CN116514565A - Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite material and preparation method thereof - Google Patents
Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite material and preparation method thereof Download PDFInfo
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- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 33
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 78
- 239000002243 precursor Substances 0.000 claims abstract description 56
- 238000005336 cracking Methods 0.000 claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 28
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 238000004132 cross linking Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 25
- 238000005470 impregnation Methods 0.000 claims description 22
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 20
- 239000004917 carbon fiber Substances 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 17
- 230000008021 deposition Effects 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005011 phenolic resin Substances 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 6
- -1 propyl titanate Chemical compound 0.000 claims description 5
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- WIEXMPDBTYDSQF-UHFFFAOYSA-N 1,3-bis(furan-2-yl)propan-2-one Chemical compound C=1C=COC=1CC(=O)CC1=CC=CO1 WIEXMPDBTYDSQF-UHFFFAOYSA-N 0.000 claims description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 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
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 239000007849 furan resin Substances 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 claims description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract description 12
- 238000007598 dipping method Methods 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 36
- 238000002679 ablation Methods 0.000 description 15
- 239000000243 solution Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 11
- 239000004744 fabric Substances 0.000 description 7
- URXDOZXTRQGRIP-UHFFFAOYSA-N [Hf].[Zr].[Ti] Chemical compound [Hf].[Zr].[Ti] URXDOZXTRQGRIP-UHFFFAOYSA-N 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 230000003628 erosive effect Effects 0.000 description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000013001 point bending Methods 0.000 description 4
- 238000000197 pyrolysis Methods 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000003776 cleavage reaction Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
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- 229910052735 hafnium Inorganic materials 0.000 description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 3
- 230000007017 scission Effects 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000004140 cleaning Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- QFXZANXYUCUTQH-UHFFFAOYSA-N ethynol Chemical group OC#C QFXZANXYUCUTQH-UHFFFAOYSA-N 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
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- 239000000843 powder Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000012700 ceramic precursor Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
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- 239000007788 liquid Substances 0.000 description 1
- 238000000626 liquid-phase infiltration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000011216 ultra-high temperature ceramic matrix composite Substances 0.000 description 1
- 239000011215 ultra-high-temperature ceramic Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
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Abstract
The invention discloses a Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite material and a preparation method thereof, comprising the following steps: step 1: preparing a high-texture pyrolytic carbon interface phase on the surface of a composite material preform; step 2: impregnating the composite material preform; step 3: cross-linking and solidifying the impregnated composite material preform; step 4: cracking the crosslinked and solidified composite material preform; step 5: repeating the steps 2, 3 and 4 until the density of the obtained composite material preform reaches 2.5-3.5 g/cm 3 . The invention adopts the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite material and the preparation method thereof, thereby effectively improving the space among ceramics, pyrolytic carbon and carbon fibersThe interface combination of the precursor and the fiber is relieved, the high-efficiency dipping and cracking of the composite material at a lower temperature is realized by adopting multiple rounds of different viscosities, and the component uniformity and bending mechanical property of the composite material are improved.
Description
Technical Field
The invention relates to the technical field of ceramic matrix composite materials, in particular to a Cf/(Ti, zr, hf) C entropy ceramic matrix composite material and a preparation method thereof.
Background
The development of new generation spacecraft is attracting great interest in ultra-high temperature refractory materials, when the Mach number 6 of hypersonic aircraft is increased to be more than Mach number 10, the surface temperature of high temperature structural components such as the end head and the front edge can reach 2000-2800 ℃, and the high oxidation and airflow scouring environment are accompanied. Accordingly, the corresponding material needs to have a higher melting point. The current ultra-high temperature ceramic matrix composite materials with zirconium carbide-silicon carbide, zirconium boride-silicon carbide, hafnium carbide-silicon carbide and the like as matrixes are difficult to meet such severe high temperature use environments, and the matrix components of the ceramic matrix composite materials need to be improved.
In recent years, mid-entropy carbide ceramics have received attention for their extremely high melting point, high hardness, high thermal conductivity, and good oxidation resistance. Compared with single-phase ceramics, the medium-entropy ceramics have higher mechanical property and better oxidation resistance, and are expected to become candidate materials for high-temperature structural members of aircrafts with higher Mach numbers in the future. However, the medium-entropy ceramic material has the problems of large brittleness, poor toughness and the like. In addition, the conventional process method for preparing the continuous fiber toughened ceramic matrix composite material comprises slurry impregnation, chemical vapor deposition, reactive melt infiltration and precursor impregnation cracking, and compared with other preparation processes, the precursor impregnation cracking (PIP) method can be performed at a lower preparation temperature, so that the damage to the fiber preform in the preparation process is effectively reduced, and the mechanical property of the composite material is improved. More importantly, the elements in the polymer precursor are uniformly dispersed at molecular level, so that the uniform distribution of the elements is maintained in the curing and cracking processes, and the completely chemically uniform solid solution ceramic is obtained. However, the PIP method is required to be subjected to multiple rounds of impregnation pyrolysis process when preparing the ceramic matrix composite material, and the ultra-high temperature ceramic precursor is preparedThe body is easy to react with carbon fiber interface phase in the cracking process, erodes the fiber matrix, causes fiber bundle deformation, forms large defects in the composite material, and causes the mechanical property of the prepared composite material to be lower. Therefore, how to ensure that the prepared composite material internal ceramic and the fiber fabric have good interface combination, and the mechanical property of the composite material is C by adjusting the bending fracture mode of the fiber f The key challenges to be addressed in the preparation and use of entropy ceramic matrix composites in/(Ti, zr, hf) C are urgent.
Disclosure of Invention
The invention aims to provide a Cf/(Ti, zr, hf) C entropy ceramic matrix composite material and a preparation method thereof, which effectively improve interface combination among ceramics, pyrolytic carbon and carbon fibers, relieve erosion problem of precursors to the fibers, realize efficient impregnation and pyrolysis of the composite material at a lower temperature by adopting multiple rounds of different viscosities, and improve component uniformity and bending mechanical property of the composite material.
In order to achieve the above purpose, the invention provides a Cf/(Ti, zr, hf) C entropy ceramic matrix composite and a preparation method thereof, comprising the following steps:
step 1: preparing a high-texture pyrolytic carbon interface phase on the surface of a composite material preform;
step 2: impregnating the composite material preform;
step 3: cross-linking and solidifying the impregnated composite material preform;
step 4: cracking the crosslinked and solidified composite material preform;
step 5: repeating the steps 2, 3 and 4 until the density of the obtained composite material preform reaches 2.5-3.5 g/cm 3 。
Preferably, in the step 1, the fiber volume fraction of the composite material preform is 45-55%, the composite material preform is placed into a chemical vapor deposition furnace, the heating rate is 3-5 ℃/min, the temperature is kept at the deposition temperature of 900-1000 ℃ for 1 hour, a methane deposition air source is introduced into the chemical vapor deposition furnace, the heating rate is 3-5 ℃/min, the temperature is kept at the deposition temperature of 900-1000 ℃ for 1 hour, and the density of 1.1-1.4g/cm 3 Is provided.
Preferably, in the step 2, the obtained composite material preform with the high-texture pyrolytic carbon interface phase is placed in an impregnation tank, then the impregnation tank is sealed and vacuumized until the pressure in the tank is between-0.1 Mpa and-0.05 Mpa, the precursor solution is pumped in by vacuum suction, and the impregnation is carried out for 1 to 2 hours under the vacuum pressure condition.
Preferably, the solute of the precursor solution comprises a precursor and a carbon source precursor, the solvent of the precursor solution is an organic solvent, and the viscosity of the precursor solution is divided into low viscosity of 100-150 mPa.s and high viscosity of 250-300 mPa.s.
Preferably, the precursor is prepared by cohydrolytic polycondensation of propyl titanate, propyl zirconate and propyl hafnate; the carbon source precursor is one or more of phenolic resin, furfuryl ketone resin, sucrose and furan resin; the organic solvent is one or more of methanol, isopropanol, ethanol, n-propanol, isobutanol, n-butanol, ethylene glycol methyl ether and ethylene glycol ethyl ether.
Preferably, in the step 3, after the impregnation is completed, transferring the vacuum impregnated composite material preform and the precursor solution into a pressurized impregnation kettle, introducing inert gas into the impregnation kettle, impregnating for 1 hour under the pressure condition of 2-5 Mpa and the temperature of 100 ℃, decompressing, taking out the composite material preform, and performing crosslinking curing in a blast oven.
Preferably, the inert gas is argon or nitrogen, and the flow rate of the introduced gas is 1-1000 sccm.
Preferably, in the step 4, the obtained crosslinked and cured composite material preform is placed in a vacuum environment or an inert atmosphere protection cracking furnace for cracking, the low-temperature cracking temperature is 1400-1500 ℃, the high-temperature cracking temperature is 1700-1800 ℃, and the heating rate is 5-20 ℃/min.
A Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite prepared according to the above method for preparing a Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite.
Preferably, the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite takes a carbon fiber preform as a framework, the volume fraction of the carbon fiber preform is 45-55%, and a high-texture pyrolytic carbon interface phase is deposited on the surface of the carbon fiber preform; the entropy ceramic in (Ti, zr, hf) C is used as a matrix, and the oxygen content in the matrix is not higher than 2%.
Therefore, the invention adopts the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite material and the preparation method thereof, and has the following beneficial effects:
(1) Compared with the traditional method of blending and sintering various carbide powder or doping the carbide powder into prepreg, the method can obtain a nano-grade single-phase (Ti, zr, hf) C ceramic product at a lower temperature of 1400-1500 ℃, and the element components are uniformly distributed from micron to nano. The prepared composite material has good mechanical property and very excellent oxidation and ablation resistance for 1000s under the extreme environment of 2600-2800 ℃.
(2) The high-fiber-volume-content preform used in the invention utilizes a chemical vapor deposition method to deposit a pyrolytic carbon interface layer with high texture on the surface of the carbon fiber, and the pyrolytic carbon grows around fiber bundles in the deposition process, so that the high-fiber-volume-content preform has higher microcrystalline crystallinity, fewer defects and more obvious guidance. The boundary of the other fibers is provided with a sub-layer and a connecting bridge structure, so that the interface combination of ceramics and the fibers can be effectively improved, the erosion of the precursor to the fibers can be relieved, and better interface matching can be realized. The high-texture pyrolytic carbon interface layer not only can remarkably reduce the physical and chemical damage to the fiber bundles in the cracking process, but also can lead cracks transmitted to the carbon fibers by the ceramic matrix to deflect at the high-texture interface layer preferentially, and reduce the generation of cracks in the fiber bundles, thereby promoting the energy consumption of fiber extraction and improving the bending strength of the composite material.
(3) The precursor has the carbon source proportion content with adjustable range, and the erosion of precursor cracking to fiber bundles and high-texture pyrolytic carbon interfaces on the surface layer of the fiber bundles in the PIP process is reduced as much as possible under the condition of ensuring carbon defect. The preparation method is matched with the viscosity of the precursor, multiple rounds and different temperatures of impregnation and cracking processes are designed, so that the smaller grain size of the ceramic is ensured, and the efficient impregnation preparation of the composite material is realized.
(4) The method has simple process, short preparation period and easy industrialized implementation, and can prepare complex abnormal-shaped components with various sizes. C prepared by the invention f The entropy ceramic matrix composite material in (Ti, zr, hf) C has good mechanical property and very excellent ablation resistance, passes through an atmospheric plasma wind tunnel ablation test of 1000s and 3000K, can meet the service requirement of a high-temperature structural member of a hypersonic aircraft, can be widely applied to the preparation of the high-temperature structural member of the hypersonic aircraft, and has wide application prospect in the aspects of the front edge, the engine, the end head and the like of a novel aircraft.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a diagram of the microscopic morphology of a preform with a high texture pyrolytic carbon interface layer prepared by chemical vapor deposition according to example 1 of the present invention;
FIG. 2 shows a single phase C after cleavage of the precursor obtained in example 1 of the present invention f /(Ti 0.17 Zr 0.33 Hf 0.5 ) C, a high-resolution transmission photograph of the entropy ceramic, wherein the inset is a diffraction pattern of the region after Fourier transformation;
FIG. 3 is C obtained in example 1 of the present invention f /(Ti 0.17 Zr 0.33 Hf 0.5 ) C, an X-ray diffraction spectrogram of the entropy ceramic matrix composite;
FIG. 4 is a graph of C obtained in example 1 of the present invention f /(Ti 0.17 Zr 0.33 Hf 0.5 ) And C, a microscopic phase diagram of a fracture of the entropy ceramic matrix composite after three-point bending fracture.
Detailed Description
The technical scheme of the invention is further described below through the attached drawings and the embodiments.
The preparation method of the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite material comprises the following steps:
step 1: preparation of high texture pyrolytic carbon interfacial phase on surface of composite material preform: the fine woven puncture carbon fiber fabric with high fiber volume fraction is put into a chemical vapor deposition furnace and is preserved for 1 to 1.5 hours at the temperature rising rate of 2 to 5 ℃/min to 1000 to 1300 ℃. Introducing a methane deposition gas source with the purity of 99%, controlling the deposition pressure to be 10-18 kPa, the gas residence time to be 0.3-0.5 s, the deposition speed to be 1500-2200 nm/h, and the deposition time to be 0.5-1.5 hours, cooling to room temperature along with a furnace, and depositing a pyrolytic carbon interface phase with high texture on the surface of the carbon fiber. The density of the preform after the interfacial phase is deposited reaches 1.1 to 1.4g/cm 3 . Then cleaning the preform by ultrasonic waves for 20-30 minutes, putting the preform into a baking oven for heat preservation at 100-150 ℃ for 1-2 hours and drying;
step 2: impregnating the composite material preform: placing the obtained composite material preform with the high-texture pyrolytic carbon interface phase into an impregnating tank, then sealing and vacuumizing the impregnating tank until the pressure in the tank is-0.1 to-0.5 Mpa, sucking the precursor solution by vacuum suction, and impregnating for 1-2 hours under the vacuum pressure condition;
step 3: crosslinking and curing the impregnated composite material preform: after the impregnation work is finished, transferring the composite material preform and the precursor solution after vacuum impregnation into a pressurized impregnation kettle, introducing inert gas, wherein the inert gas is argon or nitrogen, the flow rate of the introduced gas is 1-1000 sccm, impregnating for 1 hour under the pressure condition of 2-5 Mpa and the temperature of 100 ℃, decompressing, taking out the composite material preform, and carrying out crosslinking curing in a blast oven, wherein the heating speed is 3-5 ℃/min in the crosslinking curing process, preserving heat for 2-3 hours at 100-120 ℃, preserving heat for 2-3 hours at 150-160 ℃, preserving heat for 1-2 hours at 200-220 ℃ and preserving heat for 1-2 hours at 250-300 ℃.
Step 4: splitting the crosslinked and cured composite material preform: placing the obtained crosslinked and cured composite material preform in a vacuum environment or an inert atmosphere-protected cracking furnace for cracking, wherein the low-temperature cracking temperature is 1400-1500 ℃, the high-temperature cracking temperature is 1700-1800 ℃, and the heating rate is 5-20 ℃/min;
step 5: repeating the operation steps 2, 3 and 4 until the obtainedThe density of the composite material preform reaches 2.5-3.5 g/cm 3 。
Specifically, in step 2, the solute of the precursor solution includes a precursor and a carbon source precursor, the solvent of the precursor solution is an organic solvent, and the viscosity of the precursor solution is divided into a low viscosity of 100 to 150mpa.s and a high viscosity of 250 to 300 mpa.s. The precursor is prepared by cohydrolytic polycondensation of propyl titanate, propyl zirconate and propyl hafnate, and the proportion of titanium, zirconium and hafnium in the precursor is regulated and controlled by the feed ratio of the raw materials. The carbon source precursor is one or more of phenolic resin, furfuryl ketone resin, sucrose and furan resin, wherein the phenolic resin is preferably allyl phenolic resin, and the mass ratio of the allyl phenolic resin to the total metal substances in the metal alkoxide copolymer is 18-22 g/1 mol. The mass ratio of the carbon source precursor to the titanium zirconium hafnium precursor copolymer is (10-20): 1, a step of; the organic solvent is one or more of methanol, isopropanol, ethanol, n-propanol, isobutanol, n-butanol, ethylene glycol methyl ether and ethylene glycol ethyl ether, preferably ethylene glycol methyl ether, and the mass ratio of the titanium zirconium hafnium precursor copolymer contained in the titanium zirconium hafnium ceramic precursor solution to the organic solvent is 10 (2-5).
Further, the viscosity of the titanium zirconium hafnium precursor in step 2 is different for each round. Specifically, the viscosity of the precursor used in the 1 st to 2 nd rounds is 100 to 150mPa.s, the viscosity of the precursor used in the 3 rd to 6 th rounds is 250 to 300mPa.s, and the viscosity of the precursor used in the 7 th to 8 th rounds is less than 100mPa.s.
Further, the cleavage temperature is different for each round of step 4. Specifically, the cracking temperature of each of the 1 st to 6 th wheels is 1400 to 1500 ℃, and then the cracking temperature of each of the 7 th to 8 th wheels is 1700 to 1800 ℃; the cleavage time is preferably 2 to 5 hours. If the number of preparation rounds is small, the final cracking at 1700-1800 ℃ is ensured.
The invention is further illustrated by the following specific examples.
Example 1
Step 1: preparing a high-texture pyrolytic carbon interface phase on the surface of a composite material preform: placing the finely woven puncture carbon fiber fabric with the fiber volume fraction of 53% into a chemical vapor deposition furnace, and heating to 1100 ℃ at a heating rate of 3 ℃/minThe temperature was kept for 1 hour. Introducing a methane deposition gas source with the purity of 99%, controlling the deposition pressure to be 15kPa, the gas residence time to be 0.5s, the deposition speed to be 2000nm/h, and the deposition time to be 1 hour, cooling to room temperature along with a furnace, and depositing a pyrolytic carbon interface phase with high texture on the surface of the carbon fiber. The density of the fine woven puncture carbon fiber preform after the interface phase is deposited reaches 1.13g/cm 3 . And cleaning the preform deposited with the pyrolytic carbon interface phase by ultrasonic waves for 20 minutes, and then, preserving the temperature of the oven at 120 ℃ for 2 hours and drying.
Step 2: impregnating the composite material preform: placing the composite material preform in the step 1 into an impregnating tank, sealing, vacuumizing for 15min until the pressure in the tank is-0.1 Mpa, and sucking a precursor solution, wherein titanium in the precursor solution: zirconium: the mole ratio of hafnium is 1:2:3. and (3) immersing for 1 hour in a vacuum environment, transferring the composite material and the immersion liquid after vacuum immersion into a pressure kettle, introducing nitrogen, raising the pressure to 3MPa, raising the temperature to 100 ℃ at a heating rate of 2 ℃/min, and immersing for 1 hour, so that the precursor solution is fully immersed into the composite fabric.
Step 3: crosslinking and curing the impregnated composite material preform: after the impregnation is finished, the composite material preform is decompressed and taken out, the composite material preform is placed in a blast oven, the temperature is raised to 100 ℃ at 3 ℃/min, the temperature is kept for 3 hours at 150 ℃, the temperature is kept for 1 hour at 200 ℃, the temperature is kept for 2 hours at 250 ℃, and the titanium-zirconium-hafnium precursor is fully crosslinked and solidified.
Step 4: splitting the crosslinked and cured composite material preform: placing the fabric obtained in the step 3 into a cracking furnace for cracking: keeping the heating rate at 10 ℃/min, carrying out argon environment cracking for 2 hours, cooling to room temperature along with a furnace, and taking out a sample.
Step 5: repeating the operation steps 2, 3 and 4. The viscosity of the titanium zirconium hafnium precursor in the step 2 is different in each round, the viscosity of the precursor used in the 1 st round to the 2 nd round is 150mPa.s, the viscosity of the precursor used in the 3 rd round to the 6 th round is 250mPa.s, and the viscosity of the precursor used in the 7 th round to the 8 th round is 90mPa.s. Wherein, in the step 4, the cracking temperature of the 1 st to 4 th rounds is 1500 ℃, the cracking temperature of the 6 th to 8 th rounds is 1800 ℃, and the density of the obtained composite material is 2.66g/cm 3 。
The microstructure of the preform with high fiber content and high texture interface phase prepared by the embodiment is shown in figure 1, the interface layer can better wrap the whole fiber bundle, thereby being beneficial to protecting the fiber from the erosion effect of the precursor pyrolysis process, realizing better interface combination with the ceramic phase and improving the mechanical property of the composite material
Single phase C prepared in this experimental example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) The high resolution transmission electron microscope picture of C ceramic is shown in FIG. 2, wherein the inset is the region after Fourier transform [100 ]]Crystal plane diffraction pattern. The product obtained is in the form of a face-centered cubic single phase (Ti 0.17 Zr 0.33 Hf 0.5 ) C, ceramic.
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) The C composite material was subjected to density testing by Archimedes drainage method, and the measured drainage method density was 2.92g/cm 3 The porosity is 8.9%, and the compactness of the composite material is higher.
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) Phase analysis of the C composite material was performed using XRD diffractometer as shown in FIG. 3, and it can be seen that the material was composed mainly of C and single phase (Ti 0.17 Zr 0.33 Hf 0.5 ) And C, amplifying the characteristic diffraction peak without dividing the peak, and obtaining the single-phase ceramic with better solid solution effect.
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) And C, testing the room-temperature bending strength of the composite material by using a three-point bending method, wherein the room-temperature bending strength of the material is 252.64Mpa.
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) C composite material is subjected to plasma wind tunnel ablation resistance test, and the heat flux density is 3.6Mw/m 2 Ablation at high temperature at dwell point pressure 5kPa,2973K for 1000s with a linear ablation rate of only 5.1X10 -4 mm/s, has very excellent ultra-high temperature ablation resistance.
Example 2
Unlike example 1, the present example used a needled carbon fiber fabric with a fiber volume fraction of 50%, and the density of the deposited needled carbon fiber preform reached 1.1g/cm 3 The preparation method is the same as in example 1, and the density of the prepared composite material is 2.67g/cm 3 。
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) The C composite material was subjected to density testing by Archimedes drainage method, and the measured drainage method density was 2.76g/cm 3 The porosity is 6.88%, and the compactness of the composite material is higher.
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) Phase analysis of the C composite material was performed using XRD diffractometer, and it was found that the material consisted mainly of C and single phase (Ti 0.17 Zr 0.33 Hf 0.5 ) And C, the ceramic composition is characterized in that the characteristic diffraction peak is amplified and is not separated, and the obtained single-phase ceramic has a good solid solution effect.
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) And C, testing the room-temperature bending strength of the composite material by using a three-point bending method, wherein the room-temperature bending strength of the material is 291.51Mpa. The microscopic morphology of the fracture after bending test is shown in fig. 4, and a remarkable fiber pulling-out phenomenon can be observed.
C prepared in this example f /(Ti 0.17 Zr 0.33 Hf 0.5 ) C composite material is subjected to oxyacetylene ablation resistance test, and the heat flux density is 5Mw/m 2 Ablation at 2700K at high temperature for 200s with a linear ablation rate of only 3.75X10 -4 mm/s, has very excellent ultra-high temperature ablation resistance.
Example 3
As in example 1, a finely woven and needled carbon fiber fabric with a fiber volume fraction of 53% was used to prepare a finely woven and needled carbon fiber preform with a density of 1.16g/cm after deposition of the interfacial phase 3 . The preparation method is the same as in example 1, and the density of the obtained composite material is 2.42g/cm 3 。
C prepared in this example f /(Ti 0.33 Zr 0.33 Hf 0.34 ) The C composite material was subjected to density testing by Archimedes drainage method, and the measured drainage method density was 2.63g/cm 3 The porosity is 7.98%, and the compactness of the composite material is high.
C prepared in this example f /(Ti 0.33 Zr 0.33 Hf 0.34 ) The C composite material is subjected to phase analysis by using an XRD diffractometer, and the material is mainly composed of C and single-phase C f /(Ti 0.33 Zr 0.33 Hf 0.34 ) And C, the ceramic composition is characterized in that the characteristic diffraction peak is amplified and is not separated, and the obtained single-phase ceramic has a good solid solution effect.
C prepared in this example f /(Ti 0.33 Zr 0.33 Hf 0.34 ) And C, testing the room-temperature bending strength of the composite material by using a three-point bending method, wherein the room-temperature bending strength of the material is 270.45Mpa.
C prepared in this example f /(Ti 0.33 Zr 0.33 Hf 0.34 ) C composite material is subjected to oxyacetylene ablation resistance test, and the heat flux density is 5Mw/m 2 Ablation at 2700K high temperature for 200s with a linear ablation rate of only 5.12 x 10 -4 mm/s, has very excellent ultra-high temperature ablation resistance.
The invention is not described in detail in part as known to those skilled in the art.
Therefore, the invention adopts the Cf/(Ti, zr, hf) C entropy ceramic matrix composite material and the preparation method thereof, effectively improves the interface combination among ceramics, pyrolytic carbon and carbon fibers, relieves the erosion problem of precursors to the fibers, realizes the efficient impregnation and pyrolysis of the composite material at a lower temperature by adopting multiple rounds of different viscosities, and improves the component uniformity and bending mechanical property of the composite material.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting it, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that: the technical scheme of the invention can be modified or replaced by the same, and the modified technical scheme cannot deviate from the spirit and scope of the technical scheme of the invention.
Claims (10)
1. A preparation method of a Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite is characterized by comprising the following steps: the method comprises the following steps:
step 1: preparing a high-texture pyrolytic carbon interface phase on the surface of a composite material preform;
step 2: impregnating the composite material preform;
step 3: cross-linking and solidifying the impregnated composite material preform;
step 4: cracking the crosslinked and solidified composite material preform;
step 5: repeating the steps 2, 3 and 4 until the density of the obtained composite material preform reaches 2.5-3.5 g/cm 3 。
2. The method for preparing the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite according to claim 1, wherein: in the step 1, the fiber volume fraction of the composite material preform is 45-55%, the composite material preform is put into a chemical vapor deposition furnace, the heating rate is 3-5 ℃/min, the temperature is kept at the deposition temperature of 900-1000 ℃ for 1 hour, a methane deposition air source is introduced into the chemical vapor deposition furnace, the heating rate is 3-5 ℃/min, the temperature is kept at the deposition temperature of 900-1000 ℃ for 1 hour, and the density of 1.1-1.4g/cm is obtained 3 Is provided.
3. The method for preparing the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite according to claim 1, wherein: in the step 2, the obtained composite material preform with the high-texture pyrolytic carbon interface phase is placed in an impregnating tank, then the impregnating tank is sealed and vacuumized until the pressure in the tank is between-0.1 Mpa and-0.05 Mpa, the precursor solution is pumped in through vacuum suction, and the impregnating is performed for 1 to 2 hours under the vacuum pressure condition.
4. A method for preparing an entropy ceramic matrix composite in Cf/(Ti, zr, hf) C according to claim 3, wherein: the solute of the precursor solution comprises a precursor and a carbon source precursor, the solvent of the precursor solution is an organic solvent, and the viscosity of the precursor solution is divided into low viscosity of 100-150 mPa.s and high viscosity of 250-300 mPa.s.
5. The method for preparing the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite according to claim 4, wherein: the precursor is prepared by cohydrolytic polycondensation of propyl titanate, propyl zirconate and propyl hafnate; the carbon source precursor is one or more of phenolic resin, furfuryl ketone resin, sucrose and furan resin; the organic solvent is one or more of methanol, isopropanol, ethanol, n-propanol, isobutanol, n-butanol, ethylene glycol methyl ether and ethylene glycol ethyl ether.
6. The method for preparing the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite according to claim 1, wherein: in the step 3, after the impregnation work is completed, transferring the composite material preform subjected to vacuum impregnation and the precursor solution into a pressurized impregnation kettle, introducing inert gas into the impregnation kettle, impregnating for 1 hour under the pressure condition of 2-5 Mpa and the temperature of 100 ℃, decompressing, taking out the composite material preform, and carrying out crosslinking curing in a blast oven.
7. The method for preparing the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite according to claim 6, wherein: the inert gas is argon or nitrogen, and the flow rate of the gas is 1-1000 sccm.
8. The method for preparing the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite according to claim 1, wherein: in the step 4, the obtained crosslinked and cured composite material preform is placed in a vacuum environment or an inert atmosphere protection cracking furnace for cracking, the low-temperature cracking temperature is 1400-1500 ℃, the high-temperature cracking temperature is 1700-1800 ℃, and the heating rate is 5-20 ℃/min.
9. A Cf/(Ti, zr, hf) C entropy ceramic matrix composite prepared by the method of preparing a Cf/(Ti, zr, hf) C entropy ceramic matrix composite according to any one of claims 1-8.
10. The Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite of claim 9, wherein: the Cf/(Ti, zr, hf) C medium entropy ceramic matrix composite takes a carbon fiber preform as a framework, the volume fraction of the carbon fiber preform is 45-55%, and a high-texture pyrolytic carbon interface phase is deposited on the surface of the carbon fiber preform; the entropy ceramic in (Ti, zr, hf) C is used as a matrix, and the oxygen content in the matrix is not higher than 2%.
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