CN117658655A - SiC/PyC nanowire reinforced Al 2 O 3 High-temperature-resistant wave-absorbing ceramic and preparation method thereof - Google Patents
SiC/PyC nanowire reinforced Al 2 O 3 High-temperature-resistant wave-absorbing ceramic and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 93
- 229910018072 Al 2 O 3 Inorganic materials 0.000 title claims abstract description 42
- 239000002070 nanowire Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 35
- 238000000151 deposition Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 239000007789 gas Substances 0.000 claims description 27
- 229910052786 argon Inorganic materials 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 238000005229 chemical vapour deposition Methods 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
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- 238000000605 extraction Methods 0.000 claims description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 6
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 6
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
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- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 150000002815 nickel Chemical group 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 19
- 239000011358 absorbing material Substances 0.000 abstract description 17
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 24
- 229910010271 silicon carbide Inorganic materials 0.000 description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
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- 239000000835 fiber Substances 0.000 description 6
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- 239000011787 zinc oxide Substances 0.000 description 5
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- 238000010146 3D printing Methods 0.000 description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 3
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- 229910010293 ceramic material Inorganic materials 0.000 description 3
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- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000004246 zinc acetate Substances 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
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- 239000011259 mixed solution Substances 0.000 description 2
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- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
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- 238000004108 freeze drying Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
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- 239000000696 magnetic material Substances 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention discloses an SiC/PyC nanowire reinforced Al 2 O 3 High temperature resistant wave-absorbing ceramic made of Al 2 O 3 Porous ceramic matrix, graphene interface and SiC/PyC nanowire, and Al is adopted 2 O 3 The porous ceramic is used as a matrix, and the porous structure type wave-absorbing material is formed by depositing a graphene interface and SiC/PyC nano wires on the skeleton of the porous ceramic, so that the porous ceramic has the characteristics of light weight and high strength, can be stably used in a high-temperature environment, realizes the characteristic application of high-temperature wave absorption, optimizes the electromagnetic parameters of the composite material due to the introduction of the graphene interface and the SiC/PyC nano wires, and can obtain better impedance matching and attenuation coefficient, thereby obtaining excellent wave-absorbing performance. In addition, al is used 2 O 3 Porous ceramics provide a porous structure by chemical vapor phaseThe deposition method introduces a graphene interface and SiC/PyC nanowires, has strong interface binding force and high chemical purity, has better repeatability of the preparation process, and can provide a new idea for the mass production of the three-dimensional structure composite wave-absorbing material.
Description
Technical Field
The invention relates to a wave-absorbing ceramic, in particular to a ceramicSiC/PyC nanowire reinforced Al 2 O 3 The high-temperature resistant wave-absorbing ceramic can be applied to long-time service in a high-temperature complex environment.
Technical Field
Wave absorbing materials are materials that absorb and attenuate incident electromagnetic wave energy, converting the electromagnetic energy into thermal energy or other forms of energy, and dissipating the energy, thereby reducing electromagnetic wave reflection or transmission. Most magnetic materials are limited by curie temperature and can only provide stable wave-absorbing properties at lower temperatures. When the ambient temperature rises to a certain extent, the magnetic loss function disappears. Therefore, dielectric loss type wave-absorbing materials are necessary choices for high temperature wave-absorbing materials. The wave-absorbing materials can be divided into two categories of coating type wave-absorbing materials and structural wave-absorbing materials according to the forming process and bearing capacity of the wave-absorbing materials. The structural wave-absorbing material has the dual functions of bearing and reducing radar scattering cross section, has the advantages of light weight and high strength of the composite material, but the traditional structural wave-absorbing material is mostly prepared by combining a foaming method and a freeze drying method, the former has higher requirements on raw materials, the process conditions are not easy to control, the foaming degree is difficult to ensure in mass production, the repeatability is poor, and the latter can prepare the porous material with a complex structure, but the high production cost limits the wide popularization of the porous material. Meanwhile, the research and application of the high-temperature wave-absorbing ceramic are less at present, and the ceramic still belongs to the starting stage.
The Chinese patent application No. 201710951568.5 discloses a wave-absorbing ceramic and a preparation method thereof, comprising the following contents: (1) Taking a mixed solution of zinc acetate, an aluminum compound, an alcohol amine compound and a benign solvent, wherein the molar concentration of the zinc acetate in the mixed solution is 0.1-1 mol/L, the molar ratio of the zinc acetate to the alcohol amine compound is 1:1, the molar ratio of Al to Zn is 0.01-0.02:1, stirring and standing to obtain a precursor; (2) Soaking porous alumina ceramic in the precursor to obtain a prefabricated body, and performing heat treatment to obtain soaked ceramic; (3) Dipping the dipped ceramic in a precursor, and then carrying out heat treatment; repeating the steps to obtain the impregnated ceramic with the zinc oxide content of 7.0-11.5 wt%; (4) Heating, and performing heat treatment under protective atmosphere to obtain the wave-absorbing ceramic material.The invention adopts wet chemical method to synthesize ZnO, can greatly reduce the particle size and crystallization temperature of ZnO product, and can obtain ZnO/Al 2 O 3 ZnO in the complex phase ceramic is uniformly distributed, which is beneficial to improving the wave absorbing performance of the material.
The Chinese patent application No. 202010495060.0 discloses a porous alumina-based composite wave-absorbing material and a preparation method thereof, wherein the porous alumina-based composite wave-absorbing material comprises a porous alumina matrix and transition metal phosphide thereon, and the preparation method comprises the following steps: pretreating a porous alumina matrix; adding transition metal salt, ammonium fluoride and urea into deionized water, and magnetically stirring until the transition metal salt, ammonium fluoride and urea are uniformly mixed to obtain a precursor solution; immersing the porous alumina matrix in the precursor solution, maintaining the pressure in vacuum, heating again for loading, and phosphating the loaded product. The porous alumina ceramic can meet the light weight requirement of the wave absorbing material, and after being compounded with transition metal phosphide, the porous alumina ceramic can regulate electromagnetic parameters, raise impedance matching performance, make electromagnetic wave produce multiple reflection and scattering when the electromagnetic wave is incident, and increase the propagation path of the electromagnetic wave in the wave absorbing material, so as to reach the function of enhancing wave absorbing performance.
The Chinese patent application No. 201710693281.7 discloses a preparation method of a special-shaped negative-curvature composite ceramic wave-transmitting radome based on winding forming, which comprises the steps of core mold preparation, silica gel solution preparation, fiber winding, shaping of prefabricated blank, curing of a radome blank, dipping compounding of the radome blank, sintering forming and processing. The invention has the advantages that: (1) The silicon dioxide matrix material is introduced in the process of braiding and forming the fiber fabric, so that the performance of the quartz composite ceramic material can be designed and adjusted by designing and adjusting the structure trend, the fiber volume content, the composite material density, the porosity and other structures and parameters of the fiber fabric, the production efficiency is high, the period is short, and the cost is low; (2) The shaping step of the prefabricated blank can adopt the cylindrical rod to roll the positive curvature convex surface to be attached to the negative curvature concave surface of the shaping core mold through the shaping core mold with the negative curvature concave surface and the winding core mold with the positive curvature convex surface, so that the shaping core mold can be suitable for preparing a radome body product with a negative curvature abnormal structure, the problem that fabrics with 2.5D structures cannot be subjected to negative curvature braiding is effectively solved, and the defect that wrinkles are very easy to generate when braiding the abnormal structure is avoided; (3) The silicon dioxide matrix can be introduced in advance when the fiber fabric is wound and woven, so that the densification speed of the composite ceramic is improved, and the production efficiency is improved; (4) The material performance can be designed and adjusted according to the performance requirements of the radome product, for example, the strength of the composite ceramic in each direction can be adjusted by adjusting the trend of winding fiber, winding tension and the like, and the dielectric performance of the material can be adjusted by adjusting the density of the product, the heat treatment temperature and the like.
The invention patent of China with application number 202010893483.8 discloses a graphene ceramic composite material prepared based on 3D printing and a preparation method thereof, and belongs to the field of ceramic composite material preparation. The graphene ceramic composite material is prepared from Al 2 O 3 The SiC particles and the graphene are prepared from three raw materials. The preparation process mainly comprises the following steps: ball milling and mixing, preparing slurry, 3D printing, drying and microwave sintering. The invention has the main advantages that: after sintering, alumina and silicon carbide form a nano ceramic composite material by adopting a method combining a 3D printing technology and microwave pressurizing sintering, and the graphene modifies silicon carbide alumina ceramic, so that the prepared composite material has good fracture toughness, electric conduction, thermal conductivity and the like. The ceramic composite material prepared by the method has simple process and strong universality, realizes the die-free additive manufacturing of the ceramic composite material, greatly reduces the production cost and has good economic benefit.
As shown in the above patent, a wave-absorbing ceramic material is disclosed, but the integral molding preparation and the application of the wave-absorbing ceramic in high temperature environment are less introduced, and the further application of the high temperature wave-absorbing ceramic is limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high-temperature-resistant wave-absorbing ceramic integrating light weight, high strength, high temperature resistance and wave absorption.
The technical scheme adopted for realizing the purposes of the patent of the invention is as follows: siC/PyC nanowire reinforced Al 2 O 3 High temperature resistant wave-absorbing ceramic made of Al 2 O 3 The porous ceramic matrix, the graphene interface and the SiC/PyC nanowire are characterized in that the porous ceramic matrix is made of Al 2 O 3 The porous ceramic matrix is of an open-pore continuous structure, and the volume density is 3.2-4.0 g/cm 3 The average pore diameter is 5-20 mu m, and the porosity is 90-95%; the graphene interface is formed on Al through a vacuum chemical vapor deposition method 2 O 3 The porous ceramic matrix skeleton surface is prepared, the reaction source gases are methane, hydrogen and argon, the gas flow ratio is 40-60:80-120:750-850 sccm, the deposition time is 1-2 h, the graphene interface thickness is 5-10 nm, and the porous ceramic matrix skeleton surface is of a discontinuous structure; siC/PyC nano wire is prepared on Al by chemical vapor infiltration method 2 O 3 The porous ceramic matrix is prepared by pores, reaction source gases are trichloromethylsilane, hydrogen and argon, the gas flow ratio is 5-10:50-100:50-100 sccm, the deposition time is 4-8 h, and the SiC nanowire is arranged on Al 2 O 3 A discontinuous bridging structure is formed in the pores of the porous ceramic matrix, the diameter is 20-50 nm, the PyC coating is uniformly coated on the surface of the SiC nanowire to form a core-shell structure, the reaction source gas is propylene and argon, the gas flow ratio is 50-100:150-250 sccm, the deposition time is 4-8 h, and the thickness of the PyC coating is 5-10 nm.
Further, the SiC/PyC nanowire enhances Al 2 O 3 The preparation method of the high-temperature-resistant wave-absorbing ceramic is characterized by comprising the following steps of:
(1) First for Al 2 O 3 Pretreating porous foam, soaking in high-purity alcohol for 2-4 h, cleaning with cleaning agent, and drying to obtain Al 2 O 3 A porous ceramic matrix;
(2) Al is added with 2 O 3 Placing the porous ceramic matrix into a chemical vapor deposition furnace, performing vacuum pumping treatment, wherein the vacuum degree is 0.1-1 Pa, then introducing methane, hydrogen and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with the furnace to obtain Al with a graphene deposited interface on the surface 2 O 3 A porous ceramic matrix;
(3) Al in (2) 2 O 3 Placing the porous ceramic matrix into nickel nitrate solution with the concentration of 0.1-1 mol/L and the soaking time of 2-4 h, and then adding Al 2 O 3 Drying the porous ceramic matrix in a muffle furnace at 60-80 deg.c for 1-2 hr, and cooling to obtain nickel atom loaded graphene/Al 2 O 3 A porous ceramic matrix;
(4) graphene/Al in (3) 2 O 3 Placing a porous ceramic matrix into chemical vapor deposition, performing air extraction treatment, wherein the vacuum degree is 1-10 Pa, then introducing trichloromethylsilane, hydrogen and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with a furnace to obtain the SiC nanowire reinforced graphene/Al 2 O 3 A porous ceramic matrix;
(5) graphene/Al with SiC nanowire enhancement in (4) 2 O 3 Placing the porous ceramic matrix into chemical vapor deposition and performing air extraction treatment, wherein the vacuum degree is 1-10 Pa, then introducing propylene and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with a furnace to obtain SiC/PyC nanowire reinforced Al 2 O 3 High temperature resistant wave absorbing ceramic.
The beneficial effects of the invention are as follows: (1) the invention adopts Al 2 O 3 The porous ceramic is used as a matrix, and a porous structure type wave-absorbing material is formed by depositing a graphene interface and SiC/PyC nanowires on a skeleton of the porous ceramic, so that the porous ceramic has the characteristics of light weight and high strength, and the electromagnetic parameters of the composite material are optimized by introducing the discontinuous graphene interface and the SiC/PyC nanowires, so that good impedance matching and attenuation coefficients are obtained, and excellent wave-absorbing performance is obtained; (2) the invention uses Al 2 O 3 The porous ceramic provides a porous structure, a graphene interface and a SiC/PyC nanowire are introduced by a chemical vapor deposition method, so that the interface binding force is strong, the chemical purity is high, the repeatability of the preparation process is good, and a new thought can be provided for the large-scale production of the three-dimensional structure composite wave-absorbing material; (3) the invention adopts Al 2 O 3 The porous ceramic is taken as a matrix, a graphene interface and SiC/PyC nanowire are deposited to modify and strengthen the porous ceramic, and the SiC nanowire is arranged on Al 2 O 3 Non-porous ceramic matrix formed in poresThe continuous bridge connection structure forms an aerogel network, can be stably in service in a high-temperature environment, and realizes the characteristic application of high-temperature wave absorption.
Detailed Description
The present invention is further illustrated below in conjunction with specific embodiments, it being understood that these embodiments are meant to be illustrative of the invention only and not limiting the scope of the invention, and that modifications of the invention, which are equivalent to those skilled in the art to which the invention pertains, will fall within the claims appended hereto.
Example 1
SiC/PyC nanowire reinforced Al 2 O 3 High temperature resistant wave-absorbing ceramic made of Al 2 O 3 The porous ceramic matrix, the graphene interface and the SiC/PyC nanowire are characterized in that the porous ceramic matrix is made of Al 2 O 3 The porous ceramic matrix is of an open-cell continuous structure, and has a volume density of 3.5g/cm 3 The average pore diameter is 10 mu m, and the porosity is 95%; the graphene interface is formed on Al through a vacuum chemical vapor deposition method 2 O 3 The porous ceramic matrix skeleton surface is prepared, the reaction source gases are methane, hydrogen and argon, the gas flow ratio is 40:90:800sccm, the deposition time is 1.5h, the graphene interface thickness is 8nm, and the porous ceramic matrix skeleton surface is of a discontinuous structure; siC/PyC nano wire is prepared on Al by chemical vapor infiltration method 2 O 3 The porous ceramic matrix is prepared by pores, reaction source gases are trichloromethylsilane, hydrogen and argon, the gas flow ratio is 8:60:80sccm, the deposition time is 6h, and the SiC nanowire is arranged on Al 2 O 3 A discontinuous bridging structure is formed in the pores of the porous ceramic matrix, the diameter is 30nm, the PyC coating is uniformly coated on the surface of the SiC nanowire to form a core-shell structure, the reaction source gas is propylene and argon, the gas flow ratio is 60:200sccm, the deposition time is 6h, and the thickness of the PyC coating is 8nm.
Further, the SiC/PyC nanowire enhances Al 2 O 3 The preparation method of the high-temperature-resistant wave-absorbing ceramic comprises the following steps:
(1) First for Al 2 O 3 The porous foam is pretreated, high-purity alcohol is adopted for soaking treatment for 3 hours, then a cleaning agent is adopted for cleaning,drying to obtain Al 2 O 3 A porous ceramic matrix;
(2) Al is added with 2 O 3 Placing the porous ceramic matrix into a chemical vapor deposition furnace, performing vacuum pumping treatment, wherein the vacuum degree is 0.5Pa, then introducing methane, hydrogen and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with the furnace to obtain Al with a graphene deposited interface on the surface 2 O 3 A porous ceramic matrix;
(3) Al in (2) 2 O 3 Placing the porous ceramic matrix into nickel nitrate solution with concentration of 0.5mol/L and soaking time of 3h, and then adding Al 2 O 3 Drying the porous ceramic matrix in a muffle furnace at 70deg.C for 1.5 hr, and cooling with furnace to obtain graphene/Al with nickel atoms loaded on the surface 2 O 3 A porous ceramic matrix;
(4) graphene/Al in (3) 2 O 3 Placing a porous ceramic matrix into chemical vapor deposition, performing air extraction treatment, wherein the vacuum degree is 5Pa, then introducing trichlorosilane, hydrogen and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with a furnace to obtain the SiC nanowire reinforced graphene/Al 2 O 3 A porous ceramic matrix;
(5) graphene/Al with SiC nanowire enhancement in (4) 2 O 3 Placing the porous ceramic matrix into chemical vapor deposition, performing air extraction treatment, vacuum degree is 5Pa, then introducing propylene and argon, adjusting gas flow ratio, setting reaction time, and cooling along with furnace to obtain SiC/PyC nanowire reinforced Al 2 O 3 High temperature resistant wave absorbing ceramic.
The foregoing is merely one specific embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modification of the present invention by using the concept shall fall within the scope of the present invention. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention will still fall within the protection scope of the technical solution of the present invention.
Claims (2)
1. SiC/PyC nanowire reinforced Al 2 O 3 High temperature resistant wave-absorbing ceramic made of Al 2 O 3 The porous ceramic matrix, the graphene interface and the SiC/PyC nanowire are characterized in that the porous ceramic matrix is made of Al 2 O 3 The porous ceramic matrix is of an open-pore continuous structure, and the volume density is 3.2-4.0 g/cm 3 The average pore diameter is 5-20 mu m, and the porosity is 90-95%; the graphene interface is formed on Al through a vacuum chemical vapor deposition method 2 O 3 The porous ceramic matrix skeleton surface is prepared, the reaction source gases are methane, hydrogen and argon, the gas flow ratio is 40-60:80-120:750-850 sccm, the deposition time is 1-2 h, the graphene interface thickness is 5-10 nm, and the porous ceramic matrix skeleton surface is of a discontinuous structure; siC/PyC nano wire is prepared on Al by chemical vapor infiltration method 2 O 3 The porous ceramic matrix is prepared by pores, reaction source gases are trichloromethylsilane, hydrogen and argon, the gas flow ratio is 5-10:50-100:50-100 sccm, the deposition time is 4-8 h, and the SiC nanowire is arranged on Al 2 O 3 A discontinuous bridging structure is formed in the pores of the porous ceramic matrix, the diameter is 20-50 nm, the PyC coating is uniformly coated on the surface of the SiC nanowire to form a core-shell structure, the reaction source gas is propylene and argon, the gas flow ratio is 50-100:150-250 sccm, the deposition time is 4-8 h, and the thickness of the PyC coating is 5-10 nm.
2. A SiC/PyC nanowire reinforced Al of claim 1 2 O 3 The preparation method of the high-temperature-resistant wave-absorbing ceramic is characterized by comprising the following steps of:
(1) First for Al 2 O 3 Pretreating porous foam, soaking in high-purity alcohol for 2-4 h, cleaning with cleaning agent, and drying to obtain Al 2 O 3 A porous ceramic matrix;
(2) Al is added with 2 O 3 Placing the porous ceramic matrix into a chemical vapor deposition furnace, performing vacuum pumping treatment, wherein the vacuum degree is 0.1-1 Pa, then introducing methane, hydrogen and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with the furnace to obtain the surface deposited grapheneAl of interface 2 O 3 A porous ceramic matrix;
(3) Al in (2) 2 O 3 Placing the porous ceramic matrix into nickel nitrate solution with the concentration of 0.1-1 mol/L and the soaking time of 2-4 h, and then adding Al 2 O 3 Drying the porous ceramic matrix in a muffle furnace at 60-80 deg.c for 1-2 hr, and cooling to obtain nickel atom loaded graphene/Al 2 O 3 A porous ceramic matrix;
(4) graphene/Al in (3) 2 O 3 Placing a porous ceramic matrix into chemical vapor deposition, performing air extraction treatment, wherein the vacuum degree is 1-10 Pa, then introducing trichloromethylsilane, hydrogen and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with a furnace to obtain the SiC nanowire reinforced graphene/Al 2 O 3 A porous ceramic matrix;
(5) graphene/Al with SiC nanowire enhancement in (4) 2 O 3 Placing the porous ceramic matrix into chemical vapor deposition and performing air extraction treatment, wherein the vacuum degree is 1-10 Pa, then introducing propylene and argon, adjusting the gas flow ratio, setting the reaction time, and cooling along with a furnace to obtain SiC/PyC nanowire reinforced Al 2 O 3 High temperature resistant wave absorbing ceramic.
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