CN116143536A - Preparation method of micro-nano multi-scale ceramic matrix modified C/C composite material - Google Patents
Preparation method of micro-nano multi-scale ceramic matrix modified C/C composite material Download PDFInfo
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Abstract
The preparation method of the micro-nano multi-scale ceramic matrix modified C/C composite material comprises the steps of alternately superposing and layering micron-sized ceramic powder and carbon fibers, uniformly dispersing the ceramic powder in each layer of net tire in the layering process, connecting the net tire layer containing the ceramic powder and fiber cloth into a whole by needling or puncturing, and introducing the carbon fibers in the thickness direction to prepare a micron-sized ceramic powder modified carbon fiber preform; after densification by a ceramic matrix, performing pressure sintering densification, and finally supplementing densification treatment to the ceramic matrix until the density of the material reaches 2.2g/cm 3 The above. Thereby forming a micro-nano multi-scale ceramic matrix, which is beneficial to improving the compactness of the matrix and the obtained material has the following characteristics ofHigh temperature ablation resistance and anti-scour properties.
Description
Technical Field
The invention relates to a preparation method of a micro-nano multi-scale ceramic matrix modified C/C composite material, which is mainly used in the field of aerospace lightweight thermal structure protection, wherein the application field of the micro-nano multi-scale ceramic matrix modified C/C composite material comprises components such as a high-temperature oxidation-resistant ablation-resistant gas rudder, a nose cone, a spray pipe and the like, and the micro-nano multi-scale ceramic matrix modified C/C composite material prepared by the method has potential application prospects in the fields of metallurgy, chemical industry and the like.
Background
The C/C composite material has a series of excellent high-temperature properties, such as high-temperature strength retention rate, thermal shock resistance, ablation resistance and the like, but the C/C composite material which is not protected is extremely easy to generate oxidation failure, so that a ceramic phase is generally introduced into the C/C composite material by adopting a matrix modification technology to improve the high-temperature oxidation resistance and ablation resistance of the material, and the principle is that a molten oxide protection layer can be formed on the surface of the material in the oxidation ablation process of the introduced ceramic phase, thereby playing the role of oxygen and heat resistance similar to a thermal barrier coating. The precursor soaking-cracking process is one of the common methods for preparing carbon/ceramic composite material, and the precursor is mainly solution or molten as the impregnant to realize the densification of the material through repeated soaking and high temperature cracking, so that the process can meet the requirement of mass production of large-size special-shaped sample pieces.
Although the precursor dipping-cracking process has the great advantage of easy engineering application and popularization, a certain amount of gas is often generated in the process of forming a ceramic phase by cracking an organic precursor at high temperature, and the ceramic yield of the precursor is lower (less than or equal to 65 percent), so that the formed nano ceramic grains have more defects such as pores, and the like, thereby influencing the further improvement of the material density. On one hand, because the nano ceramic crystal grains formed by cracking are not sintered and densified, the hardness and the compactness of the ceramic matrix are lower, and under the scouring action of high-temperature fuel gas, the unsintered nano ceramic crystal grains are extremely easy to be scoured and eroded to form ablation defects; on the other hand, since the ceramic matrix is formed by stacking a large number of unsintered nanocrystals, a large number of defects such as voids in the matrix directly become diffusion and invasion channels of oxygen at high temperature, and further oxidation and ablation of materials are promoted. Therefore, how to further improve the compactness and density of the carbon/ceramic composite material prepared by precursor dipping-cracking has become the basis for improving the high-temperature ablation resistance of the carbon/ceramic composite material. In addition, in the process of repeated impregnation and cracking, particularly in the thickness direction, precursors tend to be enriched in the surface layer area during impregnation, so that the phenomenon of hole sealing and crusting of the material after repeated densification is caused, and the subsequent densification process is influenced.
Aiming at the problems, in order to solve the problem that the pores in the matrix of the ceramic modified C/C composite material prepared by a precursor dipping-cracking process are higher, the compactness and the density of the material are further improved, the patent discloses a preparation method of the micro-nano multi-scale ceramic matrix modified C/C composite material, the composite material mainly comprises a carbon fiber reinforcement body and a micro-nano multi-scale ceramic matrix phase, wherein the micro-ceramic powder is introduced by adopting a powder carbon fiber mixed knitting mode, and nano ceramic grains are generated by cracking a ceramic precursor. The technology utilizes the characteristic that micro-nano multi-scale ceramic phase is easy to sinter, and introduces high-temperature pressure sintering in the middle and later stages of densification of the composite material so as to realize sintering densification of micro-nano ceramic grains in a matrix, thereby reducing closed pore defects in the matrix, opening pore channels in the material and providing pore channels for subsequent impregnation and pyrolysis. The technology effectively improves the density of the carbon/ceramic composite material by constructing the micro-nano ceramic matrix and adopting a hot-pressing sintering mode, thereby improving the gas scouring resistance and the ablation resistance of the material and providing a new way for preparing the ablation-resistant carbon/ceramic composite material with compact structure.
Disclosure of Invention
The invention aims to provide a preparation method of a micro-nano multi-scale ceramic matrix modified C/C composite material, which is characterized in that micro-nano multi-scale matrix ceramic grains are constructed by combining ceramic powder mixed weaving and precursor dipping and cracking processes, and densification of a ceramic matrix is realized by high-temperature hot pressing in the later stage by utilizing the characteristic that the micro-nano ceramic grains are easy to sinter, so that the defect of closed pores in the ceramic matrix is reduced, and a large number of through holes are formed in the material due to shrinkage of the ceramic grains after sintering, so that pore channels are provided for the later-stage supplementary densification. In addition, the sintering densification of the micro-nano ceramic phase can obviously improve the compactness of the matrix, and meanwhile, the through holes generated by sintering provide impregnation channels for subsequent supplementary densification, so that the density and the anti-scouring performance of the prepared material are effectively improved.
The invention provides a preparation method of a micro-nano multi-scale ceramic matrix modified C/C composite material, which is characterized in that the composite material mainly comprises a micro-nano multi-scale ceramic phase matrix and a carbon fiber reinforcement;
the preparation method of the micro-nano multi-scale ceramic matrix modified C/C composite material comprises the following steps:
(1) Preparing a micron-sized ceramic powder modified carbon fiber preform: the method comprises the steps of taking micron-sized ceramic powder and carbon fiber as raw materials, alternately superposing and layering fiber net tyres and carbon fiber cloth in sequence, uniformly dispersing the ceramic powder in each layer of net tyre in the layering process, then connecting the net tyre layers containing the ceramic powder and the fiber cloth into a whole by adopting a needling or puncturing technology, and introducing the carbon fiber in the thickness direction to obtain the micron-sized ceramic powder modified carbon fiber preform.
(2) Densification of ceramic substrates: the method is characterized in that an organic ceramic precursor is used as a raw material, and a precursor dipping-cracking process is adopted to densify the prepared ceramic powder modified carbon fiber preform. After multiple times of dipping-cracking densification, the carbon fiber reinforced micro-nano multi-scale ceramic composite material framework is prepared.
(3) And (3) pressure sintering densification: and (3) carrying out high-temperature hot pressing or Spark Plasma Sintering (SPS) on the prepared carbon fiber reinforced micro-nano multi-scale ceramic composite material skeleton to promote sintering densification of ceramic micro-nano grains in a matrix, and preparing a sintered carbon/ceramic composite material blank after high-temperature hot pressing sintering.
(4) And (3) supplementing densification treatment of the ceramic matrix: the prepared sintered/ceramic composite material blank is subjected to machining and perforating treatment, and then is subjected to supplementary densification treatment by adopting a precursor dipping-cracking process until the density of the material reaches 2.2g/cm 3 The above.
(1) The micron-sized ceramic powder is SiC, zrC, hfC, taC, zrB 2 、HfB 2 One of them.
(1) The micron-sized ceramic powder has a powder particle size ranging from 1 to 50 mu m. .
(1) The density of the micron-sized ceramic powder modified carbon fiber preform ranges from 0.8 g/cm to 1.35g/cm 3 。
(2) The organic ceramic precursor is one of polycarbosilane, alkoxy zirconium and alkoxy hafnium.
(2) The precursor dipping-cracking process comprises the following steps: and (3) dissolving the organic ceramic precursor in dimethylbenzene to form a liquid impregnant, and repeatedly carrying out impregnation-cracking densification treatment on the carbon fiber preform prepared in the step (1). The nano-scale ceramic grains are formed in the carbon fiber preform through repeated dipping, drying and pyrolysis treatment. In the cracking process, argon is introduced for protection, the high-temperature cracking temperature is 900-1600 ℃, and the cracking heat preservation time is 0.5-2 h. The above dip-cracking process is repeated until the material reaches a predetermined density.
(2) The carbon fiber reinforced micro-nano multi-scale ceramic composite material framework has the density range of 1.6-1.85 g/cm 3 。
(3) The high-temperature hot-pressing process is as follows: placing the carbon fiber reinforced micro-nano multi-scale ceramic composite material framework in the step (2) in a high-temperature hot-pressing furnace, heating to 1600-2000 ℃ for pressurized sintering, wherein the pressure is 10-30 MPa, and the pressure maintaining time is 30min.
(3) The SPS process is as follows: and (3) placing the carbon fiber reinforced micro-nano multi-scale ceramic composite material framework in the step (2) in a discharge plasma sintering furnace, heating to 1600-2000 ℃ for SPS sintering, wherein the pressure is 10-40 MPa, and the pressure maintaining time is 5-15 min.
(4) The precursor dipping-cracking process is similar to that in the step (2), in the densification process, when the crusting and hole sealing phenomena occur on the surface of the material, the surface machining and hole opening treatment are needed to be carried out on the material, and then the dipping-cracking densification process is repeated until the material reaches 2.2g/cm 3 The above.
The invention has the following advantages:
(1) In order to solve the problem of high pore space in the matrix of the ceramic modified C/C composite material prepared by a precursor dipping-cracking process, the compactness and density of the material are further improved.
(2) And on the basis of preparing a carbon fiber reinforced micro-nano multi-scale ceramic matrix skeleton, sintering and densifying micro-nano ceramic particles by adopting a high-temperature low-pressure sintering process by utilizing the characteristic that micro-nano ceramic grains are easy to sinter, so as to reduce the closed pore defect in the matrix. Meanwhile, due to sintering shrinkage of the micro-nano ceramic grains, a large number of through holes are formed in the material, so that a pore channel is provided for later-stage supplementary densification.
(3) The carbon fiber reinforced micro-nano multi-scale ceramic matrix skeleton has good pore opening effect by high-temperature low-pressure sintering densification, and the through holes generated by sintering provide impregnation channels for subsequent supplementary densification, so that the density of the material and the compactness of the ceramic matrix are effectively improved, and the high-temperature ablation resistance and the anti-scouring performance of the material are enhanced.
Drawings
FIG. 1 is a hot press sintering density of 1.8g/cm prepared in example 1 3 A C/C-SiC skeleton;
FIG. 2 shows the density of 2.30g/cm prepared in example 1 3 A surface topography of the C/C-SiC composite material; wherein, fig. 2a is a morphology diagram after hot press sintering and subsequent dip-cracking densification treatment; FIG. 2b is an enlarged view of the profile of FIG. 2 a;
FIG. 3 is a density of 2.30g/cm prepared in example 1 3 A cross-sectional morphology of the C/C-SiC composite material; wherein FIG. 3a is a cross-sectional morphology of the sintered nano-micron ceramic particles in the hot pressed sintered material; FIG. 3b is an enlarged partial cross-sectional profile view of the fiber bundle of FIG. 3 a;
FIG. 4 is a density of 2.30g/cm prepared in example 1 3 The C/C-SiC composite material is subjected to plasma ablation for 60 seconds; wherein FIG. 4a is a photograph of the real object before ablation and FIG. 4b is a photograph of the real object after ablation;
FIG. 5 shows a real objectThe density prepared in example 1 was 2.30g/cm 3 A microscopic morphology graph and an energy spectrum analysis result of the C/C-SiC composite material after plasma ablation; wherein FIG. 5a is a topography of the ablation center; FIG. 5b is an enlarged view of a portion of FIG. 5 a;
FIG. 6 is a surface microtopography of the C/C-SiC composite material prepared in example 2.
Detailed Description
Example 1: the method comprises the steps of taking a carbon fiber net tire, satin cloth and micron SiC ceramic powder as raw materials (average grain diameter is about 25 microns), adopting a SiC ceramic powder and carbon fiber mixed knitting technology, firstly spreading the carbon fiber net tire on the surface of the satin cloth, then uniformly spreading the SiC micron powder at the positions of pores of the carbon fiber net tire, then alternately laminating and paving a prefabricated body according to the sequence of the satin cloth/carbon fiber net tire, the SiC ceramic powder/the satin cloth/the carbon fiber net tire and the SiC ceramic powder, and finally performing puncture connection on a net tire layer containing the SiC powder and the satin cloth layer in a puncture manner to prepare the carbon fiber reinforced composite fabric with the density of 0.11g/cm 3 Is a SiC powder modified carbon fiber preform. Polycarbosilane is used as a ceramic precursor, the polycarbosilane is dissolved in dimethylbenzene to form liquid impregnating solution, and a precursor impregnating-cracking process is adopted to densify the SiC powder modified carbon fiber preform to 1.8g/cm 3 . In the cracking process, flowing argon is introduced for protection, the cracking temperature of the SiC ceramic precursor is 1200 ℃, and the cracking heat preservation time is 1-2h. And (3) carrying out high-temperature hot-pressing sintering on the prepared C/C-SiC skeleton, wherein the sintering temperature is 1800 ℃, the pressure is 20MPa, the dwell time is 30min, and then naturally cooling to room temperature. The prepared sintered C/C-SiC skeleton is subjected to machining and perforating treatment, polycarbosilane is used as a raw material, repeated dipping-cracking densification treatment is carried out, and the density of the finally prepared C/C-SiC composite material is up to 2.30g/cm 3 。
FIG. 1 is a hot press sintering density of 1.8g/cm prepared in example 1 3 The microscopic morphology graph of the C/C-SiC skeleton of the fiber web is characterized in that a large amount of SiC ceramic phases are filled in the fiber web after the primary impregnation-cracking densification, and the SiC nano ceramic particles formed by cracking and the SiC micron powder form a massive ceramic phase, but obvious holes exist between the ceramic particles and the fibers because the high-temperature sintering is not carried outA gap.
FIG. 2 shows the density of 2.30g/cm prepared in example 1 3 The surface topography of the C/C-SiC composite material. As can be seen from fig. 2a, after hot pressed sintering and subsequent impregnation-cracking densification, the surface of the material is almost completely covered by the ceramic layer, no obvious pores are present, and the amount of exposed carbon fibers is small. Further enlarged analysis shows that (figure 2 b) the ceramic layer on the surface has microcrack defects, but the whole structure is compact, and further proves that the density and compactness of the material can be effectively improved after hot pressed sintering and subsequent impregnation-cracking densification. Because the surface of the material is covered by the SiC ceramic layer, almost no carbon fiber is exposed, the inside of the material can be protected from being corroded by oxidizing atmosphere to a certain extent, and the oxidation resistance and ablation resistance of the material are improved.
FIG. 3 is a density of 2.30g/cm prepared in example 1 3 Cross-sectional morphology of the C/C-SiC composite material. As can be seen from fig. 3a, after hot-pressed sintering, the nano-micron ceramic particles in the material form a massive ceramic phase with compact structure after sintering, and a distinct ceramic block can be seen inside the fiber bundle. It can be seen that the partial enlargement of the fiber bundle (fig. 3 b), the introduction of the ceramic phase brings about a tight fiber-to-fiber bond. The structure can improve the oxidation resistance and ablation resistance of the material to a certain extent.
FIG. 4 is a density of 2.30g/cm prepared in example 1 3 Is a physical photograph of the C/C-SiC composite material before and after 60 seconds of plasma ablation. It can be seen that the sample is dark gray before ablation (fig. 4 a), and the surface is attached with a more obvious ceramic phase, so that the amount of bare carbon fibers is less; after 60s plasma flame ablation, although obvious oxidation marks and white oxidation products appear in the ablation center of the surface, obvious ablation pits and cracks are not formed. After ablation, the mass ablation rate of the sample was-0.047 mg/s. The SiC ceramic powder modified carbon fiber preform with the same density is adopted without pressurized sintering, and after the SiC precursor is immersed and cracked, the density of the prepared C/C-SiC composite material is only 2.10g/cm 3 After the sample is subjected to plasma flame ablation for 60 seconds under the same conditions, the mass ablation rate of the sample is 0.123mg/s. The above results furtherThe step proves that the high-temperature hot-pressing sintering is carried out in the dipping-cracking process, and the nano-micron ceramic particles can form a ceramic matrix with compact structure after sintering and subsequent dipping-cracking densification, so that the density and the high-temperature ablation resistance of the C/C-SiC composite material are effectively improved.
FIG. 5 is a density of 2.30g/cm for the preparation of example 1 3 The microstructure graph and the energy spectrum analysis result of the C/C-SiC composite material after plasma ablation. FIG. 5a is a topography of the ablation center, and it can be seen that no significant ablation pits are formed in the ablation center area after the plasma for 60s ablation, and no carbon fibers are exposed. Although microcracks and hole marks formed by active oxidation of SiC appear in the ablation center, the ablation center is covered with a more obvious silicon oxide fusion protection layer. Further analysis of the melt phase of the ablation center revealed (fig. 5 b) that the surface spheres were built up from numerous molten globules, and that these globules were built up and fused to form a more continuous melt protective layer, which was shown by the spectral analysis to contain mainly Si and O elements, indicating that the ablation center surface consisted of a molten and not completely melted SiO2 phase. In the ablation process, the SiC ceramic layer with compact surface layer and the formed SiO2 fusion protective layer can play a better role in resisting oxygen, so that the high-temperature ablation resistance of the C/C-SiC composite material is effectively improved.
Example 2: taking a carbon fiber net tyre, a weft-free cloth and micron SiC ceramic powder as raw materials (the average grain diameter is about 25 microns), adopting a mixed knitting technology of the SiC ceramic powder and the carbon fiber, firstly spreading the carbon fiber net tyre on the surface of the weft-free cloth, then uniformly spreading the SiC micron powder at the pores of the carbon fiber net tyre, then alternately laminating and paving the prefabricated body according to the sequence of 0-degree non-woven cloth/carbon fiber net tire, siC ceramic powder, 90-degree non-woven cloth/carbon fiber net tire, siC ceramic powder, 0-degree non-woven cloth/carbon fiber net tire and SiC ceramic powder, and finally performing needling connection on the net tire layer containing the SiC powder and the non-woven cloth layer in a needling manner to prepare the fiber reinforced plastic fabric with the density of 0.86g/cm 3 Is a SiC powder modified carbon fiber preform. Polycarbosilane is used as a ceramic precursor, the polycarbosilane is dissolved in dimethylbenzene to form liquid impregnating solution, and a precursor impregnating-cracking process is adopted to densify the SiC powder modified carbon fiber preform to 1.6g/cm 3 . Cracking ofIn the decomposition process, flowing argon is introduced for protection, the cracking temperature of the SiC ceramic precursor is 1200 ℃, and the cracking heat preservation time is 1-2h. And (3) performing spark plasma sintering on the prepared C/C-SiC skeleton, wherein the sintering temperature is 1800 ℃, the pressure is 30MPa, the pressure maintaining time is 10min, and then cooling to room temperature. The prepared sintered C/C-SiC skeleton is subjected to machining and perforating treatment, polycarbosilane is taken as a raw material, repeated dipping-cracking densification treatment is carried out, and the density of the finally prepared C/C-SiC composite material is 2.22g/cm 3 。
FIG. 6 is a surface microtopography of the C/C-SiC composite material prepared in example 2. It can be seen that after hot pressing and subsequent impregnation-cracking densification processes, the surface of the sample is almost completely covered by the ceramic layer, no obvious pores or obvious exposed carbon fibers are formed, and the structure can protect the interior of the material from being corroded by high-temperature oxygen atmosphere to a certain extent, thereby being beneficial to improving the high-temperature oxidation resistance and ablation resistance of the material.
Example 3: taking a carbon fiber net tire, a weft-free cloth and micron HfC ceramic powder as raw materials (about 10 microns in average particle diameter), adopting a mixed weaving technology of the HfC ceramic powder and carbon fiber, firstly spreading the carbon fiber net tire on the surface of the weft-free cloth, then uniformly spreading the HfC micron powder at the positions of pores of the carbon fiber net tire, then alternately laminating and paving a prefabricated body according to the sequence of 0-degree weft-free cloth/carbon fiber net tire, plus HfC ceramic powder, and finally performing needle punching connection on a net tire layer containing the HfC powder and the weft-free cloth layer in a needle punching mode to prepare the fiber reinforced fabric with the density of 0.93g/cm 3 Is a HfC powder modified carbon fiber preform. Polycarbosilane is used as a ceramic precursor, the polycarbosilane is dissolved in dimethylbenzene to form liquid impregnating solution, and the precursor impregnating-cracking process is adopted to densify the HfC powder modified carbon fiber preform to 1.78g/cm 3 . In the cracking process, flowing argon is introduced for protection, the cracking temperature of the SiC ceramic precursor is 1200 ℃, and the cracking heat preservation time is 1-2h. And (3) performing spark plasma sintering on the prepared C/C-SiC skeleton, wherein the sintering temperature is 1800 ℃, the pressure is 30MPa, the pressure maintaining time is 10min, and then cooling to room temperature. The prepared sintered C/C-HfC-SiC skeleton is subjected to machining and perforating treatmentAnd then, taking polycarbosilane and zirconium alkoxide as raw materials, dissolving the polycarbosilane and the zirconium alkoxide in dimethylbenzene according to a mass ratio of 1:2 to form impregnating solution, repeatedly impregnating, cracking and densifying the sintered C/C-HfC-SiC skeleton, and introducing flowing argon for protection in the cracking process, wherein the cracking temperature of the ceramic precursor is 1450-1600 ℃, and the cracking and heat preservation time is 1-2h. Repeating the above soaking-cracking process until the density of the material reaches 2.32g/cm 3 。
Claims (10)
1. The preparation method of the micro-nano multi-scale ceramic matrix modified C/C composite material is characterized in that the composite material consists of a micro-nano multi-scale ceramic phase matrix and a carbon fiber reinforcement; the preparation method comprises the following steps:
(1) Preparing a micron-sized ceramic powder modified carbon fiber preform: taking micron-sized ceramic powder and carbon fiber as raw materials, alternately superposing and layering fiber net tyres and carbon fiber cloth in sequence, uniformly dispersing the ceramic powder in each layer of net tyres in the layering process, then connecting the net tyre layers containing the ceramic powder and the fiber cloth into a whole by adopting a needling or puncturing method, and introducing the carbon fiber in the thickness direction to prepare a micron-sized ceramic powder modified carbon fiber preform;
(2) Densification of ceramic substrates: the preparation method comprises the steps of taking an organic ceramic precursor as a raw material, adopting a precursor dipping-cracking process to densify the prepared ceramic powder modified carbon fiber preform, and preparing a carbon fiber reinforced micro-nano multi-scale ceramic composite material framework after multiple dipping-cracking densification;
(3) And (3) pressure sintering densification: carrying out high-temperature hot-pressing or spark plasma sintering on the prepared carbon fiber reinforced micro-nano multi-scale ceramic composite material skeleton to promote sintering densification of ceramic micro-nano grains in a matrix, and preparing a sintered carbon/ceramic composite material blank after high-temperature hot-pressing sintering; the high-temperature hot-pressed sintering temperature is 1600-2000 ℃;
(4) And (3) supplementing densification treatment of the ceramic matrix: the prepared sintered/ceramic composite material blank is subjected to machining and perforating treatment, and is subjected to supplementary densification treatment by adopting a precursor dipping-cracking process until the density of the material reaches 2.2g/cm 3 The above.
2. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: the micron-sized ceramic powder in the step (1) is SiC, zrC, hfC, taC, zrB 2 Or HfB 2 。
3. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: the micron-sized ceramic powder in the step (1) has a powder particle size ranging from 1 to 50 μm.
4. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: the density of the micron-sized ceramic powder modified carbon fiber preform in the step (1) ranges from 0.8 g/cm to 1.35g/cm 3 。
5. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: the organic ceramic precursor in the step (2) is polycarbosilane, zirconium alkoxide or hafnium alkoxide.
6. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: the precursor dipping-cracking process in the step (2) comprises the following steps: dissolving an organic ceramic precursor in dimethylbenzene to form a liquid impregnant, and repeatedly dipping, cracking and densifying the carbon fiber preform prepared in the step (1); forming nano-scale ceramic grains in the carbon fiber preform through repeated dipping, drying and pyrolysis treatment; in the cracking process, argon is introduced for protection, the high-temperature cracking temperature is 900-1600 ℃, the cracking heat preservation time is 0.5-2 h, and the soaking-cracking process is repeated until the material reaches the preset density.
7. A micro-nano multi-ruler according to claim 1The preparation method of the modified C/C composite material of the ceramic matrix is characterized by comprising the following steps: the carbon fiber reinforced micro-nano multi-scale ceramic composite material framework in the step (2) has the density range of 1.6-1.85 g/cm 3 。
8. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: the high-temperature hot pressing process in the step (3) is as follows: and (3) placing the carbon fiber reinforced micro-nano multi-scale ceramic composite material skeleton in the step (2) in a high-temperature hot-pressing furnace, heating to 1700-2000 ℃ for pressurized sintering, wherein the pressure is 10-30 MPa, and the pressure maintaining time is 30min.
9. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: the spark plasma sintering process in the step (3) is as follows: and (3) placing the carbon fiber reinforced micro-nano multi-scale ceramic composite material framework in the step (2) in a discharge plasma sintering furnace, heating to 1600-2000 ℃ for discharge plasma sintering, wherein the pressure is 10-40 MPa, and the pressure maintaining time is 5-15 min.
10. The method for preparing the micro-nano multi-scale ceramic matrix modified C/C composite material according to claim 1, which is characterized in that: in the precursor dipping-cracking process in the step (4), when the crusting and hole sealing phenomena occur on the surface of the material, carrying out surface machining and hole opening treatment on the material, and then repeating the dipping-cracking densification process until the material reaches 2.2g/cm 3 The above.
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