CN117567165A - Continuous fiber reinforced ceramic matrix composite material and preparation method thereof - Google Patents
Continuous fiber reinforced ceramic matrix composite material and preparation method thereof Download PDFInfo
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- CN117567165A CN117567165A CN202311543850.1A CN202311543850A CN117567165A CN 117567165 A CN117567165 A CN 117567165A CN 202311543850 A CN202311543850 A CN 202311543850A CN 117567165 A CN117567165 A CN 117567165A
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- fiber
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- 239000002131 composite material Substances 0.000 title claims abstract description 85
- 239000000835 fiber Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000011159 matrix material Substances 0.000 title claims abstract description 19
- 239000011226 reinforced ceramic Substances 0.000 title claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 67
- 239000000843 powder Substances 0.000 claims abstract description 56
- 238000002347 injection Methods 0.000 claims abstract description 47
- 239000007924 injection Substances 0.000 claims abstract description 47
- 239000000919 ceramic Substances 0.000 claims abstract description 46
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 230000008569 process Effects 0.000 claims abstract description 36
- 238000005470 impregnation Methods 0.000 claims abstract description 33
- 238000005336 cracking Methods 0.000 claims abstract description 32
- 238000001764 infiltration Methods 0.000 claims abstract description 28
- 230000008595 infiltration Effects 0.000 claims abstract description 28
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 24
- 238000000151 deposition Methods 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000011153 ceramic matrix composite Substances 0.000 claims abstract description 12
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims description 30
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 28
- 239000005011 phenolic resin Substances 0.000 claims description 27
- 229920001568 phenolic resin Polymers 0.000 claims description 27
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 25
- 239000004917 carbon fiber Substances 0.000 claims description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000011863 silicon-based powder Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 150000004767 nitrides Chemical class 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
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- 239000003822 epoxy resin Substances 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 238000009954 braiding Methods 0.000 claims description 3
- 239000002041 carbon nanotube Substances 0.000 claims description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
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- 239000007849 furan resin Substances 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000280 densification Methods 0.000 abstract description 8
- 239000000543 intermediate Substances 0.000 description 31
- 238000002679 ablation Methods 0.000 description 17
- 238000007598 dipping method Methods 0.000 description 16
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- 229910010271 silicon carbide Inorganic materials 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- 238000000626 liquid-phase infiltration Methods 0.000 description 11
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 11
- 238000003756 stirring Methods 0.000 description 10
- 238000000498 ball milling Methods 0.000 description 9
- 238000009826 distribution Methods 0.000 description 8
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- 230000000052 comparative effect Effects 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
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- 238000005452 bending Methods 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
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- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 3
- 239000011216 ultra-high temperature ceramic matrix composite Substances 0.000 description 3
- 238000009827 uniform distribution Methods 0.000 description 3
- 229910026551 ZrC Inorganic materials 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
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- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
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- XINQFOMFQFGGCQ-UHFFFAOYSA-L (2-dodecoxy-2-oxoethyl)-[6-[(2-dodecoxy-2-oxoethyl)-dimethylazaniumyl]hexyl]-dimethylazanium;dichloride Chemical compound [Cl-].[Cl-].CCCCCCCCCCCCOC(=O)C[N+](C)(C)CCCCCC[N+](C)(C)CC(=O)OCCCCCCCCCCCC XINQFOMFQFGGCQ-UHFFFAOYSA-L 0.000 description 1
- WEAMLHXSIBDPGN-UHFFFAOYSA-N (4-hydroxy-3-methylphenyl) thiocyanate Chemical compound CC1=CC(SC#N)=CC=C1O WEAMLHXSIBDPGN-UHFFFAOYSA-N 0.000 description 1
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910001029 Hf alloy Inorganic materials 0.000 description 1
- 229910039444 MoC Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910000946 Y alloy Inorganic materials 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- LRTTZMZPZHBOPO-UHFFFAOYSA-N [B].[B].[Hf] Chemical compound [B].[B].[Hf] LRTTZMZPZHBOPO-UHFFFAOYSA-N 0.000 description 1
- CEPICIBPGDWCRU-UHFFFAOYSA-N [Si].[Hf] Chemical compound [Si].[Hf] CEPICIBPGDWCRU-UHFFFAOYSA-N 0.000 description 1
- TWRSDLOICOIGRH-UHFFFAOYSA-N [Si].[Si].[Hf] Chemical compound [Si].[Si].[Hf] TWRSDLOICOIGRH-UHFFFAOYSA-N 0.000 description 1
- NVZBIFPUMFLZLM-UHFFFAOYSA-N [Si].[Y] Chemical compound [Si].[Y] NVZBIFPUMFLZLM-UHFFFAOYSA-N 0.000 description 1
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 239000008367 deionised water Substances 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- WHJFNYXPKGDKBB-UHFFFAOYSA-N hafnium;methane Chemical compound C.[Hf] WHJFNYXPKGDKBB-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- UNASZPQZIFZUSI-UHFFFAOYSA-N methylidyneniobium Chemical compound [Nb]#C UNASZPQZIFZUSI-UHFFFAOYSA-N 0.000 description 1
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
- 229910021344 molybdenum silicide Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
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- 229910003468 tantalcarbide Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 1
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 230000004584 weight gain Effects 0.000 description 1
- 235000019786 weight gain Nutrition 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 description 1
- 229910021355 zirconium silicide Inorganic materials 0.000 description 1
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- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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Abstract
The invention belongs to the technical field of composite material preparation, and in particular relates to a continuous fiber reinforced ceramic matrix composite material and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a carbon source solution and ceramic powder to prepare slurry; depositing an interface inside the fiber preform; introducing the slurry into the central area of the fiber preform by adopting an injection method, and then curing and cracking to prepare an intermediate I; introducing the slurry into the edge area in the first intermediate by adopting a vacuum impregnation and pressure impregnation method, and then curing and cracking to obtain a second intermediate; and embedding the second intermediate by adopting powder, and then densifying by adopting an RMI infiltration process to obtain the densified ceramic matrix composite. The porous composite material intermediate with lower open porosity is prepared in a short time, and the composite material with higher densification degree can be prepared by carrying out RMI infiltration treatment on the composite material intermediate.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a continuous fiber reinforced ceramic matrix composite material and a preparation method thereof.
Background
The ceramic material mainly comprises SiC and ZrB 2 、HfB 2 Some transition metal compounds such as boride, carbide, silicide and nitride of ZrC, hfC, taN and HfN are a class of ablation resistant materials with great potential. However, the inherent brittleness and low damage tolerance of ceramics greatly limit their application, and composite materials are prepared by introducing a tough phase to improve their mechanical properties. The ultra-high temperature ceramic matrix composite is the most promising candidate material for extreme heat structural components such as nose cones, wing front edges and the like of hypersonic aircrafts by virtue of the excellent anti-ablation, high specific strength, high specific modulus and the like. The combination of the fiber reinforcement, the interface and the ultra-high temperature ceramic matrix imparts superior properties not possessed by a single component of the composite material. However, the existing composite material preparation process, such as a precursor impregnation cracking process and a chemical vapor infiltration process, has long production period and high production cost; the fiber quality is reduced in the reaction infiltration process, and the mechanical property of the material is greatly reduced; the slurry dipping process has high requirement on the granularity of powder and high porosity of the material. Therefore, a novel preparation method of the ceramic matrix composite needs to be developed, and the preparation process and cost of the ceramic matrix composite are greatly reduced so as to make up for the defects of the prior art.
Document 1"Effect of heat flux on ablation behavior and mechanism of C/C-ZrB 2 SiC composite under oxyacetylene torch flame "shows that depositing pyrolytic carbon by Thermal Chemical Vapor Infiltration (TCVI) process requires 20-50 hours, PIP process introduces ZrB 2 And SiC need to be cycled 14 times, however ZrB is introduced 2 The powder content was 17.7wt.%. The composite material prepared by the PIP process has uniformly distributed components, but the high cost of the precursor and the long manufacturing period are main disadvantages of the process.Document 2"Ablation behavior of C f the/ZrC-SiC-based composites fabricated by an improved reactive melt infiltration' indicates that: the samples prepared by the RMI infiltration process have the characteristics of high densification degree, less pores and the like, but the fiber structure can be damaged to a certain extent in the high-temperature reaction infiltration process, and the material performance is reduced. Therefore, the existing preparation method of the ceramic matrix composite material cannot have the advantages of short period, uniform component distribution and complete fiber structure.
Disclosure of Invention
In order to solve the technical problems, the invention provides a continuous fiber reinforced ceramic matrix composite material and a preparation method thereof, wherein after an interface layer is deposited on a fiber preform, ceramic powder is introduced into the central area of the fiber preform by adopting an injection process; then, the slurry is impregnated to introduce ceramic powder into the edge area of the fiber preform, so that the ceramic matrix is uniformly distributed in the preform; and finally, densification is carried out by adopting an RMI infiltration process. The invention has the advantages of short period, uniform component distribution and complete fiber structure. The invention protects the structural integrity of the fiber in the preparation process, improves the uniform distribution of the internal components of the material, can greatly shorten the preparation period of the composite material and meets the industry requirement.
The invention is realized by the following technical scheme.
The invention provides a preparation method of a continuous fiber reinforced ceramic matrix composite material, which comprises the following steps:
s1: mixing a carbon source solution and ceramic powder to prepare slurry;
depositing an interface inside the fiber preform;
s2: introducing the slurry prepared in the step S1 into the central area of the fiber preform processed in the step S1 by adopting an injection method, and then curing and cracking to prepare an intermediate I;
s3: introducing the ceramic slurry prepared in the step S1 into the edge area of the first intermediate prepared in the step S2 by adopting a vacuum impregnation and pressure impregnation method, and then performing curing and cracking to obtain a second intermediate;
s4: and embedding the second intermediate by adopting powder, and then densifying by adopting an RMI infiltration process to obtain the densified ceramic matrix composite.
Further, in S1, the carbon source is one or a combination of several of phenolic resin (PF) powder, carboxymethyl cellulose (CMC), epoxy resin (EP), furan resin (FF) and sucrose; such carbon sources need to be converted to carbon by pyrolysis;
the solvent is one or the combination of any one or more of deionized water, absolute ethyl alcohol, toluene and xylene;
the carbon source content in the carbon source solution is 30-70 wt.%.
Further, the carbon source also comprises one or a combination of any of carbon powder, diamond, graphene and carbon nano-tube, and the carbon source does not need the high-temperature treatment of the carbon source.
Further, in S1, the ceramic powder includes boride, carbide, or nitride;
the boride comprises zirconium boride, hafnium boride and titanium boride; the carbide comprises silicon carbide, zirconium carbide, hafnium carbide, niobium carbide, tantalum carbide, titanium carbide and molybdenum carbide; the nitride comprises boron nitride, hafnium nitride, zirconium nitride and silicon nitride; the silicide includes hafnium silicide, zirconium silicide, molybdenum silicide, and yttrium silicide.
The content of the ceramic powder in the slurry is 5-90 wt%;
the grain diameter of the ceramic powder is 0.05-50 mu m.
Further, in S1, the fiber preform includes carbon fibers, siC fibers, silicon nitride fibers, glass fibers, oxide fibers, and other ceramic fibers;
the forming mode of the fiber preform comprises two-dimensional lamination, three-dimensional needling fiber and three-dimensional braiding;
the fiber content of the fiber preform is 10 to 75vol.%.
Further, in S1, the interface materials are PyC, BN, siC and Si 3 N 4 One or a combination of a plurality of the above;
the deposition thickness of the interface is 100-600 nm.
In the step S2, the slurry prepared in the step S1 is introduced into the central area of the fiber preform processed in the step S1 by adopting an injection method, the slurry is distributed in a lattice in the central area of the fiber preform, the injection lattice comprises circular distribution, rectangular distribution or irregular distribution, and the interval of the lattice is adjustable.
In S2, the curing and cracking processes are carried out in inert gas, wherein the curing temperature is 80-300 ℃, the heat preservation time is 0.5-4 h, the cracking temperature is 600-1200 ℃, the heat preservation time is 0.5-4 h, and the heating rate is 1-10 ℃/min.
Further, in S2, the injection interval between X, Y and Z direction is 2-10 mm, the inner diameter of the needle is 0.2-1 mm, the injection time of the lattice point is 0.5-2.0S, and the injection pressure is 0.5-1.5 MPa.
It should be noted that if the diameter of the needle exceeds 1mm, obvious holes are left on the surface of the prepared composite material, so that the bending strength and the ablation resistance of the material are greatly affected, and the diameter of the needle is controlled to be not more than 1mm.
Further, in S3, vacuum impregnation and pressure impregnation means that firstly, the intermediate is placed in an environment with the vacuum degree lower than-0.09 MPa for standing, and then placed in the ceramic slurry prepared in S1 for pressure impregnation, wherein the pressure of the pressure impregnation is 0.5-3 MPa, and the time of the pressure impregnation is 0.5-2 h;
and S3, the curing and cracking process is carried out in inert gas, the curing temperature is 80-300 ℃, the heat preservation time is 0.5-4 h, the cracking temperature is 600-1200 ℃, the heat preservation time is 0.5-4 h, and the heating rate is 1-10 ℃/min.
In S4, the powder is silicon powder, the particle size of the powder is 0.5-200 mu m, and the mass ratio of the powder to the ceramic matrix composite intermediate is 1-5: 1, the infiltration temperature is 1400-2000 ℃, and the heat preservation time is 0.5-3 h.
The infiltration powder comprises metal silicon powder, silicon yttrium alloy, silicon hafnium alloy and glass powder.
A second object of the present invention is to provide a continuous fiber-reinforced ceramic matrix composite prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a continuous fiber reinforced ceramic matrix composite and a preparation method thereof, and an injection process adopted by the method has the advantages of short period and capability of directly densifying a sample middle area: firstly, injecting and introducing ceramic slurry with high solid content into a central area of a fiber preform, then introducing ceramic powder into other areas of the fiber preform in a slurry impregnation mode, realizing uniform distribution of the ceramic slurry in the center of the preform and other areas, and finally, adopting RMI infiltration densification to prepare the composite material. Compared with the traditional preparation process, the preparation period of the ceramic matrix composite material is only 40-70 hours.
Specifically, the beneficial effects of the invention are as follows:
(1) The invention provides a preparation method of a continuous fiber reinforced ceramic matrix composite material, which has the advantages of short preparation period, simple process, small damage to fibers, low cost and high repeatability, and is a preparation technology of a low-cost short-period composite material.
(2) The ultra-high temperature ceramic matrix composite material prepared by the method has the advantages of high densification degree, uniform component distribution and high relative density.
(3) The viscosity of the slurry and the content and the type of ceramic powder are regulated and controlled by regulating the proportion of the slurry, the content of ceramic in a composite material matrix can be regulated and controlled by combining the regulation of technological parameters, the performance of the fiber reinforced ceramic matrix composite material is further improved, the bending strength of the composite material is not lower than 400MPa, and the fracture toughness is not lower than 5.5 MPa.m 1/2 The linear ablation rate is lower than 3 mu m/s under the condition of oxyacetylene ablation at 2600-2700 ℃.
Drawings
FIG. 1 is C f /SiC-ZrB 2 A composite material preparation flow chart (a) and a mechanism chart (b).
FIG. 2 shows injection C of example 1 f /SiC-ZrB 2 CT diagram of composite material: (a) X-Z; (b) an X-Y plane; (c) 3D matrix distribution.
FIG. 3 is example 1C f /SiC-ZrB 2 Microcosmic morphology map of the intermediate of the composite material.
FIG. 4 is a graph of the microscopic morphology of the carbon fiber preform of example 1.
FIG. 5 is example 1C f /SiC-ZrB 2 And (5) a microscopic morphology graph of the composite material.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the present invention will be further described with reference to the specific examples and the accompanying drawings, but the examples are not intended to be limiting.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available unless otherwise specified.
A preparation method of a continuous fiber reinforced ceramic matrix composite material comprises the following steps:
s1: mixing a carbon source solution and ceramic powder to prepare slurry;
depositing an interface inside the fiber preform;
s2: introducing the slurry prepared in the step S1 into the central area of the fiber preform processed in the step S1 by adopting an injection method, and then performing curing and cracking to prepare an intermediate I;
s3: introducing the ceramic slurry prepared in the step S1 into the edge area of the first intermediate prepared in the step S2 by adopting a vacuum impregnation and pressure impregnation method, and then performing curing and cracking to obtain a second intermediate;
s4: and preparing an intermediate II by adopting powder embedding S3, and then densifying by adopting an RMI infiltration process to obtain the densified ceramic matrix composite.
The carbon source is a first type carbon source or a second type carbon source, and the first type carbon source is one or more of phenolic resin powder, carboxymethyl cellulose, epoxy resin, furan resin and sucrose; the second type of carbon source is one or more of carbon powder, diamond, graphene and carbon nano tube.
The ceramic powder is boride, carbide or nitride.
The fiber preform comprises carbon fibers, siC fibers, silicon nitride fibers, glass fibers, oxide fibers, or other ceramic fibers; the fiber preform is formed by two-dimensional lamination, three-dimensional needling and three-dimensional braiding.
Hereinafter referred to as C f /SiC-ZrB 2 The preparation of the composite material is illustrated by taking the composite material as an example, and as shown in fig. 1, the specific preparation steps are as follows:
step 1: depositing an interface on the needled carbon fiber preform by adopting a chemical vapor infiltration method, and controlling the thickness of the interface to be 100-600 nm.
Step 2: preparing phenolic resin solution with concentration of 30-70 wt.% and adding ZrB with particle size of 0.5-5 μm 2 Uniformly mixing the powder to obtain ceramic slurry, ball milling the ceramic slurry for 12 to 24 hours by adopting a roller ball mill at the rotating speed of 100 to 300r/min to obtain the final ceramic slurry, and performing ball milling for 41.80 seconds -1 The viscosity is 100-1200 mPa.s at a shear rate;
step 3: and (3) introducing the slurry obtained in the step (2) into the carbon fiber preform in the step (1) in an injection mode of lattice arrangement on a glue injection machine to obtain an injection embryo. Wherein the injection space between X, Y and Z direction is 2-10 mm, the inner diameter of the needle is 0.2-1 mm, the injection time of the array point is 0.5-2.0 s, the injection pressure is 0.5-1.5 MPa, and the injection volume is 0.3-1.2 cm 3 。
Step 4: solidifying the injection embryo body obtained in the step 3 at 150-300 ℃, preserving heat for 1-2 h, then cracking at 600-1200 ℃, preserving heat for 1-4 h, and carrying out the whole process in a fluid medium of Ar gas at a heating rate of 2-5 ℃/min.
Step 5: c after cleavage in step 4 f /SiC-ZrB 2 And (3) a composite intermediate, wherein the ceramic slurry obtained in the step (2) is subjected to vacuum impregnation and pressure impregnation. Wherein the vacuum degree of vacuum impregnation is controlled below-0.09 Mpa, and the impregnation time is 0.5-1.5 h; the pressure of the pressure impregnation is controlled to be 0.5-3 MPa, and the impregnation time is 0.5-2 h.
Step 6: repeating the curing and cracking processes of the step 4 to obtain semi-densified C with 15-40% open porosity f /SiC-ZrB 2 A composite intermediate.
Step 7: semi-densifying the C obtained in step 6 f /SiC-ZrB 2 Placing the composite material intermediate in silicon powder with the grain diameter of 0.5-25 mu m, and controlling the quality of the silicon powder and the semi-densification C f /SiC-ZrB 2 The mass of the composite material intermediate is (1-5): 1, densification is carried out by adopting a reaction infiltration process, the infiltration temperature is 1400-1700 ℃, and the reaction time is as follows: and (3) 2-3 h, and finally obtaining the carbon fiber reinforced ultrahigh temperature ceramic matrix composite.
The above is specifically described by the following examples.
Example 1
Step 1: and (5) preparing slurry.
Taking 40g of phenolic resin powder, putting the powder into a beaker containing 60g of absolute ethyl alcohol, and stirring the powder for 30min on a magnetic stirrer under the condition of 1000r/min to obtain a uniformly mixed and stable phenolic resin solution; 60g of ZrB with the grain diameter of 1-3 mu m is taken 2 Adding the powder into a beaker containing 40g of phenolic resin solution, stirring for 30min on a magnetic stirrer under the condition of 1200r/min, and performing roller ball milling for 12h under the condition of 120r/min rotating speed to obtain ZrB which is uniformly and stably mixed 2 Ceramic slurry.
Step 2: and (3) depositing a pyrolytic carbon PyC interface on the needled carbon fiber preform by adopting a chemical vapor infiltration method, stopping deposition when the thickness of the interface is 100nm, and performing heat treatment.
Step 3: and (3) adopting a dispensing machine to obtain ZrB in the step (1) 2 And (3) introducing the ceramic slurry into the carbon fiber preform after the interface is deposited in the step (2). The inner diameter of the needle head is 0.9mm, the distance between the injection array points in the X and Y directions is 5mm, the distance between the injection array points in the Z direction is 5mm, the injection time is 0.5s, and the injection pressure is 0.5MPa.
Step 4: taking Ar gas as a fluid medium in a vacuum tube furnace, and under the heating rate of 5 ℃/min, the composite material obtained in the step 3 is subjected to solidification temperature of 200 ℃, heat preservation time of 2h, cracking temperature of 1000 ℃ and heat preservation time of 3h to prepare the composite material with the density of 1.2g/cm 3 Porous C of (2) f /SiC-ZrB 2 Composite intermediates (as shown in fig. 3).
Step 5: slurry impregnation
The slurry dipping treatment is divided into two steps of vacuum dipping and pressure dipping: firstly, placing the composite material in the step 4 into a glass drying dish, vacuumizing until the pressure in the dish is lower than-0.09 MPa, and keeping for 30minZrB of the porous composite intermediate immersed in step 1 2 The ceramic slurry was held for 30min. And then placing the slurry and the composite material in a closed container, pressurizing to 0.5MPa, taking out after maintaining for 0.5h, wiping the surface of the preform, and drying.
Step 6: the curing and cracking process of step 4 is repeated.
Step 7: in-situ generation of SiC by a reaction melt infiltration method: placing the prepared carbon fiber composite material intermediate and silicon powder with the particle size of 0.5-25 μm into a graphite crucible by adopting an embedding method, sending into a vacuum infiltration furnace, and carrying out a reaction melt infiltration process in a vacuum environment, wherein the heat preservation temperature and the heat preservation time are 1400 ℃ and 30min respectively, and the mass ratio of the silicon powder to the ceramic matrix composite material intermediate is 1:1, and then finish C f /SiC-ZrB 2 Preparation of the sample.
Comparative example 1
Step 1: the density is 1.4g/cm by adopting the CVI process 3 The porous C/SiC composite material preform of the (2) has a pyrolytic carbon interface layer thickness of 150-250 nm, an open porosity of about 40%, a carbon fiber volume fraction of about 30%, ultrasonic cleaning of alcohol as a cleaning agent for 1h, and drying at 150 ℃ for 1h.
Step 2: 50mL of xylene, 4mL of liquid PCS, 30g of ZrB were used 2 The powder, dispersant BYK-057 is 3% of powder mass fraction and the mass is 0.95g. And (3) carrying out ultrasonic dispersion on the slurry for 1h, carrying out planetary ball milling at a rotating speed of 250r/min, and carrying out ball milling for 12h.
Step 3: the slurry was vacuum impregnated into the porous C/SiC composite preform for 0.5h at a vacuum of-0.09 MPa, and the vacuum impregnated composite was then re-impregnated for 1h at a pressure of 0.8MPa and then dried for 1h at 150 ℃.
Step 4: and (3) repeating the step (3) until the weight gain rate of the sample is not more than 3%.
Step 5: preparing a mixed solution of a SiC precursor and an organic solvent in a mass ratio of 1:1, wherein the organic solvent is dimethylbenzene, carrying out vacuum pressure impregnation on the composite material obtained in the step 4 by adopting the mixed solution, wherein the vacuum pressure impregnation step 3 is the same, the cracking process is that the heating rate is 5 ℃/min, the cracking temperature is 1400 ℃, and the cracking time is 2h.
Step 6: the final densification is achieved after repeating step 5 three times.
Comparative example 1C f /ZrB 2 The apparent density of the SiC composite material can reach 2.40g/cm 3 The open porosity is lower than 13%, and ZrB in the composite material 2 The volume fraction of the matrix is about 15%. The bending strength is 230-400 MPa, and the fracture toughness is 1.39-8.20 MPa.m 1/2 The line ablation rate was about 3.1 μm/s at 2200℃for 30 seconds of oxyacetylene ablation, according to the GJB323B-2018 ablation material ablation experimental method test standard.
Example 1 preparation C compared to comparative example 1 f /SiC-ZrB 2 The period of the composite material is only 40 hours, the content of the ultra-high temperature powder is 20Vol percent, the relative density reaches 92.4 percent, the bending strength is improved by 25 percent, and the ablation resistance is improved by 80 percent. The linear ablation rate is lower than 3 mu m/s under the oxyacetylene ablation condition of 2600-2700 ℃. FIG. 2 shows injection C of example 1 f /SiC-ZrB 2 CT diagram of composite material: (a) X-Z; (b) an X-Y plane; (c) 3D matrix distribution; it can be seen that the components are uniformly distributed. FIG. 3 is example 1C f /SiC-ZrB 2 A composite intermediate microcosmic topography map; FIG. 4 is a graph of the microscopic morphology of the carbon fiber preform of example 1; FIG. 5 is example 1C f /SiC-ZrB 2 The microcosmic appearance diagram of the composite material shows that the components are uniformly distributed and the fiber structure is complete.
The invention has the advantages of protecting the structural integrity of the fiber in the preparation process, improving the uniform distribution of the internal components of the material, greatly shortening the preparation period of the composite material and meeting the industry requirements.
Example 2
Step 1: and (5) preparing slurry.
Taking 50g of phenolic resin powder, putting the phenolic resin powder into a beaker containing 50g of absolute ethyl alcohol, and stirring the phenolic resin powder for 30min on a magnetic stirrer at the speed of 1000r/min to obtain a uniformly mixed and stable phenolic resin solution; 60g of ZrB with the grain diameter of 0.5 to 3um is taken 2 Adding the powder into a beaker containing 40g of phenolic resin solution, stirring for 30min on a magnetic stirrer under the condition of 1200r/min, and performing roller ball milling for 12h under the condition of 120r/min rotation speed to obtain uniform mixingUniform and stable ZrB 2 Ceramic slurry.
Step 2: and (3) depositing a pyrolytic carbon PyC interface on the needled carbon fiber preform by adopting a chemical vapor infiltration method, stopping deposition when the thickness of the interface is 600nm, and performing heat treatment.
Step 3: and (3) adopting a dispensing machine to obtain ZrB in the step (1) 2 And (3) introducing the ceramic slurry into the carbon fiber preform after the interface is deposited in the step (2). The inner diameter of the needle head is 0.9mm, the distance between the injection array points in the X and Y directions is 5mm, the distance between the injection array points in the Z direction is 5mm, the injection time is 2s, and the injection pressure is 1.5MPa.
Step 4: taking Ar gas as a fluid medium in a vacuum tube furnace, and under the heating rate of 5 ℃/min, the composite material obtained in the step 3 is subjected to solidification temperature of 200 ℃, heat preservation time of 2h, cracking temperature of 1000 ℃ and heat preservation time of 3h, so that the density of 1.3g/cm is prepared 3 C f /SiC-ZrB 2 A composite intermediate.
Step 5: slurry impregnation
The slurry dipping treatment is divided into two steps of vacuum dipping and pressure dipping: firstly, putting the composite material in the step 4 into a glass drying vessel, vacuumizing until the pressure in the vessel is lower than-0.1 MPa, and immersing the porous composite material intermediate into ZrB in the step 1 after 30min of maintaining 2 The ceramic slurry was held for 30min. And then placing the slurry and the composite material into a closed container, pressurizing to 3MPa, keeping for 1.5h, taking out, wiping the surface of the preform, and drying.
Step 6: the curing and cracking process of step 4 is repeated.
Step 7: in-situ generation of SiC by a reaction melt infiltration method: placing the prepared carbon fiber composite material and silicon powder with the particle size of 0.5-25 mu m into a graphite crucible by adopting an embedding method, sending the graphite crucible into a vacuum infiltration furnace, and carrying out a reaction melt infiltration process in a vacuum environment, wherein the heat preservation temperature and the heat preservation time are 1700 ℃ and 30min respectively, and the mass ratio of the silicon powder to the ceramic matrix composite material intermediate is 5:1, and then finish C f /SiC-ZrB 2 Preparation of the sample.
C prepared by the invention f /SiC-ZrB 2 The composite material only needs to be soaked once in the preparation processCompared with the PIP and other technological methods, the preparation time is greatly shortened, and the preparation cost is reduced.
Example 3
Step 1: and (5) preparing slurry.
Taking 50g of phenolic resin powder, putting the phenolic resin powder into a beaker containing 50g of absolute ethyl alcohol, and stirring the phenolic resin powder for 30min on a magnetic stirrer at the speed of 1000r/min to obtain a uniformly mixed and stable phenolic resin solution; 70g of ZrB with the grain diameter of 0.5-3 mu m is taken 2 Adding the powder into a beaker containing 30g of phenolic resin solution, stirring for 30min on a magnetic stirrer under the condition of 1200r/min, and performing roller ball milling for 12h under the condition of 120r/min rotating speed to obtain ZrB which is uniformly and stably mixed 2 Ceramic slurry.
Step 2: and (3) depositing a pyrolytic carbon PyC interface on the needled carbon fiber preform by adopting a chemical vapor infiltration method, stopping deposition when the thickness of the interface is 600nm, and performing heat treatment.
Step 3: and (3) adopting a dispensing machine to obtain ZrB in the step (1) 2 And (3) introducing the ceramic slurry into the carbon fiber preform after the interface is deposited in the step (2). The inner diameter of the needle head is 0.9mm, the distance between the injection array points in the X and Y directions is 5mm, the distance between the injection array points in the Z direction is 5mm, the injection time is 1s, and the injection pressure is 1MPa.
Step 4: taking Ar gas as a fluid medium in a vacuum tube furnace, and under the heating rate of 5 ℃/min, the composite material obtained in the step 3 is subjected to solidification temperature of 200 ℃, heat preservation time of 2h, cracking temperature of 1000 ℃ and heat preservation time of 3h, so that the density of 1.5g/cm is prepared 3 Porous C of (2) f /SiC-ZrB 2 A composite intermediate.
Step 5: slurry impregnation
The slurry dipping treatment is divided into two steps of vacuum dipping and pressure dipping: firstly, putting the composite material in the step 4 into a glass drying vessel, vacuumizing until the pressure in the vessel is lower than-0.09 MPa, and immersing the porous composite material intermediate into ZrB in the step 1 after 30min of maintaining 2 The ceramic slurry was held for 30min. And then placing the slurry and the carbon fiber preform into a closed container, pressurizing for 2MPa, keeping for 1h, taking out, wiping the surface of the preform, and drying.
Step 6: the curing and cracking process of step 4 is repeated.
Step 7: in-situ generation of SiC by a reaction melt infiltration method: placing the prepared composite material intermediate and silicon powder with the grain diameter of 0.5-25 mu m into a graphite crucible by adopting an embedding method, sending into a vacuum infiltration furnace, and performing a reaction melt infiltration process in a vacuum environment, wherein the heat preservation temperature and the heat preservation time are respectively 1500 ℃ and 30min, thereby completing C f /SiC-ZrB 2 Preparation of the sample.
In comparison with comparative example 1, this example produces C f /SiC-ZrB 2 The content of the ultra-high temperature powder of the composite material is 25Vol percent, and the ablation resistance is improved by 120 percent.
Example 4
Step 1: and (5) preparing slurry.
Taking 50g of phenolic resin powder, putting the phenolic resin powder into a beaker containing 50g of absolute ethyl alcohol, and stirring the phenolic resin powder for 30min on a magnetic stirrer at the speed of 1000r/min to obtain a uniformly mixed and stable phenolic resin solution; 70g of ZrB with the grain diameter of 0.5-3 mu m is taken 2 Adding the powder into a beaker containing 30g of phenolic resin solution, stirring for 30min on a magnetic stirrer under the condition of 1200r/min, and performing roller ball milling for 12h under the condition of 120r/min rotating speed to obtain ZrB which is uniformly and stably mixed 2 Ceramic slurry.
Step 2: and (3) depositing a pyrolytic carbon PyC interface on the needled carbon fiber preform by adopting a chemical vapor infiltration method, stopping deposition when the thickness of the interface is 100-600 nm, and performing heat treatment.
Step 3: and (3) adopting a dispensing machine to obtain ZrB in the step (1) 2 And (3) introducing the ceramic slurry into the carbon fiber preform after the interface is deposited in the step (2). The inner diameter of the needle head is 0.9mm, the distance between the injection array points in the X and Y directions is 3mm, the distance between the injection array points in the Z direction is 3mm, the injection time is 1s, and the injection pressure is 1MPa.
Step 4: taking Ar gas as a fluid medium in a vacuum tube furnace, and under the heating rate of 5 ℃/min, the composite material obtained in the step 3 is subjected to solidification temperature of 200 ℃, heat preservation time of 2h, cracking temperature of 1000 ℃ and heat preservation time of 3h, so that the density of 1.65g/cm is prepared 3 C of (2) f /SiC-ZrB 2 A composite intermediate.
Step 5: slurry impregnation
The slurry dipping treatment is divided into two steps of vacuum dipping and pressure dipping: firstly, putting the composite material in the step 4 into a glass drying vessel, vacuumizing until the pressure in the vessel is lower than-0.09 MPa, and immersing the porous composite material intermediate into ZrB in the step 1 after 30min of maintaining 2 The ceramic slurry was held for 30min. And then placing the slurry and the composite material into a closed container, pressurizing for 2MPa, taking out after keeping for 1h, and wiping and drying the surface of the preform.
Step 6: the curing and cracking process of step 4 is repeated.
Step 7: in-situ generation of SiC by a reaction melt infiltration method: the prepared carbon fiber composite material and silicon powder with the grain diameter of 0.5-25 mu m are placed into a graphite crucible by adopting an embedding method, are sent into a vacuum infiltration furnace, and undergo a reaction melt infiltration process in a vacuum environment, wherein the heat preservation time and the heat preservation temperature are 1400-1700 ℃ and 30min respectively, and then C is completed f /SiC-ZrB 2 Preparation of the sample.
This example compares example 3 post-injection C f /SiC-ZrB 2 The volume density of the composite material intermediate is improved by 16.2%, and the ablation resistance is improved by 70%.
Comparative example 2
Step 1: and (5) preparing slurry.
Taking 50g of phenolic resin powder, putting the phenolic resin powder into a beaker containing 50g of absolute ethyl alcohol, and stirring the phenolic resin powder for 30min on a magnetic stirrer at the speed of 1000r/min to obtain a uniformly mixed and stable phenolic resin solution; 70g of ZrB with the grain diameter of 0.5-3 mu m is taken 2 Adding the powder into a beaker containing 30g of phenolic resin solution, stirring for 30min on a magnetic stirrer under the condition of 1200r/min, and performing roller ball milling for 12h under the condition of 120r/min rotating speed to obtain ZrB which is uniformly and stably mixed 2 Ceramic slurry.
Step 2: and (3) depositing a pyrolytic carbon PyC interface on the needled carbon fiber preform by adopting a chemical vapor infiltration method, stopping deposition when the thickness of the interface is 600nm, and performing heat treatment.
Step 3: adopts a dispensing machine to dispenseZrB obtained in step 1 2 And (3) introducing the ceramic slurry into the carbon fiber preform after the interface is deposited in the step (2). The inner diameter of the needle head is 1.45mm, the distance between the injection array points in the X and Y directions is 5mm, the distance between the injection array points in the Z direction is 5mm, the injection time is 1s, and the injection pressure is 1MPa.
Step 4: taking Ar gas as a fluid medium in a vacuum tube furnace, and under the heating rate of 5 ℃/min, the composite material obtained in the step 3 is subjected to solidification temperature of 200 ℃, heat preservation time of 2h, cracking temperature of 1000 ℃ and heat preservation time of 3h, so that the density of 1.65g/cm is prepared 3 C of (2) f /SiC-ZrB 2 A composite intermediate.
Step 5: slurry impregnation
The slurry dipping treatment is divided into two steps of vacuum dipping and pressure dipping: firstly, putting the composite material in the step 4 into a glass drying vessel, vacuumizing until the pressure in the vessel is lower than-0.09 MPa, and immersing the porous composite material intermediate into ZrB in the step 1 after 30min of maintaining 2 The ceramic slurry was held for 30min. And then placing the slurry and the carbon fiber preform into a closed container, pressurizing for 2MPa, keeping for 1h, taking out, wiping the surface of the preform, and drying.
Step 6: the curing and cracking process of step 4 is repeated.
Step 7: in-situ generation of SiC by a reaction melt infiltration method: placing the prepared carbon fiber composite material and silicon powder with the grain diameter of 0.5-200 mu m into a graphite crucible by adopting an embedding method, sending into a vacuum infiltration furnace, and carrying out a reaction melt infiltration process in a vacuum environment, wherein the heat preservation temperature and the heat preservation time are respectively 1500 ℃ and 30min, and the mass ratio of the silicon powder to the ceramic matrix composite material intermediate is 3:1, and then finish C f /SiC-ZrB 2 Preparation of the sample.
Comparative example 2C after injection compared to example 3 f /SiC-ZrB 2 The volume density and the open porosity of the composite material intermediate are similar, but the diameter of the needle exceeds 1mm, and C is prepared f /SiC-ZrB 2 Obvious holes are reserved on the surface of the composite material, so that the bending strength and the ablation resistance of the material are greatly affected.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that such modifications and variations be included herein within the scope of the appended claims and their equivalents.
Claims (10)
1. The preparation method of the continuous fiber reinforced ceramic matrix composite material is characterized by comprising the following steps of:
s1: mixing a carbon source solution and ceramic powder to prepare slurry;
depositing an interface inside the fiber preform;
s2: introducing the slurry prepared in the step S1 into the central area of the fiber preform processed in the step S1 by adopting an injection method, and then curing and cracking to prepare an intermediate I;
s3: vacuum impregnation and pressure impregnation are adopted, the ceramic slurry prepared in the step S1 is introduced into the area except the central area in the step S2 intermediate I, and then solidification and cracking are carried out, so that an intermediate II is obtained;
s4: and embedding the second intermediate by adopting powder, and then densifying by adopting an RMI infiltration process to obtain the densified ceramic matrix composite.
2. The preparation method of claim 1, wherein in S1, the carbon source is a first type carbon source or a second type carbon source, and the first type carbon source is one or more of phenolic resin, carboxymethyl cellulose, epoxy resin, furan resin and sucrose; the second type of carbon source is one or more of carbon powder, diamond, graphene and carbon nano tube;
the solvent is one or more of water, absolute ethyl alcohol, toluene and xylene;
the carbon source content in the carbon source solution is 30-70 wt.%.
3. The method according to claim 1, wherein in S1, the ceramic powder is boride, carbide or nitride;
the content of the ceramic powder in the slurry is 5-90 wt%;
the grain diameter of the ceramic powder is 0.05-50 mu m.
4. The method according to claim 1, wherein in S1, the fiber preform is a carbon fiber, a SiC fiber, a silicon nitride fiber, a glass fiber, or an oxide fiber;
the fiber preform is formed by two-dimensional lamination, three-dimensional needling fiber or three-dimensional braiding;
the fiber content of the fiber preform is 10 to 75vol.%.
5. The method of claim 1, wherein the interfacial material in S1 is PyC, BN, siC, si 3 N 4 One or more of the following;
the deposition thickness of the interface is 100-600 nm.
6. The method according to claim 1, wherein in S2, the slurry is arranged in a lattice in a central region of the fiber preform, and the injection lattice is arranged in a circular, rectangular or irregular shape;
s2, curing and cracking are carried out in inert gas, wherein the curing temperature is 80-300 ℃, and the heat preservation time is 0.5-4 h; the cracking temperature is 600-1200 ℃, and the heat preservation time is 0.5-4 h.
7. The preparation method according to claim 6, wherein in S2, the injection interval between X, Y and Z direction is 2-10 mm, the inner diameter of the needle is 0.2-1 mm, the injection time of the lattice point is 0.5-2.0S, and the injection pressure is 0.5-1.5 MPa.
8. The preparation method according to claim 1, wherein in the step S3, vacuum impregnation and pressure impregnation means that the intermediate is placed in an environment with a vacuum degree lower than-0.09 MPa for standing, and then placed in the ceramic slurry prepared in the step S1 for pressure impregnation, wherein the pressure of the pressure impregnation is 0.5-3 MPa, and the time of the pressure impregnation is 0.5-2 h;
in S3, the curing and cracking process is carried out in inert gas, the curing temperature is 80-300 ℃, the heat preservation time is 0.5-4 h, the cracking temperature is 600-1200 ℃, and the heat preservation time is 0.5-4 h.
9. The preparation method according to claim 1, wherein in S4, the powder is silicon powder, the particle size of the powder is 0.5-200 μm, and the mass ratio of the powder to the intermediate II is 1-5: 1.
s4, the infiltration temperature is 1400-2000 ℃, and the heat preservation time is 0.5-3 h.
10. A continuous fiber reinforced ceramic matrix composite prepared according to the preparation method of any one of claims 1 to 9.
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