite coating and the preparation method thereof provide long-time antioxidant protection for the C/C composite material in an aerobic environment at 1500 ℃.
Technical scheme
Long-time oxidation resistance ZrSi on surface of C/C composite material2-Y2O3the/SiC composite coating is characterized in that: the inner coating is SiC and the outer coating is ZrSi2-Y2O3A composite ceramic coating; the mass percent of the outer coating component is 70-95 wt.% of ZrSi2And 5 to 30 wt.% of Y2O3。
Preparing the long-time oxidation-resistant ZrSi on the surface of the C/C composite material2-Y2O3The method for coating the/SiC composite coating is characterized by comprising the following steps: the inner coating SiC adopts an embedding method, and the outer coating ZrSi2-Y2O3The composite ceramic coating adopts an SAPS method and comprises the following steps:
step 1: 70 to 95 wt.% of ZrSi2And 5 to 30 wt.% of Y2O3Mixing the powder by a planetary ball mill and uniformly stirring to obtain mixed powder;
step 2: mixing and stirring 45-55 wt.% of mixed powder, 5-8 wt.% of binder and 37-50 wt.% of distilled water to form mixed slurry; the binder is a 3 wt.% polyvinyl alcohol solution;
and step 3: granulating the mixed slurry by adopting a centrifugal spray drying method to obtain spherical powder; the inlet temperature of the dryer is 300-340 ℃, and the outlet temperature is 120-150 ℃;
and 4, step 4: loading the spherical powder into a powder feeder, spraying the spherical powder onto the surface of the SiC inner coating layer of the C/C composite material by a supersonic plasma spraying method to obtain ZrSi2-Y2O3A composite ceramic outer coating; the technological parameters of the supersonic plasma spraying method are as follows: the power is as follows: 25-55 KW, 65-80L/min of Ar flow, 10-40 g/min of powder feeding amount and spraying distance80~120mm。
The preparation method of the SiC inner coating of the C/C composite material comprises the following steps:
step 1): ultrasonically cleaning and drying the C/C composite material;
step 2): embedding the C/C composite material into the mixed powder in a graphite crucible, placing the graphite crucible in a high-temperature graphitization heat treatment furnace, taking argon as protective gas, raising the temperature to 1900-2100 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 1-2 h, turning off a power supply, and naturally cooling to the normal temperature to obtain the C/C composite material protected by the SiC coating;
the mixed powder comprises the following components: 60 to 80 percent of Si powder, 10 to 20 percent of C powder and 10 to 20 percent of Al powder2O3And mixing the powder, placing the powder in a resin ball milling tank, and mixing for 3-5 h to obtain the embedded mixed powder.
The step 1) of drying is as follows: and drying in a 120 ℃ oven for 1-2 h.
Advantageous effects
The surface of the C/C composite material provided by the invention is long-time oxidation resistant ZrSi2-Y2O3The preparation method of the/SiC composite coating comprises the steps of preparing a SiC inner coating and ZrSi by an embedding method and a SAPS two-step method2-Y2O3And (3) coating the composite ceramic outer layer. Preparing SiC inner coating and ZrSi by embedding and supersonic plasma spraying (SAPS) two-step method2-Y2O3And (4) compounding an outer coating. The paint is characterized in that the outer coating comprises the following components in percentage by mass: 70 to 95 percent of ZrSi2,5%~30% Y2O3. The prepared oxidation resistant coating is ZrSi at 1500 DEG C2Produced SiO2The mobile glassy phase is capable of healing coating microcracks, and Y is added2O3Then with ZrO2React to form a solid solution and slow down SiO2And (3) volatilizing the glass phase, so that the prepared coating has good compactness, and the coating keeps weight gain after static oxidation at 1500 ℃ for 150-280 h.
The invention has the beneficial effect that ZrSi2Can generate flowing SiO at high temperature of 1500 DEG C2The glass phase effectively fills cracks and pores of the coating and improves the use of ultra-high temperature silicon base in the current researchThe ceramic can not generate SiO in a short time2The glass phase causes the defect of reduced oxidation resistance of the coating, and 5-30 wt.% of Y is added2O3ZrO capable of post-oxidation phase2React to form a solid solution and form an oxidized phase ZrSiO4Combined action on SiO inhibition2The invention breaks through the bottlenecks that the C/C composite material oxidation resistant coating prepared by the SAPS method can not continuously increase weight and maintain oxidation resistance for more than 100 hours at the temperature of 1500 ℃, and the coating can keep weight gain after static oxidation for 150-280 hours at the high temperature of 1500 ℃.
Drawings
FIG. 1 is ZrSi prepared in example 32-Y2O3Surface secondary electron morphology of/SiC composite coating
FIG. 2 is ZrSi prepared in example 32-Y2O3Surface secondary electron morphology of/SiC composite coating after being oxidized at 1500 ℃ for 253h
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1
1. Preparation of inner coating SiC:
step 1: grinding and polishing the C/C composite material by using sand paper, ultrasonically cleaning the C/C composite material for 30min by using absolute ethyl alcohol, and then drying the C/C composite material for 1h in an oven at the temperature of 120 ℃;
step 2: 75g of Si powder, 15g C powder and 10g of Al2O3The powder is mixed and placed in a resin ball milling tank, embedded powder is obtained after the powder is mixed for 3 hours, the C/C composite material is embedded into the blended powder in a graphite crucible, the graphite crucible is placed in a high-temperature graphitization heat treatment furnace, argon is used as protective gas, the temperature is raised to 1900 ℃ according to the heating rate of 10 ℃/min, the temperature is kept for 2 hours, a power supply is turned off, and the C/C composite material protected by the SiC coating is obtained after the natural cooling to the normal temperature.
2. Preparing powder for spraying by adopting a spray drying method:
step 1: 85g of ZrSi2And 15gY2O3Mixing and uniformly stirring the powder by adopting a planetary ball mill;
step 2: preparing 3 wt.% polyvinyl alcohol solution as a binder, and mixing and stirring 45g of mixed powder, 5g of binder and 50g of distilled water for 1 hour to form mixed slurry;
and step 3: granulating the mixed slurry by adopting a centrifugal spray drying method to obtain spherical powder, wherein the inlet temperature of a dryer is 320 ℃, and the outlet temperature of the dryer is 130 ℃;
3. preparation of ZrSi2-Y2O3Composite ceramic outer coating:
preparing an external coating from spherical powder by an SAPS method, mainly loading the spherical powder prepared by the technology 2 into a powder feeder by using the SiC embedded C/C composite material prepared by the fixture fixing technology 1, and spraying the spherical powder onto the surface of the SiC embedded C/C composite material to obtain ZrSi2-Y2O3And (3) coating the composite ceramic outer layer.
The technological parameters of the supersonic plasma spraying method are as follows: the power is as follows: 35KW, 70L/min Ar flow, 30g/min powder feeding amount and 105mm spraying distance.
Example 2
1. Preparation of inner coating SiC:
step 1: grinding and polishing the C/C composite material by using sand paper, ultrasonically cleaning the C/C composite material for 30min by using absolute ethyl alcohol, and then drying the C/C composite material for 1.5h in an oven at the temperature of 120 ℃;
step 2: 70g of Si powder, 15g C powder and 15g of Al2O3The powder is mixed and placed in a resin ball milling tank, embedded powder is obtained after 3 hours of mixing, the C/C composite material is embedded in the blended powder in a graphite crucible, the graphite crucible is placed in a high-temperature graphitization heat treatment furnace, argon is used as protective gas, the temperature is increased to 2000 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1.5 hours, a power supply is turned off, and the C/C composite material protected by the SiC coating is obtained after natural cooling to the normal temperature.
2. Preparing powder for spraying by adopting a spray drying method:
step 1: 75g of ZrSi2And 25gY2O3Mixing and uniformly stirring the powder by adopting a planetary ball mill;
step 2: preparing 3 wt.% polyvinyl alcohol solution as a binder, and mixing and stirring the mixture for 1 hour according to the proportion of 50g of mixed powder, 8g of binder and 42g of distilled water to form mixed slurry;
and step 3: granulating the mixed slurry by adopting a centrifugal spray drying method to obtain spherical powder, wherein the inlet temperature of a dryer is 330 ℃, and the outlet temperature of the dryer is 120 ℃;
3. preparation of ZrSi2-Y2O3Composite ceramic outer coating:
preparing an external coating from spherical powder by an SAPS method, mainly loading the spherical powder prepared by the technology 2 into a powder feeder by using the SiC embedded C/C composite material prepared by the fixture fixing technology 1, and spraying the spherical powder onto the surface of the SiC embedded C/C composite material to obtain ZrSi2-Y2O3And (3) coating the composite ceramic outer layer.
The technological parameters of the supersonic plasma spraying method are as follows: the power is as follows: 40kW, Ar flow rate of 75L/min, powder feeding amount of 25g/min, and spraying distance of 100 mm.
Example 3
1. Preparation of inner coating SiC:
step 1: grinding and polishing the C/C composite material by using sand paper, ultrasonically cleaning the C/C composite material for 30min by using absolute ethyl alcohol, and then drying the C/C composite material in an oven at 120 ℃;
step 2: 80g of Si powder, 15g C powder and 5g of Al2O3The powder is mixed and placed in a resin ball milling tank, embedded powder is obtained after 3 hours of mixing, the C/C composite material is embedded in the blended powder in a graphite crucible, the graphite crucible is placed in a high-temperature graphitization heat treatment furnace, argon is used as protective gas, the temperature is increased to 2100 ℃ at the heating rate of 10 ℃/min, the temperature is kept for 1 hour, a power supply is turned off, and the C/C composite material protected by the SiC coating is obtained after natural cooling to the normal temperature.
2. Preparing powder for spraying by adopting a spray drying method:
step 1: 90g of ZrSi2And 10gY2O3Mixing and uniformly stirring the powder by adopting a planetary ball mill;
step 2: preparing 3 wt.% polyvinyl alcohol solution as a binder, and mixing and stirring 53g of mixed powder, 7g of binder and 40g of distilled water for 1 hour to form mixed slurry;
and step 3: granulating the mixed slurry by adopting a centrifugal spray drying method to obtain spherical powder, wherein the inlet temperature of a dryer is 335 ℃, and the outlet temperature of the dryer is 125 ℃;
3. preparation of ZrSi2-Y2O3Composite ceramic outer coating:
preparing an external coating from spherical powder by an SAPS method, mainly loading the spherical powder prepared by the technology 2 into a powder feeder by using the SiC embedded C/C composite material prepared by the fixture fixing technology 1, and spraying the spherical powder onto the surface of the SiC embedded C/C composite material to obtain ZrSi2-Y2O3And (3) coating the composite ceramic outer layer.
The technological parameters of the supersonic plasma spraying method are as follows: the power is as follows: 45KW, 77L/min Ar flow, 38g/min powder feeding amount and 112mm spraying distance.
Claims (3)
1. Anti-oxidation ZrSi on surface of C/C composite material2-Y2O3The preparation method of the/SiC composite coating is characterized by comprising the following steps: the inner coating is SiC and the outer coating is ZrSi2-Y2O3A composite ceramic coating; the outer coating comprises 70-95 wt.% of ZrSi2And 5 to 30 wt.% of Y2O3;
The inner coating SiC adopts an embedding method, and the outer coating ZrSi2-Y2O3The composite ceramic coating adopts an SAPS method and comprises the following steps:
step 1: 70 to 95 wt.% of ZrSi2And 5 to 30 wt.% of Y2O3Mixing the powder by a planetary ball mill and uniformly stirring to obtain mixed powder;
step 2: mixing and stirring 45-55 wt.% of mixed powder, 5-8 wt.% of binder and 37-50 wt.% of distilled water to form mixed slurry; the binder is a 3 wt.% polyvinyl alcohol solution;
and step 3: granulating the mixed slurry by adopting a centrifugal spray drying method to obtain spherical powder; the inlet temperature of the dryer is 300-340 ℃, and the outlet temperature is 120-150 ℃;
and 4, step 4: filling the spherical powder into a powder feeder, spraying the spherical powder to the surface of the SiC inner coating layer of the C/C composite material by a supersonic plasma spraying method to obtain ZrSi2-Y2O3A composite ceramic outer coating; the technological parameters of the supersonic plasma spraying method are as follows: the power is as follows: 25-55 KW, 65-80L/min of Ar flow, 10-40 g/min of powder feeding amount and 80-120 mm of spraying distance.
2. The method of claim 1, wherein: the preparation method of the SiC inner coating of the C/C composite material comprises the following steps:
step 1): ultrasonically cleaning and drying the C/C composite material;
step 2): embedding the C/C composite material into the mixed powder in a graphite crucible, placing the graphite crucible in a high-temperature graphitization heat treatment furnace, taking argon as protective gas, raising the temperature to 1900-2100 ℃ at a heating rate of 10 ℃/min, preserving the temperature for 1-2 h, turning off a power supply, and naturally cooling to the normal temperature to obtain the C/C composite material protected by the SiC coating;
the mixed powder comprises the following components: 60 to 80 percent of Si powder, 10 to 20 percent of C powder and 10 to 20 percent of Al powder2O3And mixing the powder, placing the powder in a resin ball milling tank, and mixing for 3-5 h to obtain the embedded mixed powder.
3. The method of claim 2, wherein: the step 1) of drying is as follows: and drying in a 120 ℃ oven for 1-2 h.
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CN108503390B (en) * | 2018-05-04 | 2021-02-02 | 西北工业大学 | Surface mosaic SiC-ZrB of carbon/carbon composite material2-ZrSi2Preparation method of composite oxidation-resistant coating |
CN111960830A (en) * | 2020-08-04 | 2020-11-20 | 中国科学院金属研究所 | SiC/HfB on graphite matrix2-SiC-La2O3SiC superhigh temperature oxidation resistant composite coating |
CN112592207A (en) * | 2020-12-30 | 2021-04-02 | 南京航空航天大学 | Self-healing ZrB2-SiC-Y2O3Coating and application thereof to SiC-embedded carbon-carbon composite material |
CN112745143A (en) * | 2021-01-05 | 2021-05-04 | 北京化工大学 | ZrO preparation by adopting sol-gel method2-SiO2Method for coating C/C composite material with-SiC |
CN113563119A (en) * | 2021-08-11 | 2021-10-29 | 西安工程大学 | Preparation method of C/C composite material surface oxidation-resistant coating |
CN114853506B (en) * | 2022-03-30 | 2023-11-10 | 西北工业大学 | Carbon/carbon composite surface (HfZrTi) C 3 Mid-entropy carbide anti-ablation coating and preparation method thereof |
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