CN114455968A - C/SiC-SiO2Composite material and preparation method thereof - Google Patents
C/SiC-SiO2Composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses C/SiC-SiO2The preparation method of the composite material comprises the following steps of (1) cleaning a carbon fiber fabric; (2) depositing a pyrolytic carbon interface layer; (3) high-temperature treatment; (4) carrying out vacuum impregnation, curing and cracking treatment on the SiC precursor for 2-7 times in a circulating manner to obtain a C/SiC blank; (5) dipping the C/SiC blank in vacuum by using silica sol, and then sequentially carrying out gelation, drying and heat treatment; (6) and (5) circulating until the weight gain rate of a single round is lower than 0.5%. The invention also discloses C/SiC-SiO2The composite material uses carbon fiber as reinforcement and SiC and SiO2As a substrate, pyrolytic carbon is used as an interface layer between the reinforcement and the substrate; SiC in the fiber bundle mainly plays a role in high-temperature bearing and fiber protection; SiO 22Mainly distributed among fiber bundles, so that porous SiC matrixes are connected into a compact wholeThe mechanical and ablation resistance of the material is improved in one step, and the obtained C/SiC-SiO2The composite material can be used as a heat-proof bearing integrated material and can be in service at high temperature.
Description
Technical Field
The invention relates to C/SiC-SiO2A ceramic matrix composite and a preparation method thereof belong to the technical field of thermostructural composite and preparation.
Background
The C/SiC is taken as a representative ceramic matrix composite material, and the C/SiC has important application in the aerospace field as a heat-proof load-bearing integrated material due to excellent high-temperature mechanics and ablation resistance. Among them, the C/SiC composite material has high technical maturity and stable and reliable performance, and becomes one of the most important material systems in the field of thermal structural materials. The C/SiC composite material has multiple preparation processes, a precursor impregnation cracking (PIP) process is low in preparation temperature, small in fiber damage, strong in process adaptability and low in equipment requirement, and has outstanding advantages in the aspect of large-size, special-shaped and thin-wall thermal structural member near net size forming, so that the C/SiC composite material has important application in the development of thermal structural products. However, the raw material SiC precursor used in the process reaches thousands of yuan per kilogram, and the utilization rate of the raw material is very low in the densification process of the special-shaped thermal structural member, so that the cost of the C/SiC composite material is high, and the wide application of the C/SiC composite material is seriously restricted.
In view of common structural characteristics and use conditions of a thermal structure product, related low-cost technical researches on the thermal structure material need to be carried out on the basis of a liquid phase method and a C/SiC material system, and the cost is obviously reduced on the basis of ensuring the high-temperature mechanics and the ablation resistance of the material.
Disclosure of Invention
The invention aims to overcome the defects and provides a C/SiC-SiO2The preparation method of the composite material comprises (1) cleaning the surface of the carbon fiber fabric; (2) depositing heat on the surface of a carbon fiber fabricCarbon interface layer decomposition; (3) carrying out high-temperature treatment; (4) carrying out vacuum impregnation, curing and cracking treatment on the SiC precursor for 2-7 times in a circulating manner to obtain a C/SiC blank; (5) dipping the C/SiC blank in vacuum by using silica sol, and then sequentially carrying out gelation, drying and heat treatment; (6) the step (5) is circulated until the weight gain rate of a single round is lower than 0.5 percent to obtain C/SiC-SiO2A composite material. The invention also provides C/SiC-SiO2The composite material uses carbon fiber as reinforcement and SiC and SiO2As a substrate, pyrolytic carbon is used as an interface layer between the reinforcement and the substrate; SiC in the fiber bundle mainly plays a role in high-temperature bearing and fiber protection; SiO 22The SiC porous material is mainly distributed among fiber bundles, so that porous SiC matrixes are connected into a compact whole, and the mechanical property and the ablation resistance of the material are further improved. The invention utilizes SiO2The high-temperature oxidation resistance and the mechanical property of the composite material are used as a matrix filling phase of the low-density C/SiC composite material to realize the densification of the composite material, and the obtained C/SiC-SiO2The composite material can be used as a heat-proof bearing integrated material and can be in service at high temperature.
In order to achieve the above purpose, the invention provides the following technical scheme:
C/SiC-SiO2The preparation method of the composite material comprises the following steps:
(1) cleaning the surface of the carbon fiber fabric;
(2) depositing a pyrolytic carbon interface layer on the surface of the carbon fiber fabric;
(3) carrying out high-temperature treatment at 1400-2500 ℃ on the product obtained in the last step;
(4) circularly carrying out vacuum impregnation, curing and cracking treatment on the SiC precursor for 2-7 times on the product obtained in the last step to obtain a C/SiC blank;
(5) dipping the C/SiC blank in vacuum by using silica sol, and then sequentially carrying out gelation, drying and heat treatment;
(6) the step (5) is circulated until the weight gain rate of a single round is lower than 0.5 percent to obtain C/SiC-SiO2A composite material.
Further, in the step (1), the carbon fiber adopted by the carbon fiber fabric is one or more of T300-1K, T300-3K or T700-12K, and the structure of the carbon fiber fabric is one or more of laying sewing, puncturing, needling sewing or orthogonal three directions;
in the step (1), the density of the carbon fiber fabric is more than 0.7g/cm3；
In the step (1), the method for cleaning the surface of the carbon fiber fabric comprises the steps of putting the carbon fiber fabric into heat treatment equipment, and heating to 400-1400 ℃ under the protection of inert gas.
Further, in the step (2), a pyrolytic carbon interface layer is deposited on the surface of the carbon fiber fabric by a chemical vapor deposition method, wherein the thickness of the pyrolytic carbon interface layer is 50 nm-2 μm.
Furthermore, in the step (3), the time for performing high-temperature treatment on the product obtained in the last step at 1400-2500 ℃ is more than 0.5 h.
Further, in the step (4), the curing temperature is above 150 ℃, and the cracking temperature is 800-1400 ℃.
Further, in the step (4), the SiC precursor is polycarbosilane solution or liquid polycarbosilane;
the ceramic yield of the SiC precursor is more than 40%, and the density of the ceramic powder generated by cracking the SiC precursor is 2.2g/cm3～2.5g/cm3。
Further, in the step (5), the temperature of the gel treatment is 80-100 ℃, and the temperature of the drying treatment is 120-150 ℃;
in the step (5), the heat treatment time is more than 0.5h, and the heat treatment method is to perform medium-low temperature treatment at 500-800 ℃ or medium-high temperature treatment at 1300-1500 ℃ under the protection of inert gas; in the step (6), in the process of 1-3 rounds of each cycle of the step (5), at least one round is subjected to medium-high temperature treatment at 1300-1500 ℃ during heat treatment.
Further, in the step (5), the silica sol is nano SiO2A colloidal dispersion liquid in which particles are dispersed in water;
the diameter of colloidal particles in the colloidal dispersion liquid is 10 nm-80 nm, and the diameter of nano SiO is2The mass fraction of the particles is 15-65%.
Further, in the vacuum impregnation treatment process in the step (4), the SiC precursor is immersed in the product obtained in the previous step, and the liquid level of the SiC precursor is 20mm or more higher than the highest point of the product obtained in the previous step;
and (5) in the vacuum impregnation treatment process, the silica sol is enabled to be submerged in the C/SiC blank, and the surface of the silica sol is 20mm above the highest point of the C/SiC blank.
C/SiC-SiO2Composite material, according to one of the above C/SiC-SiO2The composite material is prepared by taking carbon fiber as a reinforcement and SiC and SiO2As a substrate, pyrolytic carbon is used as an interface layer between the reinforcement and the substrate;
SiC is coated on the surface of the carbon fiber, and SiC and SiO are arranged in the fiber bundle2Mass ratio of > SiC and SiO between fiber bundles2The mass ratio of (A) to (B);
in the matrix, SiC and SiO2Is greater than 1/2.
Compared with the prior art, the invention has at least one of the following beneficial effects:
(1) the invention is C/SiC-SiO2In the preparation method of the composite material, SiC precursors and silica sol are adopted for successive impregnation, so that the content of SiC matrix in fiber bundles in the obtained composite material is relatively high, and SiO with certain high-temperature mechanical property and ablation resistance is utilized2Healing SiC matrix cracks and filling pores to obtain C/SiC-SiO2The composite material has good mechanical property and ablation resistance, and can be used as a thermal structure material;
(2) the invention utilizes silica sol to prepare C/SiC-SiO2The composite material comprises silica sol as main component, water and nanometer SiO2The particle and sol system is stable, the environment is friendly, the dipping process is simple, and the cost is only about 1 percent of that of the SiC precursor; in addition, because the utilization rate of the impregnation phase of large-size, thin-wall and special-shaped thermal structure products is low, the required dosage of the impregnation phase in each round is basically the same no matter how the compact state of the blank is, the cost of the impregnation phase used by the composite material is closely related to the compounding times of the C/SiC blank, and the invention adopts 2-7 roundsThe low-density C/SiC is used as a blank and is impregnated by silica sol to obtain compact C/SiC-SiO2Composite material, C/SiC-SiO of the invention, compared with C/SiC composite material obtained in at least 9 rounds in the prior art2On the premise of equivalent performance of the composite material, the cost of the matrix raw material can be reduced by 22-77%.
(3) The invention is C/SiC-SiO2Pyrolytic carbon interface layers with certain thicknesses are prepared on the surfaces of the composite material fibers, and the fibers and the interface layers are subjected to high-temperature treatment, so that the corrosion resistance of the fibers is improved; meanwhile, because the SiC precursor is preferentially impregnated, the formed SiC matrix is coated on the surface of the carbon fiber with the pyrolytic carbon interface layer, and SiO is below 1500 DEG C2The matrix can not damage the carbon fiber;
(4) the invention is C/SiC-SiO2The composite material has certain high-temperature mechanical and oxidation resistance, can be used as a thermal structural material to serve in high-temperature oxidation and bearing environments, and simultaneously, SiO is used2The raw material of the matrix is silica sol, so that the cost is low, and the cost of the C/SiC composite material can be obviously reduced;
(5) the invention can flexibly regulate and control SiC and SiO according to the use working condition2The distribution and relative content of the matrix ensure that the high-temperature mechanical property and the ablation resistance of the composite material meet the requirements;
(6) when the invention adopts silica sol to carry out densification, a heat treatment system is innovatively designed, the high-efficiency densification of the composite material can be realized, and SiO can be enabled2The matrix is sintered to improve the mechanical property.
Drawings
FIG. 1 shows a C/SiC-SiO of the present invention2SEM photograph of the composite material.
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The invention provides C/SiC-SiO obtained based on C/SiC composite material modification2A composite material. The composite material takes carbon fiber as a reinforcement, pyrolytic carbon as an interface layer, SiC and SiO2Is a substrate. Using low-density C/SiC composite material as blank, adopting sol-gel method to introduce SiO2The nanometer particle is prepared through soaking silica sol, heating to gel the sol, stoving and sintering to obtain SiO2The matrix is subjected to a plurality of rounds of cyclic sol dipping-gel-drying-sintering processes to form compact C/SiC-SiO2A composite material. On one hand, the cost of the silica sol is only about 1 percent of that of the SiC precursor, so that the cost of the raw material of the matrix can be greatly reduced by using the silica sol, and the development cost of the C/SiC composite material is further remarkably reduced. On the other hand, SiO2Has certain mechanical and oxidation resistance at high temperature, and SiO is formed by basically molding the SiC matrix skeleton in the low-density C/SiC composite material2The introduction of the composite material mainly plays roles in healing SiC matrix cracks and sealing and filling pores, so that the high-temperature mechanical property and the ablation resistance of the composite material are not obviously influenced, and the obtained C/SiC-SiO2The performance of the composite material in the aspects of strength, ablation resistance and the like is equivalent to that of a C/SiC composite material, and the composite material can be used as a thermal structural material to replace the C/SiC composite material in most scenes.
The invention relates to C/SiC-SiO2The preparation method of the composite material comprises the following steps:
(1) putting the carbon fiber fabric into heat treatment equipment, heating to 400-1400 ℃ under the protection of inert gas, and removing organic matters such as sizing agent and the like in the fabric to clean the surface of the fiber.
(2) And (3) putting the carbon fiber fabric without the organic matters into a chemical vapor deposition furnace, and depositing a pyrolytic carbon interface layer on the surface of the carbon fiber, wherein the thickness of the interface layer is 50 nm-2 mu m.
(3) The carbon fiber fabric with the interface layer deposited is treated at 1400-2500 deg.c to make the carbon fiber fabric possess high temperatureGraphitization of the carbon fiber and pyrolytic carbon interface layer, reduction of the bonding strength of the carbon fiber and pyrolytic carbon interface layer and the matrix, improvement of the toughness of the composite material, and alleviation of SiO2Corrosion phenomena to carbon fibers;
(4) and putting the fabric subjected to high-temperature treatment into a tool, vacuum impregnating the SiC precursor, curing at the temperature of more than 150 ℃, cracking at the temperature of 800-1400 ℃, and circulating the impregnation-curing-cracking process for 2-7 times to obtain the low-density C/SiC blank.
(5) Putting a low-density C/SiC blank into a tool, vacuum-impregnating silica sol, heating to 80-100 ℃ to gel the silica sol, heating to 120-150 ℃ to dry the blank with the gel, putting the dried blank into a heat treatment furnace, and performing heat treatment under the protection of inert gas, wherein the heat treatment has the function of enabling SiO to be thermally treated2The bound water was stripped and the pores opened to open the channels for the next round of dipping.
(6) And (5) circulating the step, and stopping compounding when the weight gain rate of the single round is lower than 0.5%. The obtained composite material is C/SiC-SiO2A composite material.
Furthermore, in the step (1), the carbon fiber and the fabric structure form thereof are not critical, wherein the carbon fiber may be T300-1K, T300-3K or T700-12K, etc., and the fabric structure form may be ply sewing, piercing, needle punching sewing or three-way orthogonal sewing, etc.
Further, in the step (1), the density of the carbon fiber fabric is up to 0.7g/cm3The above.
Further, in the step (4), the SiC precursor is polycarbosilane or liquid polycarbosilane, and when polycarbosilane is used for impregnation, a solvent is used for dissolution; the yield of the SiC precursor ceramic is above 40%, and the density of the ceramic powder generated by cracking the SiC precursor is 2.2g/cm3～2.5g/cm3。
Further, in the step (5), there are two heat treatment temperatures after silica sol impregnation, one is medium-low temperature treatment: 500-800 ℃, and the other is medium-high temperature treatment: 1300-1500 ℃; in the step (6), the treatment is carried out at least once at a high temperature every 1-3 rounds.
Further, in the step (5), the silica sol used is nano SiO2The colloidal dispersion liquid formed by dispersing the particles in water is colorless or milk white transparent liquid; the diameter of colloidal particles in the colloidal dispersion liquid is 10 nm-80 nm, and SiO is2The mass fraction of the silica sol is 15-65%, and the silica sol has the characteristics of no odor, no toxicity, good corrosion resistance and the like.
Further, in the steps (4) and (5), the used impregnation phase, namely the SiC precursor or the silica sol, should be sufficient, and after vacuum impregnation, the impregnation phase solution should completely cover the surface of the product and be higher than the highest point of the surface of the product by more than 20 mm.
As shown in figure 1, the invention relates to C/SiC-SiO2The composite material is prepared with carbon fiber as reinforcing body, pyrolytic carbon as interface layer, SiC and SiO2Composite material as matrix, SiC and SiO in composite material2Is higher than 1/2. Firstly, carrying out SiC precursor vacuum impregnation on a carbon fiber fabric, wherein SiC fully enters the fabric after 2-7 times, the surface of the carbon fiber is mainly coated by a SiC matrix, and the SiC matrix mainly plays a role in high-temperature bearing and fiber protection; then carrying out silica sol vacuum impregnation to ensure that SiO is generated2Fully filled into the inner pores and cracks of the composite material, and made of SiO2The porous SiC basal bodies are connected into a compact whole, and the function of further improving the mechanical property and the oxidation resistance is mainly played. Adopting a low-density C/SiC composite material as a blank, circularly dipping silica sol, drying and carrying out heat treatment to finally form compact C/SiC-SiO2The composite material has certain high-temperature mechanical and oxidation resistance, and can be used as a thermal structure material to serve in high-temperature oxidation and bearing environments. Meanwhile, because of SiO2The raw material of the matrix is silica sol, so that the cost is low, and the cost of the C/SiC composite material can be obviously reduced.
Example 1
Aiming at a hollow special-shaped structure product with the envelope of the external dimension of 1500m multiplied by 400mm multiplied by 50mm and the wall thickness of 3-10 mm, C/SiC-SiO is adopted2The composite material is developed. The method comprises the following specific development steps:
(1) according to the product drawing, adopting TWeaving the fabric by 300-3K carbon fiber and a layering-sewing process, sampling in a blank allowance area, and determining whether the density of the fabric meets 0.7g/cm3The above; putting the carbon fiber fabric meeting the requirements into heat treatment equipment, heating to 600 ℃ under the protection of argon, and removing organic matters such as sizing agents and the like in the fabric to clean the surface of the fiber.
(2) And (3) placing the fabric without the organic matters into a chemical vapor deposition furnace, and depositing a pyrolytic carbon interface layer on the surface of the carbon fiber, wherein the thickness of the interface layer is about 150 nm.
(3) And (3) carrying out high-temperature treatment on the deposited fabric, wherein the treatment temperature is 1500 ℃.
(4) Designing the size of an inner cavity of the dipping tool to 1550m multiplied by 450mm according to the size of a product, and then putting the fabric subjected to high-temperature treatment into the tool; and (4) sucking liquid polycarbosilane in vacuum, and stopping dipping when the liquid polycarbosilane covers the highest point of the product by about 20 mm. Taking out the fabric, putting the fabric into a shaping tool, heating to 200 ℃ for curing, putting the cured fabric into heat treatment equipment, and cracking at 1000 ℃. The dipping-curing-cracking process is circulated for 4 times to obtain the density of 1.54g/cm3A low density C/SiC blank.
(5) Putting the low-density C/SiC blank into a tool, and dipping SiO in vacuum2The mass fraction is 40% of silica sol, and the impregnation is stopped when the precursor covers about 20mm of the highest point of the blank. Then heating to 80 ℃ to make the silica sol gel, heating to 120 ℃ to dry the blank, putting the dried blank into a heat treatment furnace, and carrying out heat treatment under the protection of inert gas, wherein the heat treatment temperature is 600 ℃.
(6) And (5) a circulating step, namely selecting 20% by mass of silica sol, and controlling the temperature of the second round of heat treatment to be 1300 ℃.
(7) The step (6) is circulated until the weight gain of a certain turn is lower than 0.5 percent, and the compounding can be stopped to obtain C/SiC-SiO2A composite material.
In this example, the liquid polycarbosilane used has a density of about 0.95g/cm3The unit price is about 4000 yuan/kg, and the density of the silica sol is about 1.2g/cm3The unit price is about 40 yuan/kg; the volume of the impregnation phase used in each round was 48.8L; product composition 9 wheels (liquid poly-carbon)Silane dipping for 4 rounds and silica sol dipping for 5 rounds) to realize densification, and the cost of the dipping phase is reduced by about 55 percent.
The tensile strength of the obtained composite material at 1500 ℃ and high temperature is 255MPa, and reaches 89.5 percent of the strength data of the C/SiC composite material; when the temperature of the ablation surface of oxyacetylene reaches 1500 ℃, the linear ablation rate reaches 10-4The mm/s is equivalent to that of a C/SiC composite material.
Example 2
Aiming at a hollow special-shaped structure product with the envelope of the external dimension of 1800m multiplied by 500mm multiplied by 50mm and the wall thickness of 5mm, C/SiC-SiO is adopted2The composite material is developed. The method comprises the following specific development steps:
(1) according to the product drawing, weaving the fabric by adopting T300-1K fibers and a layering-sewing process, sampling in a blank allowance area, and determining whether the fabric density meets 0.7g/cm3The above; putting the carbon fiber fabric meeting the requirements into heat treatment equipment, heating to 600 ℃ under the protection of argon, and removing organic matters such as sizing agents and the like in the fabric to clean the surface of the fiber.
(2) And (3) placing the fabric without the organic matters into a chemical vapor deposition furnace, and depositing a pyrolytic carbon interface layer on the surface of the carbon fiber, wherein the thickness of the interface layer is about 500 nm.
(3) And (3) carrying out high-temperature treatment on the deposited fabric, wherein the treatment temperature is 2000 ℃.
(4) According to the size of a product, the size of an inner cavity of the dipping tool is designed to be 1850m multiplied by 550mm, and then the fabric after high-temperature treatment is put into the tool; and (4) sucking the polycarbosilane solution in vacuum, and stopping dipping when the polycarbosilane solution covers the highest point of the product by about 20 mm. Taking out the fabric, putting the fabric into a shaping tool, heating to 200 ℃ for curing, putting the cured fabric into heat treatment equipment, and cracking at 1200 ℃. The dipping-curing-cracking process is circulated for 2 rounds, and the density is 1.34g/cm3A low density C/SiC blank.
(5) And (3) putting the low-density C/SiC blank into a tool, vacuum-impregnating silica sol with the mass fraction of 30%, and stopping impregnation when the precursor covers about 20mm of the highest point of the blank. Then heating to 80 ℃ to make the silica sol gel, heating to 120 ℃ to dry the blank, putting the dried blank into a heat treatment furnace, and carrying out heat treatment under the protection of inert gas, wherein the heat treatment temperature is 600 ℃.
(6) And (5) circulating, wherein the temperature of the second round of heat treatment is 800 ℃, and the temperature of the third round of heat treatment is 1400 ℃.
(7) The step (6) is circulated until the weight gain of a certain turn is lower than 0.5 percent, and the compounding can be stopped to obtain C/SiC-SiO2A composite material.
In this example, the polycarbosilane solution used had a density of about 0.92g/cm3The unit price is about 3900 yuan/kg, and the silica sol density is about 1.2g/cm3The unit price is about 38 yuan/kg; the volume of the impregnation phase used in each round was 110L; the product is compact after being compounded for 9 rounds (2 rounds of carbosilane solution impregnation and 7 rounds of silica sol impregnation), and the cost of the impregnation phase is reduced by about 76.2 percent.
The tensile strength of the obtained composite material at the high temperature of 1400 ℃ is 363MPa, which reaches 92.1 percent of the strength data of the C/SiC composite material, and when the temperature of the oxyacetylene ablation surface reaches 1500 ℃, the linear ablation rate reaches 10-4The mm/s is equivalent to that of a C/SiC composite material.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Those skilled in the art will appreciate that those matters not described in detail in the present specification are well known in the art.
Claims (10)
1. C/SiC-SiO2The preparation method of the composite material is characterized by comprising the following steps:
(1) cleaning the surface of the carbon fiber fabric;
(2) depositing a pyrolytic carbon interface layer on the surface of the carbon fiber fabric;
(3) carrying out high-temperature treatment at 1400-2500 ℃ on the product obtained in the last step;
(4) circularly carrying out vacuum impregnation, curing and cracking treatment on the SiC precursor for 2-7 times on the product obtained in the last step to obtain a C/SiC blank;
(5) dipping the C/SiC blank in vacuum by using silica sol, and then sequentially carrying out gelation, drying and heat treatment;
(6) the step (5) is circulated until the weight gain rate of a single round is lower than 0.5 percent to obtain C/SiC-SiO2A composite material.
2. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the step (1), the carbon fiber adopted by the carbon fiber fabric is one or more of T300-1K, T300-3K or T700-12K, and the structure of the carbon fiber fabric is one or more of layering sewing, puncturing, needling sewing or orthogonal three-way;
in the step (1), the density of the carbon fiber fabric is more than 0.7g/cm3；
In the step (1), the method for cleaning the surface of the carbon fiber fabric comprises the steps of putting the carbon fiber fabric into heat treatment equipment, and heating to 400-1400 ℃ under the protection of inert gas.
3. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the step (2), a pyrolytic carbon interface layer is deposited on the surface of the carbon fiber fabric by a chemical vapor deposition method, and the thickness of the pyrolytic carbon interface layer is 50 nm-2 microns.
4. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the step (3), the time for performing high-temperature treatment on the product obtained in the last step at 1400-2500 ℃ is more than 0.5 h.
5. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the step (4), the curing temperature is more than 150 ℃, and the cracking is carried outThe temperature is 800-1400 ℃.
6. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the step (4), the SiC precursor is polycarbosilane solution or liquid polycarbosilane;
the ceramic yield of the SiC precursor is more than 40%, and the density of the ceramic powder generated by cracking the SiC precursor is 2.2g/cm3～2.5g/cm3。
7. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the step (5), the temperature of the gel treatment is 80-100 ℃, and the temperature of the drying treatment is 120-150 ℃;
in the step (5), the heat treatment time is more than 0.5h, and the heat treatment method is to perform medium-low temperature treatment at 500-800 ℃ or medium-high temperature treatment at 1300-1500 ℃ under the protection of inert gas; in the step (6), in the process of 1-3 rounds of each cycle of the step (5), at least one round is subjected to medium-high temperature treatment at 1300-1500 ℃ during heat treatment.
8. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the step (5), the silica sol is nano SiO2A colloidal dispersion liquid in which particles are dispersed in water;
the diameter of colloidal particles in the colloidal dispersion liquid is 10 nm-80 nm, and the diameter of nano SiO is2The mass fraction of the particles is 15-65%.
9. C/SiC-SiO according to claim 12The preparation method of the composite material is characterized in that in the vacuum impregnation treatment process in the step (4), the SiC precursor is immersed in the product obtained in the previous step, and the liquid level of the SiC precursor is 20mm or more higher than the highest point of the product obtained in the previous step;
and (5) in the vacuum impregnation treatment process, the silica sol is immersed in the C/SiC blank, and the surface of the silica sol is 20mm above the highest point of the C/SiC blank.
10. C/SiC-SiO2Composite material, characterized in that it is a C/SiC-SiO according to any one of claims 1 to 92The composite material is prepared by taking carbon fiber as a reinforcement and SiC and SiO2As a substrate, pyrolytic carbon is used as an interface layer between the reinforcement and the substrate;
SiC is coated on the surface of the carbon fiber, and SiC and SiO are arranged in the fiber bundle2Mass ratio of > SiC and SiO between fiber bundles2The mass ratio of (A) to (B);
in the matrix, SiC and SiO2Is greater than 1/2.
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