CN116178051A - Preparation method of rare earth oxide modified C/(C-) SiC-ZrC composite material - Google Patents
Preparation method of rare earth oxide modified C/(C-) SiC-ZrC composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 58
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 47
- 229920003257 polycarbosilane Polymers 0.000 claims abstract description 30
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 27
- 238000005336 cracking Methods 0.000 claims abstract description 26
- 238000005470 impregnation Methods 0.000 claims abstract description 24
- -1 rare earth nitrate Chemical class 0.000 claims abstract description 23
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 18
- 238000007598 dipping method Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 10
- 239000008096 xylene Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 230000004584 weight gain Effects 0.000 claims description 2
- 235000019786 weight gain Nutrition 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims description 2
- 238000002679 ablation Methods 0.000 abstract description 23
- 239000000463 material Substances 0.000 abstract description 10
- 239000011216 ultra-high temperature ceramic matrix composite Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 40
- 238000012876 topography Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- RCVUBQJWUGSTEZ-UHFFFAOYSA-N C(C)O.[N+](=O)([O-])[O-].[Yb+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] Chemical compound C(C)O.[N+](=O)([O-])[O-].[Yb+3].[N+](=O)([O-])[O-].[N+](=O)([O-])[O-] RCVUBQJWUGSTEZ-UHFFFAOYSA-N 0.000 description 1
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- 229910007735 Zr—Si Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000035876 healing Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention discloses a preparation method of a rare earth oxide modified C/(C-) SiC-ZrC composite material, belonging to the technical field of preparation of ultrahigh-temperature ceramic matrix composite materials. According to the invention, a polymer impregnation cracking (PIP) process is adopted, and the rare earth oxide modified C/(C-) SiC-ZrC composite material is prepared by alternately carrying out impregnation cracking on the polycarbozirconane, the polycarbosilane precursor solution and the rare earth nitrate solution, so that the influence of the introduction of the rare earth oxide on the mechanical properties is small, the ablation resistance of the C/(C-) SiC-ZrC composite material is remarkably improved, and the possibility is provided for the repeated use of the composite material.
Description
Technical field:
the invention relates to the technical field of preparation of ultrahigh-temperature ceramic matrix composite materials, in particular to a preparation method of a rare earth oxide modified C/(C-) SiC-ZrC composite material.
The background technology is as follows:
when a high-speed aircraft flies in the atmosphere and across the atmosphere, components such as nose cones, wing front edges and the like on the surface of the aircraft are subjected to ultra-high temperatures above 2000 ℃ due to the severe pneumatic heating effect, so that the materials are required to have good mechanical, oxidation and ablation resistance. The C/(C-) SiC-ZrC composite material has the characteristics of low density, high specific strength and specific modulus, ultrahigh temperature resistance, oxidization resistance, ablation resistance and the like, and is widely focused in the field of aerospace heat protection. However, zrO produced after ablation 2 The occurrence of phase transition causes cracking and peeling of the oxide film, and furthermore, siO 2 Decomposition and volatilization also occur at ultra-high temperaturesThereby obtaining porous ZrO 2 The oxide film is easy to peel off under high-speed gas flushing, and finally the long-time and repeatable use of the material is influenced. The patent CN 105967759 A,CN107673762A,CN 107056336 A,CN 110981546A and CN 113956050A study the preparation of rare earth oxide-containing coatings on the surface of C/C composite materials to form low-volatility composite oxides for pore and crack healing, and in addition, the addition of rare earth oxides reduces SiO 2 Is volatilized into ZrO 2 The effect of phase stabilization is achieved, but the effect of the coating is relatively limited, and once the coating fails, the composite material is difficult to continuously recycle. And patent CN 103864451A and literature "Lei Luo, junpeng Liu, liuyang Duan, YIGUang Wang.multiple ablation resistance of La 2 O 3 /Y 2 O 3 -doped C/SiC-ZrC composites[J]Ceramics International,41 (2015) 12878-12886' vacuum impregnating resin solution containing rare earth in C/C, C/SiC matrix, then introducing Zr-Si alloy by adopting a reaction infiltration method to prepare the C/SiC-ZrC composite material so as to achieve the aim of repeated use. However, the temperature of the method is high, the fiber is damaged, and in addition, the content and uniformity of the fiber are limited.
The invention comprises the following steps:
aiming at the defects existing in the prior art, the invention aims to provide a preparation method of a rare earth oxide modified C/(C-) SiC-ZrC composite material, which is used for preparing the C/(C-) SiC-ZrC composite material containing rare earth oxide by alternately impregnating polycarbozirconane, polycarbosilane precursor solution and rare earth nitrate solution by a PIP method so as to reduce SiO 2 Is volatilized to form a low-volatility composite oxide, and the ZrO is inhibited 2 The phase change has excellent anti-ablation performance, and finally meets the requirement of repeated use.
The technical scheme adopted by the invention is as follows:
the preparation method of the rare earth oxide modified C/(C-) SiC-ZrC composite material adopts a PIP process to prepare the rare earth oxide modified C/(C-) SiC-ZrC composite material, and specifically comprises the following steps: and alternately introducing polycarbozircon, polycarbosilane precursor solution and rare earth nitrate solution into the porous C/(C-) SiC composite material, and preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material after multiple curing-cracking.
The method comprises the following steps:
(1) Preparing a porous C/(C-) SiC composite material;
(2) Preparing a polycarbozirconane and polycarbosilane precursor solution: respectively dissolving polycarbozirconane and polycarbosilane in an organic solvent, and magnetically stirring for 2-10 hours to obtain a polycarbozirconane solution and a polycarbosilane solution, wherein the concentration ranges are 50% -70%; mixing a polycarbozirconane solution and a polycarbosilane solution according to a mass ratio of 4:1-20:1, and magnetically stirring for 1-5 h to obtain a polycarbozirconane and polycarbosilane precursor solution;
(3) Preparing rare earth nitrate solution: the mass concentration of the rare earth nitrate solution is 25% -50%;
(4) The polycarbozircon and polycarbosilane precursor solution and the rare earth nitrate solution are alternately introduced into the porous C/(C-) SiC composite material: firstly, dipping a polycarbozirconane and a polycarbosilane precursor solution, and then curing and high-temperature cracking, wherein the dipping-curing-cracking process is carried out for 1-3 times; dipping the rare earth nitrate solution for 1 time, and then curing and carrying out pyrolysis treatment;
(5) Repeating the process of the step (4) for a plurality of times until the weight gain rate of the composite material is less than 1% or reaches the specified density; the content of the rare earth oxide added into the composite material can also be adjusted by adjusting the alternate impregnation times, and the rare earth oxide can be uniformly distributed in the composite material.
In the step (1), the density of the porous C/(C-) SiC composite material is 0.6-1.8 g/cm 3 Between them.
In the step (2), the organic solvent is xylene, divinylbenzene, tetrahydrofuran, or the like.
In the step (3), the solvent used for preparing the rare earth nitrate solution is deionized water or ethanol, and the rare earth is one or more of Y, la, sc, gd, lu and Yb; the content of the rare earth oxide added into the composite material is adjusted by adjusting the concentration of the rare earth nitrate solution.
In the step (4), the impregnation process is vacuum impregnation and/or pressure impregnation; during vacuum impregnation, the impregnation time is 1-5 h, and the vacuum degree is less than or equal to 200Pa; when in pressure impregnation, the impregnation time is 0.5 to 3 hours, and the pressure is 0.5 to 5MPa.
In the curing process of the step (4): the curing temperature is 180-200 ℃, the heating speed is less than or equal to 2 ℃/min, and the heat preservation time is 3-5 h.
In the pyrolysis process of the step (4): the cracking temperature is 1400-1600 ℃, the heating speed is less than or equal to 1 ℃/min, the heat preservation time is 0.5-2 h, and the process is carried out under inert atmosphere.
The invention has the beneficial effects that:
the PIP method is used for alternatively impregnating the polycarbozirconane, the polycarbosilane precursor solution and the rare earth nitrate solution, so that the content and uniformity of rare earth oxide are effectively regulated, and the addition of the rare earth oxide effectively reduces SiO in the C/(C-) SiC-ZrC composite material 2 The volatilization of the generated rare earth silicate can reduce the diffusion of oxygen into the material, and ZrO 2 The phase change of the material is effectively inhibited, and the ablation resistance of the material is further improved.
Description of the drawings:
FIG. 1 is a flow chart of the preparation of a rare earth oxide modified C/(C-) SiC-ZrC composite material.
FIG. 2 is a cross-sectional micro-topography and EDS of example 1; wherein: (a) cross-sectional microtopography; (b) EDS.
FIG. 3 is the macroscopic topography after ablation for comparative example 1 and example 1; wherein: (a) comparative example 1; (b) example 1.
FIG. 4 is the macroscopic and microscopic morphology and phase composition after ablation of example 3; wherein: (a) is the macroscopic topography after ablation, (b) is the phase composition of the surface after ablation, (c) is the microscopic topography after ablation, and (d) is the EDS at position 1 in (c).
The specific embodiment is as follows:
in order that those skilled in the art will better understand the technical scheme of the present invention, the present invention will be described in further detail with reference to comparative examples and examples.
Comparative example 1
According to the process flow shown in FIG. 1, first, a density of 1.6g/cm is selected 3 Porous C of (2)(C-) SiC composite. Secondly, respectively dissolving polycarbozirconane and polycarbosilane in dimethylbenzene to prepare 50% solutions, and respectively magnetically stirring for 2 hours; the 50% polycarbozirconane xylene solution and the 50% polycarbosilane xylene solution are configured according to the mass ratio of 16:1, and are fully magnetically stirred for 2 hours. Finally, preparing the C/(C-) SiC-ZrC composite material by adopting a PIP process, wherein the vacuum degree during impregnation is 100Pa, and the vacuum impregnation is carried out for 2 hours; pressure impregnation is carried out for 2 hours under the pressure of 2MPa; curing at 180deg.C for 3h, cracking at 1500deg.C for 1h, repeating the above soaking-curing-cracking process for 13 times to obtain a density of 1.88g/cm 3 C/(C-) SiC-ZrC composite material, oxyacetylene is ablated for 1000s at 1700 ℃, 200s at a time, and the line ablation rate is 0.32 mu m/s. Fig. 3 (a) is a macro topography after ablation of a material.
Example 1
According to the process flow shown in FIG. 1, first, a density of 1.6g/cm is selected 3 Porous C/(C-) SiC composites. Secondly, respectively dissolving polycarbozirconane and polycarbosilane in dimethylbenzene to prepare 50% solutions, and respectively magnetically stirring for 2 hours; a50 wt% polycarbozirconane xylene solution and a 50wt% polycarbosilane xylene solution were configured at a mass ratio of 16:1 and sufficiently magnetically stirred for 2 hours. Rare earth yttrium nitrate is dissolved in deionized water to prepare 25wt% solution. Finally, dipping and cracking 1 time of polycarbozirconane and polycarbosilane precursor solution by adopting a PIP process, dipping and cracking 1 time of rare earth yttrium nitrate aqueous solution, and preparing the C/(C-) SiC-ZrC composite material in a reciprocating manner, wherein the vacuum degree during dipping is 100Pa, and the vacuum dipping is carried out for 2 hours; pressure impregnation is carried out for 2 hours under the pressure of 2MPa; curing at 180deg.C for 3h, cracking at 1500deg.C for 1h, repeating the above soaking-curing-cracking process for 13 times to obtain a density of 1.82g/cm 3 C/(C-) SiC-ZrC-Y 2 O 3 A composite material. As shown in FIG. 2, Y 2 O 3 Is uniformly distributed in the C/(C-) SiC-ZrC composite material. The oxyacetylene is ablated for 1000s at 1700 ℃, 200s is carried out once, the linear ablation rate is 0.23 mu m/s, and the linear ablation rate is reduced by 28 percent compared with the linear ablation rate of the comparative example. Fig. 3 (b) is a macro topography after ablation of the material.
Example 2
According to the process flow shown in FIG. 1, first, a density of 1.7g/cm is selected 3 Porous C/(C-) SiC composite materialAnd (5) material. Secondly, respectively dissolving polycarbozirconane and polycarbosilane in dimethylbenzene to prepare 60% solution, and respectively magnetically stirring for 5 hours; preparing 60wt% of polycarbozirconane xylene solution and 60wt% of polycarbosilane xylene solution according to a mass ratio of 20:1, and fully magnetically stirring for 4 hours; rare earth yttrium nitrate is dissolved in deionized water to prepare 50% solution. Finally, dipping and cracking 1 time of polycarbozirconane and polycarbosilane precursor solution by adopting a PIP process, dipping and cracking 1 time of rare earth yttrium nitrate aqueous solution, and preparing the C/(C-) SiC-ZrC composite material in a reciprocating manner, wherein the vacuum degree during dipping is 100Pa, and the vacuum dipping is carried out for 4 hours; pressure impregnation is carried out for 2 hours under the pressure of 3MPa; curing at 200deg.C for 5h, cracking at 1500deg.C for 1h, repeating the above soaking-curing-cracking process for 13 times to obtain a density of 1.90g/cm 3 C/(C-) SiC-ZrC-Y 2 O 3 A composite material. Oxyacetylene ablation at 2100 ℃ for 600s, 200s at a time, and the line ablation rate of 2.33 μm/s.
Example 3
According to the process flow shown in FIG. 1, first, a density of 1.7g/cm is selected 3 Porous C/(C-) SiC composites. Secondly, respectively dissolving polycarbozirconane and polycarbosilane in dimethylbenzene to prepare 60wt% solution, and respectively magnetically stirring for 5 hours; preparing 60% of polycarbozirconane xylene solution and 60% of polycarbosilane xylene solution according to a mass ratio of 20:1, and fully magnetically stirring for 4 hours; the rare earth ytterbium nitrate was dissolved in ethanol to prepare a 28wt% solution. Finally, dipping and cracking 1 time of polycarbozirconane and polycarbosilane precursor solution by adopting a PIP process, dipping and cracking 1 time of rare earth ytterbium nitrate ethanol solution, and preparing the C/(C-) SiC-ZrC composite material in a reciprocating manner, wherein the vacuum degree during dipping is 100Pa, and the vacuum dipping is carried out for 4 hours; pressure impregnation is carried out for 2 hours under the pressure of 3MPa; curing at 200deg.C for 5h, cracking at 1500deg.C for 1h, repeating the above soaking-curing-cracking process for 13 times to obtain a density of 1.89g/cm 3 C/(C-) SiC-ZrC-Yb 2 O 3 A composite material. The oxyacetylene is ablated for 600s at 1900 ℃ and 200s at a time, and the linear ablation rate is 0.37 mu m/s. As shown in FIG. 4, the phase composition after ablation, the microstructure and the EDS result indicate Yb 2 O 3 The addition of (C) serves to stabilize ZrO 2 In addition, effectively reduce SiO 2 Is not limited to the volatile of the solvent,and produce Yb 2 Si 2 O 7 The phase is favorable for the generation of a continuous oxide film, thereby obtaining excellent ablation resistance.
Claims (8)
1. A preparation method of a rare earth oxide modified C/(C-) SiC-ZrC composite material is characterized by comprising the following steps: the method adopts PIP technology to prepare rare earth oxide modified C/(C-) SiC-ZrC composite material, which comprises the following steps: and alternately introducing polycarbozircon, polycarbosilane precursor solution and rare earth nitrate solution into the porous C/(C-) SiC composite material, and preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material after multiple curing-cracking.
2. The method for preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) Preparing a porous C/(C-) SiC composite material;
(2) Preparing a polycarbozirconane and polycarbosilane precursor solution: respectively dissolving polycarbozirconane and polycarbosilane in an organic solvent, and magnetically stirring for 2-10 hours to obtain a polycarbozirconane solution and a polycarbosilane solution, wherein the concentration ranges are 50% -70%; mixing a polycarbozirconane solution and a polycarbosilane solution according to a mass ratio of 4:1-20:1, and magnetically stirring for 1-5 h to obtain a polycarbozirconane and polycarbosilane precursor solution;
(3) Preparing rare earth nitrate solution: the mass concentration of the rare earth nitrate solution is 25% -50%;
(4) The polycarbozircon and polycarbosilane precursor solution and the rare earth nitrate solution are alternately introduced into the porous C/(C-) SiC composite material: firstly, dipping a polycarbozirconane and a polycarbosilane precursor solution, and then curing and high-temperature cracking, wherein the dipping-curing-cracking process is carried out for 1-3 times; dipping the rare earth nitrate solution for 1 time, and then curing and carrying out pyrolysis treatment;
(5) Repeating the process of the step (4) for a plurality of times until the weight gain rate of the composite material is less than 1% or reaches the specified density; the content of the rare earth oxide added into the composite material can also be adjusted by adjusting the alternate impregnation times, and the rare earth oxide can be uniformly distributed in the composite material.
3. The method for preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material according to claim 1, wherein the method comprises the following steps: the density of the porous C/(C-) SiC composite material is 0.6-1.8 g/cm 3 Between them.
4. The method for preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material according to claim 2, wherein the method comprises the following steps: in the step (2), the organic solvent is xylene, divinylbenzene, tetrahydrofuran or the like.
5. The method for preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material according to claim 2, wherein the method comprises the following steps: in the step (3), the solvent used in preparing the rare earth nitrate solution is deionized water or ethanol, and the rare earth is one or more of Y, la, sc, gd, lu and Yb; the content of the rare earth oxide added into the composite material is adjusted by adjusting the concentration of the rare earth nitrate solution.
6. The method for preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material according to claim 2, wherein the method comprises the following steps: in the step (4), the impregnation process is vacuum impregnation and/or pressure impregnation; during vacuum impregnation, the impregnation time is 1-5 h, and the vacuum degree is less than or equal to 200Pa; when in pressure impregnation, the impregnation time is 0.5 to 3 hours, and the pressure is 0.5 to 5MPa.
7. The method for preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material according to claim 2, wherein the method comprises the following steps: in the curing process of the step (4): the curing temperature is 180-200 ℃, the heating speed is less than or equal to 2 ℃/min, and the heat preservation time is 3-5 h.
8. The method for preparing the rare earth oxide modified C/(C-) SiC-ZrC composite material according to claim 2, wherein the method comprises the following steps: in the high-temperature cracking process of the step (4): the cracking temperature is 1400-1600 ℃, the heating speed is less than or equal to 1 ℃/min, the heat preservation time is 0.5-2 h, and the process is carried out under inert atmosphere.
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