CN114716268B - Preparation of Glass-MoSi on surface of carbon/carbon composite material 2 @Y 2 O 3 Method for preparing-SiC oxidation-resistant coating - Google Patents
Preparation of Glass-MoSi on surface of carbon/carbon composite material 2 @Y 2 O 3 Method for preparing-SiC oxidation-resistant coating Download PDFInfo
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Abstract
The invention discloses a method for preparing Glass-MoSi on the surface of a carbon/carbon composite material 2 @Y 2 O 3 -a method of oxidation resistant coating of SiC comprising the steps of: step one, moSi preparation 2 @Y 2 O 3 Microcapsules; step two, preparing a carbon/carbon composite material with a SiC inner coating on the surface; step three, preparing MoSi by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 An outer coating of core-shell structure; step four, preparing glass powder; step five, mixing the glass powder prepared in the step four with molybdenum disilicide according to the mass ratio of (4-8) to 1, diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, brushing the slurry on the surface of the sample by using a brush, and then preserving the temperature of the sample for 2-6 min at 1400 ℃ in an argon atmosphere to finally obtain compactThe high-temperature oxidation resistant coating; the method forms compact Glass-MoSi on the surface of the carbon/carbon composite material 2 @Y 2 O 3 -SiC oxidation resistant coating.
Description
Technical Field
The invention belongs to the technical field of C/C composite materials, relates to a preparation method of a high-temperature oxidation resistant coating of a C/C composite material, and particularly relates to a method for preparing Glass-MoSi on the surface of a carbon/carbon composite material 2 @Y 2 O 3 -SiC oxidation resistant coating process.
Background
The C/C composite material is a novel ultra-high temperature structural material, and not only has the advantages of small density, large specific strength, low linear expansion coefficient, strong heat and electricity conducting capability, corrosion resistance, high friction factor and the like, but also has a series of excellent high-temperature properties, such as thermal shock resistance, good thermal stability, ablation resistance and the like. Therefore, the method is widely applied to the aerospace field. However, the C/C composite material is severely oxidized in an oxidizing environment exceeding 500 ℃, so that the application of the C/C composite material in the high temperature field is severely limited. At present, there are two methods for oxidation resistance of the C/C composite material, which are respectively as follows: the method comprises the steps of adopting an internal matrix modification technology for improving the oxidation resistance of carbon fibers and matrix carbon by adding modification inhibitors (such as borate and phosphate) and an external oxidation resistant coating technology for isolating oxygen-containing gas from contacting with a matrix [ Yang Xin, huang Qizhong, su Zhean and Chang Xin ] high-temperature oxidation resistant protection research of C/C composite materials advances [ J ] aerospace material technology, 2014,44 (01): 1-15 ]. However, the oxidation-resistant coating technology has great potential for future applications.
MoSi 2 The melting point is as high as 2030 ℃, the self-healing capability is good at high temperature, the self-healing coating can be stably used at 1600 ℃, and the self-healing coating is a good high-temperature protective coating candidate material, but the self-healing coating has larger brittleness and insufficient high-temperature strength below 1000 ℃, and particularly the creep resistance is low, so that the application of the self-healing coating as a high-temperature structural material is limited. Therefore, we give MoSi 2 Surface is wrapped with a layer of Y 2 O 3 To weaken the brittleness of the product at medium and low temperature to form MoSi 2 /Y 2 O 3 Microcapsules of core-shell structure. Chen et al prepared 0.5 wt% Y by pressureless sintering 2 O 3 -MoSi 2 The SiC composite material has the advantages that the sintering activation energy is reduced, the grains are refined, the composite material structure is compact and uniform, and the mechanical property and the high-temperature oxidation resistance at 1200 ℃ are improved to different degrees [ F, chen, J.G, xu, J.H, yan, S.W. Tang, effects of Y 2 O 3 on SiC/MoSi 2 composite by mechanical-assistant combustion synthesis, Int. J. Refract Metal Hard Mater. 36 (2013) 143-148.]. Wang et al prepared MoSi by supersonic atmospheric plasma spraying 2 -Y 2 O 3 The composite coating has a compact microstructure, good adhesion on the SiC transition layer and no obvious defect at the interface, so that the Oxidation resistance of the composite coating is effectively improved at 1500 ℃ (Wang Chang-Cong, li Ke-Zhi, he Dan-Yang, et al, oxidation floor and mechanism of MoSi 2 -Y 2 O 3 composite coating fabricated by supersonic atmospheric plasma spraying. 2020, 506(C).]. Direct synthesis of MoSi with self-healing performance 2 /Y 2 O 3 Microcapsules of core-shell structure have not been reported. The synthesized microcapsule has excellent oxidation resistance, thereby having wide application prospect.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for preparing a Glass-MoSi2@ Y2O3-SiC oxidation-resistant coating on the surface of a carbon/carbon composite material, which can form a compact coating on the surface of the C/C composite material, and can realize self-healing oxidation-resistant coating and thermal shock resistance in a high-temperature environment.
In order to achieve the purpose, the invention adopts the following technical scheme:
Glass-MoSi prepared on surface of carbon/carbon composite material 2 @Y 2 O 3 -a method of oxidation resistant coating of SiC comprising the steps of:
step one, moSi preparation 2 @Y 2 O 3 Core-shell structure microcapsules:
1) Mixing MoSi 2 Adding the powder into a conical flask, mixing isopropanol and absolute ethyl alcohol, pouring into the conical flask, and performing ultrasonic oscillation to obtain MoSi 2 Suspension A with the mass concentration of 10-20 g/L;
wherein the volume ratio of the isopropanol to the absolute ethyl alcohol is (0~4): 1;
2) Adding yttrium nitrate, urea and polyethylene glycol 4000 into the suspension A, and stirring to uniformly disperse the yttrium nitrate, urea and polyethylene glycol 4000 to obtain a suspension B;
wherein the molar ratio of yttrium nitrate to urea is 1 (1~8); the mass concentration of yttrium nitrate is 20 to 40g/L; the mass concentration of the polyethylene glycol 4000 is 0.01 to 0.04g/mL;
3) Putting the obtained suspension B into a hydrothermal kettle, heating and stirring for 2 to 5 hours at the temperature of 80 to 150 ℃, and then carrying out centrifugal separation on the obtained product and washing to obtain a product C;
4) Drying the product C separated in the step 3), putting the product C into a tube furnace, and keeping the temperature for 2 to 3 hours at 500 to 800 ℃ under the argon atmosphere to obtain a final product D, namely MoSi 2 @Y 2 O 3 Microcapsules;
step two, preparing a SiC inner coating of the carbon/carbon composite material sample:
burying the carbon/carbon composite material into the mixed powder of the graphite crucible, so that the mixed powder completely covers the carbon/carbon composite material;
the mixed powder comprises, by mass, 40 to 60 parts of silicon powder, 20 to 40 parts of graphite powder and 5 to 20 parts of alumina powder;
putting the graphite crucible into a reaction furnace, carrying out vacuum treatment on the reaction furnace, introducing argon, heating the reaction furnace from room temperature to 1900-2200 ℃ at the speed of 5-20 ℃/min in the whole process under the protection of the argon, keeping the temperature for 1~4 hours, then closing a power supply, and naturally cooling the reaction furnace to the room temperature to obtain the carbon/carbon composite material with the SiC inner coating on the surface;
step three, preparing MoSi of carbon/carbon composite material by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 Intermediate coating of core-shell structure microcapsule:
MoSi 2 @Y 2 O 3 suspension preparation: self-made MoSi 2 @Y 2 O 3 Adding the core-shell structure microcapsule powder into an isopropanol solution to ensure that the mass concentration is as follows: 10 to 40g/L, and magnetically stirring for 12 hours;
adding iodine to ensure that the mass concentration of iodine is 0-3g/L, magnetically stirring for 30min, ultrasonically oscillating for 30min, and finally magnetically stirring for 24h to obtain MoSi 2 @Y 2 O 3 A suspension;
mixing MoSi 2 @Y 2 O 3 Placing the suspension in a self-made hydrothermal electrodeposition device for preparation, taking the carbon/carbon composite material containing the SiC inner coating prepared in the step two as a negative electrode, and carrying out hydrothermal electrodeposition for 20-60min under the conditions that the deposition voltage is 10-30V and the hydrothermal temperature is 80-160 ℃; repeating the deposition for 3-5 times to realize MoSi 2 @Y 2 O 3 Uniformly depositing core-shell structure microcapsules on the surface of a carbon/carbon composite material containing a SiC inner coating;
step four, preparing glass powder:
mixing 50-75% of silicon dioxide, 15-30% of boron oxide and 5-20% of alumina powder according to mass percentage, carrying out ball milling and sieving, then calcining for 2-5 h at 1000-1500 ℃, and carrying out ball milling and sieving to obtain glass powder;
step five, preparing the glass external coating of the carbon/carbon composite material sample:
mixing the glass powder prepared in the fourth step with molybdenum disilicide powder according to the mass ratio of (4~8): 1, diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, and brushing the slurry on MoSi prepared in the third step by using a brush 2 @Y 2 O 3 The surface of the-SiC-carbon/carbon composite material is then insulated for 2 to 6min at 1400 ℃ in argon atmosphere to finally obtain compactGlass-MoSi of 2 @Y 2 O 3 A C/C composite material high-temperature oxidation resistant coating of-SiC.
Preferably, the ultrasonic oscillation in the step one is to put the suspension into an ultrasonic generator of 200 to 300W and oscillate for 30 to 60min.
Preferably, the stirring in the step one is performed for 1 to 3h by using a magnetic stirrer.
Preferably, the washing in the first step is 2~5 times by respectively using distilled water and absolute ethyl alcohol.
Preferably, the drying in the step one is carried out in an oven at 60 to 80 ℃ for 1 to 3 hours.
Compared with the prior art, the invention has the following technical effects:
the MoSi is synthesized and prepared by a solvothermal method-solid phase sintering method 2 @Y 2 O 3 The microcapsule is applied to the surface of the C/C composite material, has good compatibility with a matrix, is used for relieving the problem of easy cracking of a ceramic coating caused by thermal mismatch, and improves the oxidation resistance of the carbon/carbon composite material; moSi at high temperature 2 Oxidized to form SiO 2 ，SiO 2 And Y 2 O 3 The formation of yttrium silicate whiskers is reacted, and the toughening of the whiskers can prevent the coating from further cracking; at the same time increase SiO 2 The viscosity of the Glass is reduced, so that the diffusion rate of oxygen is reduced, and the self-healing effect is achieved, and the Glass-MoSi prepared by the method 2 @Y 2 O 3 The surface of the-SiC composite coating is compact, has no cracks or holes, and can effectively prevent oxygen from permeating into the carbon oxide/carbon matrix; a compact coating can be formed on the surface of the C/C composite material, and the coating can self-repair and self-heal in a high-temperature environment and has strong oxidation resistance and thermal shock resistance;
the preparation method has the advantages of simple preparation process, easily controlled conditions, low production cost and easy industrial production.
Drawings
FIG. 1 is a Glass-MoSi prepared by the method of the present invention 2 @Y 2 O 3 -surface XRD pattern of SiC oxidation resistant coating;
FIG. 2 is the present inventionMoSi prepared by the method of the invention 2 @Y 2 O 3 SEM image of microcapsules;
FIG. 3 is a Glass-MoSi prepared by the method of the present invention 2 @Y 2 O 3 -surface topography SEM image of SiC oxidation resistant coating;
FIG. 4 is a Glass-MoSi prepared by the method of the present invention 2 @Y 2 O 3 -static oxidation profile of SiC oxidation resistant coating samples in air at 1773K;
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1:
step one, moSi preparation 2 @Y 2 O 3 Core-shell structure microcapsules:
1) 1g of MoSi 2 Adding the powder into a conical flask, mixing 50mL of isopropanol and absolute ethyl alcohol, pouring the mixture into the conical flask, placing the suspension into a 300W ultrasonic generator, and oscillating for 30min to obtain MoSi 2 Suspension A with the mass concentration of 20g/L;
wherein the volume ratio of the isopropanol to the absolute ethyl alcohol is 4:1;
2) Adding 1.375g of yttrium nitrate, 2.4g of urea and polyethylene glycol 4000 into the suspension A, and stirring for 2 hours by using a magnetic stirrer to uniformly disperse the mixture to obtain a suspension B;
wherein the molar ratio of yttrium nitrate to urea is 1:8; the mass concentration of yttrium nitrate is 27.5g/L; the mass concentration of the polyethylene glycol 4000 is 0.025g/mL;
3) Putting the obtained suspension B into a hydrothermal kettle, heating and stirring at 120 ℃ for 3 hours, then carrying out centrifugal separation on the obtained product, and washing the product for 5 times by using distilled water and absolute ethyl alcohol respectively to obtain a product C;
4) Drying the product C separated in the step 3) in a 60 ℃ drying oven for 3h, then putting the product C into a tube furnace, and keeping the temperature at 800 ℃ for 2h under the argon atmosphere to obtain a final product D, namely MoSi 2 @Y 2 O 3 Microcapsules;
step two, preparing a SiC inner coating of the carbon/carbon composite material sample:
burying the carbon/carbon composite material into the mixed powder of the graphite crucible, so that the mixed powder completely covers the carbon/carbon composite material;
the mixed powder comprises 60 parts of silicon powder, 30 parts of graphite powder and 10 parts of alumina powder in parts by mass;
putting the graphite crucible into a reaction furnace, carrying out vacuum treatment on the reaction furnace, introducing argon, heating the reaction furnace to 2200 ℃ from room temperature at the speed of 10 ℃/min under the protection of argon, keeping the temperature for 2 hours, then turning off a power supply, and naturally cooling the reaction furnace to room temperature to obtain the carbon/carbon composite material with the SiC inner coating on the surface;
step three, preparing MoSi of carbon/carbon composite material by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 Intermediate coating of core-shell structure microcapsule:
MoSi 2 @Y 2 O 3 suspension preparation: self-made MoSi 2 @Y 2 O 3 Adding the core-shell structure microcapsule powder into an isopropanol solution to ensure that the mass concentration is as follows: 30g/L, and stirring for 12 hours by magnetic force;
adding iodine to make its mass concentration be 2g/L, magnetically stirring for 30min, ultrasonically oscillating for 30min, and magnetically stirring for 24 hr to obtain MoSi 2 @Y 2 O 3 A suspension;
mixing MoSi 2 @Y 2 O 3 Placing the suspension in a self-made hydrothermal electrodeposition device for preparation, taking the carbon/carbon composite material containing the SiC inner coating prepared in the step two as a negative electrode, and carrying out hydrothermal electrodeposition for 40min under the conditions that the deposition voltage is 25V and the hydrothermal temperature is 100 ℃; repeating the deposition for 3 times to realize MoSi 2 @Y 2 O 3 Uniformly depositing core-shell structure microcapsules on the surface of a carbon/carbon composite material containing a SiC inner coating;
step four, preparing glass powder:
mixing 65% of silicon dioxide, 20% of boron oxide and 15% of alumina powder according to the mass percentage, carrying out ball milling and sieving, then calcining for 3 hours at 1300 ℃, and carrying out ball milling and sieving to obtain glass powder;
step five, preparing the glass external coating of the carbon/carbon composite material sample:
mixing the glass powder prepared in the fourth step with molybdenum disilicide powder according to the mass ratio of 4:1, diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, and brushing the slurry on MoSi prepared in the third step by using a brush 2 @Y 2 O 3 The surface of the-SiC-carbon/carbon composite material is then subjected to heat preservation for 4min at 1400 ℃ in an argon atmosphere, and finally the compact Glass-MoSi is obtained 2 @Y 2 O 3 A C/C composite material high-temperature oxidation resistant coating of-SiC.
Example 2:
step one, moSi preparation 2 @Y 2 O 3 Core-shell structure microcapsules:
1) 0.5g of MoSi 2 Adding the powder into a conical flask, mixing 50mL of isopropanol and absolute ethyl alcohol, pouring the mixture into the conical flask, placing the suspension into a 200W ultrasonic generator, and vibrating for 60min to obtain MoSi 2 Suspension A with the mass concentration of 10 g/L;
wherein the volume ratio of the isopropanol to the absolute ethyl alcohol is 2:1;
2) Adding yttrium nitrate, urea and polyethylene glycol 4000 into the suspension A, and stirring for 3 hours by using a magnetic stirrer to uniformly disperse the yttrium nitrate, the urea and the polyethylene glycol 4000 to obtain a suspension B;
wherein the molar ratio of yttrium nitrate to urea is 1:6; the mass concentration of yttrium nitrate is 20g/L; the mass concentration of the polyethylene glycol 4000 is 0.01g/mL;
3) Putting the obtained suspension B into a hydrothermal kettle, heating and stirring at 80 ℃ for 5 hours, then carrying out centrifugal separation on the obtained product, and washing the product for 3 times by using distilled water and absolute ethyl alcohol respectively to obtain a product C;
4) Drying the product C separated in the step 3) in an oven at 80 ℃ for 1h, putting the product C into a tube furnace, and keeping the temperature at 600 ℃ for 2.5h under the argon atmosphere to obtain a final product D, namely MoSi 2 @Y 2 O 3 Microcapsules;
step two, preparing a SiC inner coating of the carbon/carbon composite material sample:
burying the carbon/carbon composite material into the mixed powder of the graphite crucible, so that the mixed powder completely covers the carbon/carbon composite material;
the mixed powder comprises 40 parts of silicon powder, 20 parts of graphite powder and 5 parts of alumina powder in parts by mass;
placing the graphite crucible into a reaction furnace, carrying out vacuum treatment on the reaction furnace, introducing argon, heating the reaction furnace to 1900 ℃ from room temperature at the speed of 20 ℃/min under the protection of argon, keeping the temperature for 4 hours, then turning off a power supply, and naturally cooling the reaction furnace to room temperature to obtain the carbon/carbon composite material with the SiC inner coating on the surface;
step three, preparing MoSi of carbon/carbon composite material by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 Intermediate coating of core-shell structure microcapsule:
MoSi 2 @Y 2 O 3 suspension preparation: self-made MoSi 2 @Y 2 O 3 Adding the core-shell structure microcapsule powder into an isopropanol solution to ensure that the mass concentration is as follows: 10g/L, and stirring for 12 hours by magnetic force;
adding iodine to make its mass concentration be 3g/L, magnetically stirring for 30min, ultrasonically oscillating for 30min, and magnetically stirring for 24 hr to obtain MoSi 2 @Y 2 O 3 A suspension;
mixing MoSi 2 @Y 2 O 3 Placing the suspension in a self-made hydrothermal electrodeposition device for preparation, taking the carbon/carbon composite material containing the SiC inner coating prepared in the step two as a negative electrode, and carrying out hydrothermal electrodeposition for 60min under the conditions that the deposition voltage is 30V and the hydrothermal temperature is 80 ℃; the deposition is repeated for 5 times to realize MoSi 2 @Y 2 O 3 Uniformly depositing core-shell structure microcapsules on the surface of a carbon/carbon composite material containing a SiC inner coating;
step four, preparing glass powder:
mixing 75% of silicon dioxide, 15% of boron oxide and 10% of alumina powder according to the mass percentage, carrying out ball milling and sieving, then calcining for 5 hours at 1000 ℃, and carrying out ball milling and sieving to obtain glass powder;
step five, preparing the glass external coating of the carbon/carbon composite material sample:
mixing the glass powder prepared in the step four with molybdenum disilicide powder according to the mass ratio of 8:1,diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, and brushing the slurry on the MoSi prepared in the step three by using a brush 2 @Y 2 O 3 The surface of the-SiC-carbon/carbon composite material is then subjected to heat preservation for 2min at 1400 ℃ in an argon atmosphere, and finally the compact Glass-MoSi is obtained 2 @Y 2 O 3 A C/C composite material high-temperature oxidation resistant coating of-SiC.
Example 3:
step one, moSi preparation 2 @Y 2 O 3 Core-shell structure microcapsules:
1) 0.75g of MoSi 2 Adding the powder into a conical flask, mixing 50mL of absolute ethyl alcohol, pouring into the conical flask, placing the suspension into a 250W ultrasonic generator, and vibrating for 50min to obtain MoSi 2 Suspension A with the mass concentration of 15 g/L;
2) Adding yttrium nitrate, urea and polyethylene glycol 4000 into the suspension A, and stirring for 1h by using a magnetic stirrer to uniformly disperse the yttrium nitrate, the urea and the polyethylene glycol 4000 to obtain a suspension B;
wherein the molar ratio of yttrium nitrate to urea is 1; the mass concentration of yttrium nitrate is 40g/L; the mass concentration of the polyethylene glycol 4000 is 0.04g/mL;
3) Putting the obtained suspension B into a hydrothermal kettle, heating and stirring for 2 hours at 150 ℃, then carrying out centrifugal separation on the obtained product, and washing the product for 4 times by using distilled water and absolute ethyl alcohol respectively to obtain a product C;
4) Drying the product C separated in the step 3) in a 70 ℃ drying oven for 2h, putting the product C into a tube furnace, and keeping the temperature at 500 ℃ for 3h under the argon atmosphere to obtain a final product D, namely MoSi 2 @Y 2 O 3 Microcapsules;
step two, preparing a SiC inner coating of the carbon/carbon composite material sample:
burying the carbon/carbon composite material into the mixed powder of the graphite crucible, so that the mixed powder completely covers the carbon/carbon composite material;
the mixed powder comprises 50 parts of silicon powder, 40 parts of graphite powder and 20 parts of alumina powder in parts by mass;
putting the graphite crucible into a reaction furnace, carrying out vacuum treatment on the reaction furnace, introducing argon, heating the reaction furnace to 2000 ℃ from room temperature at the speed of 5 ℃/min under the protection of argon, keeping the temperature for 1 hour, then turning off a power supply, and naturally cooling the reaction furnace to room temperature to obtain the carbon/carbon composite material with the SiC inner coating on the surface;
step three, preparing MoSi of carbon/carbon composite material by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 Intermediate coating of core-shell structure microcapsule:
MoSi 2 @Y 2 O 3 suspension preparation: self-made MoSi 2 @Y 2 O 3 Adding the core-shell structure microcapsule powder into an isopropanol solution to ensure that the mass concentration is as follows: 40g/L, and stirring for 12 hours by magnetic force;
adding iodine to make its mass concentration be 1g/L, magnetically stirring for 30min, ultrasonically oscillating for 30min, and magnetically stirring for 24 hr to obtain MoSi 2 @Y 2 O 3 A suspension;
mixing MoSi 2 @Y 2 O 3 Placing the suspension in a self-made hydrothermal electrodeposition device for preparation, taking the carbon/carbon composite material containing the SiC inner coating prepared in the step two as a negative electrode, and carrying out hydrothermal electrodeposition for 20min under the conditions of deposition voltage of 10V and hydrothermal temperature of 160 ℃; the deposition is repeated for 4 times to realize MoSi 2 @Y 2 O 3 Uniformly depositing core-shell structure microcapsules on the surface of a carbon/carbon composite material containing a SiC inner coating;
step four, preparing glass powder:
mixing 50% of silicon dioxide, 30% of boron oxide and 20% of alumina powder according to mass percent, carrying out ball milling and sieving, calcining for 2 hours at 1500 ℃, and carrying out ball milling and sieving to obtain glass powder;
step five, preparing the glass external coating of the carbon/carbon composite material sample:
mixing the glass powder prepared in the fourth step with molybdenum disilicide powder according to the mass ratio of 6:1, diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, and brushing the slurry on MoSi prepared in the third step by using a brush 2 @Y 2 O 3 The surface of the-SiC-carbon/carbon composite material is then subjected to heat preservation for 6min at 1400 ℃ in an argon atmosphere to finally obtain compact Glass-MoSi 2 @Y 2 O 3 A C/C composite material high-temperature oxidation resistant coating of-SiC.
Example 4:
step one, moSi preparation 2 @Y 2 O 3 Core-shell structure microcapsules:
1) Mixing MoSi 2 Adding the powder into a conical flask, mixing isopropanol and anhydrous ethanol, pouring into the conical flask, placing the suspension into a 250W ultrasonic generator, and shaking for 50min to obtain MoSi 2 Suspension A with the mass concentration of 18 g/L;
wherein the volume ratio of the isopropanol to the absolute ethyl alcohol is 3:1;
2) Adding yttrium nitrate, urea and polyethylene glycol 4000 into the suspension A, and stirring for 3 hours by using a magnetic stirrer to uniformly disperse the yttrium nitrate, the urea and the polyethylene glycol 4000 to obtain a suspension B;
wherein the molar ratio of yttrium nitrate to urea is 1:2; the mass concentration of yttrium nitrate is 25g/L; the mass concentration of the polyethylene glycol 4000 is 0.03g/mL;
3) Putting the obtained suspension B into a hydrothermal kettle, heating and stirring for 3h at 100 ℃, then carrying out centrifugal separation on the obtained product, and washing the product for 5 times by using distilled water and absolute ethyl alcohol respectively to obtain a product C;
4) Drying the product C separated in the step 3) in a 70 ℃ drying oven for 2h, putting the product C into a tube furnace, and keeping the temperature at 700 ℃ for 2.5h under the argon atmosphere to obtain a final product D, namely MoSi 2 @Y 2 O 3 Microcapsules;
step two, preparing a SiC inner coating of the carbon/carbon composite material sample:
burying the carbon/carbon composite material into the mixed powder of the graphite crucible, so that the mixed powder completely covers the carbon/carbon composite material;
the mixed powder comprises 55 parts of silicon powder, 30 parts of graphite powder and 15 parts of alumina powder in parts by mass;
putting the graphite crucible into a reaction furnace, carrying out vacuum treatment on the reaction furnace, introducing argon, heating the reaction furnace to 2000 ℃ from room temperature at a speed of 15 ℃/min under the protection of argon, keeping the temperature for 3 hours, then turning off a power supply, and naturally cooling the reaction furnace to room temperature to obtain the carbon/carbon composite material with the SiC inner coating on the surface;
step three, preparing MoSi of carbon/carbon composite material by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 Intermediate coating of core-shell structure microcapsule:
MoSi 2 @Y 2 O 3 suspension preparation: self-made MoSi 2 @Y 2 O 3 Adding the core-shell structure microcapsule powder into an isopropanol solution to ensure that the mass concentration is as follows: 25g/L, magnetically stirring for 12h, then ultrasonically shaking for 30min, and finally magnetically stirring for 24h to obtain MoSi 2 @Y 2 O 3 A suspension;
mixing MoSi 2 @Y 2 O 3 Placing the suspension in a self-made hydrothermal electrodeposition device for preparation, taking the carbon/carbon composite material containing the SiC inner coating prepared in the step two as a negative electrode, and carrying out hydrothermal electrodeposition for 50min under the conditions of deposition voltage of 30V and hydrothermal temperature of 800 ℃; repeating the deposition for 3 times to realize MoSi 2 @Y 2 O 3 Uniformly depositing core-shell structure microcapsules on the surface of a carbon/carbon composite material containing a SiC inner coating;
step four, preparing glass powder:
mixing 70% of silicon dioxide, 20% of boron oxide and 10% of alumina powder according to mass percent, carrying out ball milling and sieving, calcining for 2.5h at 1300 ℃, and carrying out ball milling and sieving to obtain glass powder;
step five, preparing the glass external coating of the carbon/carbon composite material sample:
mixing the glass powder prepared in the fourth step with molybdenum disilicide powder according to the mass ratio of 5:1, diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, and brushing the slurry on MoSi prepared in the third step by using a brush 2 @Y 2 O 3 The surface of the-SiC-carbon/carbon composite material is then subjected to heat preservation for 4min at 1400 ℃ in an argon atmosphere, and finally the compact Glass-MoSi is obtained 2 @Y 2 O 3 A C/C composite material high-temperature oxidation resistant coating of-SiC.
Example 5:
1) 0.75g of MoSi 2 The powder was added to an Erlenmeyer flask and 50mL of anhydrousMixing with ethanol, pouring into a conical flask, placing the suspension into a 250W ultrasonic generator, and shaking for 50min to obtain MoSi 2 Suspension A with the mass concentration of 15 g/L;
wherein the volume ratio of the isopropanol to the absolute ethyl alcohol is 2:1;
2) Adding yttrium nitrate, urea and polyethylene glycol 4000 into the suspension A, and stirring for 1h by using a magnetic stirrer to uniformly disperse the yttrium nitrate, the urea and the polyethylene glycol 4000 to obtain a suspension B;
wherein the molar ratio of yttrium nitrate to urea is 1:1; the mass concentration of yttrium nitrate is 30g/L; the mass concentration of the polyethylene glycol 4000 is 0.015g/mL;
3) Putting the obtained suspension B into a hydrothermal kettle, heating and stirring at 120 ℃ for 3 hours, then carrying out centrifugal separation on the obtained product, and washing the product for 2 times by using distilled water and absolute ethyl alcohol respectively to obtain a product C;
4) Drying the product C separated in the step 3) in a 70 ℃ drying oven for 2h, putting the product C into a tubular furnace, and keeping the temperature for 3h at 600 ℃ under the argon atmosphere to obtain a final product D, namely MoSi 2 @Y 2 O 3 Microcapsules;
step two, preparing a SiC inner coating of the carbon/carbon composite material sample:
burying the carbon/carbon composite material into the mixed powder of the graphite crucible, so that the mixed powder completely covers the carbon/carbon composite material;
the mixed powder comprises 60 parts of silicon powder, 2-40 parts of graphite powder and 10 parts of alumina powder in parts by mass;
putting the graphite crucible into a reaction furnace, carrying out vacuum treatment on the reaction furnace, introducing argon, heating the reaction furnace to 2200 ℃ from room temperature at the speed of 5 ℃/min under the protection of argon, keeping the temperature for 4 hours, then turning off a power supply, and naturally cooling the reaction furnace to room temperature to obtain the carbon/carbon composite material with the SiC inner coating on the surface;
step three, preparing MoSi of carbon/carbon composite material by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 Intermediate coating of core-shell structure microcapsule:
MoSi 2 @Y 2 O 3 suspension preparation: self-made MoSi 2 @Y 2 O 3 Adding the core-shell structure microcapsule powder into an isopropanol solution to ensure that the mass concentration is as follows: 30g/L, and stirring for 12 hours by magnetic force;
adding iodine to make its mass concentration be 2g/L, magnetically stirring for 30min, ultrasonically oscillating for 30min, and magnetically stirring for 24 hr to obtain MoSi 2 @Y 2 O 3 A suspension;
mixing MoSi 2 @Y 2 O 3 Placing the suspension in a self-made hydrothermal electrodeposition device for preparation, taking the carbon/carbon composite material containing the SiC inner coating prepared in the step two as a negative electrode, and carrying out hydrothermal electrodeposition for 30min under the conditions of deposition voltage of 30V and hydrothermal temperature of 140 ℃; the deposition is repeated for 4 times to realize MoSi 2 @Y 2 O 3 Uniformly depositing core-shell structure microcapsules on the surface of a carbon/carbon composite material containing a SiC inner coating;
step four, preparing glass powder:
mixing 60% of silicon dioxide, 30% of boron oxide and 10% of alumina powder according to the mass percentage, carrying out ball milling and sieving, then calcining for 4 hours at 1200 ℃, and carrying out ball milling and sieving to obtain glass powder;
step five, preparing the glass external coating of the carbon/carbon composite material sample:
mixing the glass powder prepared in the fourth step with molybdenum disilicide powder according to the mass ratio of 5:1, diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, and brushing the slurry on MoSi prepared in the third step by using a brush 2 @Y 2 O 3 The surface of the-SiC-carbon/carbon composite material is then insulated for 3min at 1400 ℃ in the argon atmosphere, and finally, the compact Glass-MoSi is obtained 2 @Y 2 O 3 A C/C composite material high-temperature oxidation resistant coating of-SiC.
FIG. 1 is a Glass-MoSi prepared in example 1 of the present invention 2 @Y 2 O 3 -surface XRD pattern of SiC oxidation resistant coating. As can be seen from FIG. 1, the surface coating is made of MoSi 2 Phase and SiO 2 Glass phase two-phase composition;
FIG. 2 shows MoSi prepared by the method of the present invention 2 @Y 2 O 3 SEM image of microcapsules. As can be seen from FIG. 2, Y is in the form of a sheet 2 O 3 Coated with MoSi 2 And (4) particles, forming a core-shell structure.
FIG. 3 is a Glass-MoSi prepared in example 1 of the present invention 2 @Y 2 O 3 SEM image of surface appearance of the SiC oxidation resistant coating. As can be seen from FIG. 3, the prepared composite coating has a compact surface without holes and cracks.
FIG. 4 shows Glass-MoSi prepared in example 1 of the present invention 2 @Y 2 O 3 Static oxidation profile of — SiC oxidation resistant coating samples in air at 1773K. As can be seen from fig. 4, the weight loss rate of the sample in the first 30h rapidly increased, which may be due to a large amount of loss of the outermost glass sealing layer due to high temperature; the weight loss rate of the sample after 30h was relatively stable, probably due to the MoSi of the intermediate layer 2 @Y 2 O 3 The microcapsules function, the crack propagation of the coating is hindered by the formation of yttrium silicate whiskers, so that the formation of penetrating cracks is difficult, and SiO is also increased 2 Viscosity of the glass, thereby reducing the diffusion rate of oxygen; the weight loss rate after oxidation of 182 h in 1773k air atmosphere is only 2.02%, and the carbon/carbon matrix is not oxidized, thus showing that the prepared Glass-MoSi has high purity 2 @Y 2 O 3 the-SiC composite coating has good oxidation resistance.
Claims (5)
1. Glass-MoSi prepared on surface of carbon/carbon composite material 2 @Y 2 O 3 -a method for oxidation-resistant coating of SiC, characterized in that it comprises the following steps:
step one, moSi preparation 2 @Y 2 O 3 Core-shell structure microcapsules:
1) Mixing MoSi 2 Adding the powder into a conical flask, mixing isopropanol and absolute ethyl alcohol, pouring into the conical flask, and performing ultrasonic oscillation to obtain MoSi 2 Suspension A with the mass concentration of 10-20 g/L;
wherein the volume ratio of the isopropanol to the absolute ethyl alcohol is (0~4): 1;
2) Adding yttrium nitrate, urea and polyethylene glycol 4000 into the suspension A, and stirring to uniformly disperse the yttrium nitrate, urea and polyethylene glycol 4000 to obtain a suspension B;
wherein the molar ratio of yttrium nitrate to urea is 1 (1~8); the mass concentration of yttrium nitrate is 20 to 40g/L; the mass concentration of the polyethylene glycol 4000 is 0.01 to 0.04g/mL;
3) Putting the obtained suspension B into a hydrothermal kettle, heating and stirring for 2 to 5 hours at the temperature of 80 to 150 ℃, and then carrying out centrifugal separation on the obtained product and washing to obtain a product C;
4) Drying the product C separated in the step 3), putting the product C into a tube furnace, and keeping the temperature for 2 to 3 hours at 500 to 800 ℃ under the argon atmosphere to obtain a final product D, namely MoSi 2 @Y 2 O 3 Microcapsules;
step two, preparing a SiC inner coating of the carbon/carbon composite material sample:
burying the carbon/carbon composite material into the mixed powder of the graphite crucible, so that the mixed powder completely covers the carbon/carbon composite material;
the mixed powder comprises, by mass, 40 to 60 parts of silicon powder, 20 to 40 parts of graphite powder and 5 to 20 parts of alumina powder;
putting the graphite crucible into a reaction furnace, carrying out vacuum treatment on the reaction furnace, introducing argon, heating the reaction furnace from room temperature to 1900-2200 ℃ at the speed of 5-20 ℃/min in the whole process under the protection of the argon, keeping the temperature for 1~4 hours, then closing a power supply, and naturally cooling the reaction furnace to the room temperature to obtain the carbon/carbon composite material with the SiC inner coating on the surface;
step three, preparing MoSi of carbon/carbon composite material by using self-produced water thermoelectric deposition equipment 2 @Y 2 O 3 Intermediate coating of core-shell structure microcapsule:
MoSi 2 @Y 2 O 3 suspension preparation: self-made MoSi 2 @Y 2 O 3 Adding the core-shell structure microcapsule powder into an isopropanol solution to ensure that the mass concentration is as follows: 10 to 40g/L, and magnetically stirring for 12 hours;
adding iodine to enable the mass concentration of iodine to be 0-3g/L, magnetically stirring for 30min, ultrasonically oscillating for 30min, and finally magnetically stirring for 24h to obtain MoSi 2 @Y 2 O 3 A suspension;
mixing MoSi 2 @Y 2 O 3 The suspension is placed in a self-made hydrothermal electrodeposition device for preparationTaking the carbon/carbon composite material containing the SiC internal coating prepared in the step two as a negative electrode, and carrying out hydrothermal electrodeposition for 20 to 60min under the conditions that the deposition voltage is 10 to 30V and the hydrothermal temperature is 80 to 160 ℃; repeating the deposition for 3-5 times to realize MoSi 2 @Y 2 O 3 Uniformly depositing core-shell structure microcapsules on the surface of a carbon/carbon composite material containing a SiC inner coating;
step four, preparing glass powder:
mixing 50-75% of silicon dioxide, 15-30% of boron oxide and 5-20% of alumina powder according to mass percentage, carrying out ball milling and sieving, then calcining for 2-5 h at 1000-1500 ℃, and carrying out ball milling and sieving to obtain glass powder;
step five, preparing the glass external coating of the carbon/carbon composite material sample:
mixing the glass powder prepared in the fourth step with molybdenum disilicide powder according to the mass ratio of (4~8): 1, diluting the mixture into slightly flowing slurry by using absolute ethyl alcohol, and brushing the slurry on MoSi prepared in the third step by using a brush 2 @Y 2 O 3 The surface of the-SiC-carbon/carbon composite material is then insulated for 2 to 6min at 1400 ℃ in argon atmosphere, and finally the compact Glass-MoSi is obtained 2 @Y 2 O 3 A C/C composite material high-temperature oxidation resistant coating of-SiC.
2. The carbon/carbon composite material surface preparation Glass-MoSi according to claim 1 2 @Y 2 O 3 The method for preparing the SiC oxidation-resistant coating is characterized in that in the step one, the suspension is placed in an ultrasonic generator of 200-300W and vibrated for 30-60min through ultrasonic vibration.
3. The carbon/carbon composite material surface preparation Glass-MoSi according to claim 1 2 @Y 2 O 3 The method for preparing the-SiC oxidation-resistant coating is characterized in that stirring in the step one is performed for 1 to 3 hours by using a magnetic stirrer.
4. The carbon/carbon composite material surface preparation Glass-MoSi according to claim 1 2 @Y 2 O 3 Method for preparing-SiC oxidation-resistant coatingThe method is characterized in that the washing in the first step is 2~5 times by respectively washing with distilled water and absolute ethyl alcohol.
5. The method of claim 1, wherein the Glass-MoSi is prepared on the surface of the carbon/carbon composite material 2 @Y 2 O 3 The method for preparing the-SiC oxidation-resistant coating is characterized in that in the step one, the drying is carried out in an oven at the temperature of 60-80 ℃ for 1-3 h.
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| CN115745664B (en) * | 2022-08-29 | 2023-05-19 | 陕西科技大学 | Carbon/carbon composite Glass-MoSi 2 /Y 2 O 3 Preparation method of-SiC composite antioxidation coating |
| CN115745663B (en) * | 2022-08-29 | 2023-05-19 | 陕西科技大学 | Glass-MoSi on surface of carbon/carbon composite material 2 Preparation method of-SiC composite antioxidation coating |
| CN115636691A (en) * | 2022-11-01 | 2023-01-24 | 陕西科技大学 | Spherical coating MoSi 2 @Y 2 O 3 Core-shell structure microcapsule powder and preparation method and application thereof |
| CN115724456B (en) * | 2022-12-06 | 2024-04-02 | 陕西科技大学 | In-situ self-toughening rod-shaped coated MoSi 2 /Y 2 O 3 Powder and preparation method thereof |
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