CN116639996A - Wave-absorbing Si-C-N complex phase ceramic with bidirectional periodic pore structure and preparation method thereof - Google Patents
Wave-absorbing Si-C-N complex phase ceramic with bidirectional periodic pore structure and preparation method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 135
- 230000000737 periodic effect Effects 0.000 title claims abstract description 36
- 239000011148 porous material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000002457 bidirectional effect Effects 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 23
- 238000000151 deposition Methods 0.000 claims abstract description 20
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 19
- 239000004917 carbon fiber Substances 0.000 claims abstract description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 claims abstract description 15
- 239000004744 fabric Substances 0.000 claims abstract description 8
- 230000008595 infiltration Effects 0.000 claims abstract description 5
- 238000001764 infiltration Methods 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims description 11
- 230000003647 oxidation Effects 0.000 claims description 11
- 238000007254 oxidation reaction Methods 0.000 claims description 11
- 230000003064 anti-oxidating effect Effects 0.000 claims description 7
- 238000009941 weaving Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 28
- 238000010521 absorption reaction Methods 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 3
- 238000009940 knitting Methods 0.000 abstract 1
- 239000011241 protective layer Substances 0.000 abstract 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 83
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 81
- 230000008021 deposition Effects 0.000 description 14
- 229910052581 Si3N4 Inorganic materials 0.000 description 9
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000004321 preservation Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000011358 absorbing material Substances 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 229910021417 amorphous silicon Inorganic materials 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000011153 ceramic matrix composite Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 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
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
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- 230000001788 irregular Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of wave-absorbing Si-C-N complex phase ceramic with a bidirectional periodic pore structure, which comprises the steps of firstly adopting a chemical vapor infiltration method to deposit Si with a certain thickness on carbon fiber cloth with a two-dimensional woven structure in situ 3 N 4 Ceramics, obtain C f /Si 3 N 4 A composite material; then the material is oxidized to obtain Si with nearly hollow tubular knitting structure 3 N 4 (C) A porous ceramic; then sequentially depositing SiC nano interface layers as electromagnetic wave loss layers and Si 3 N 4 Ceramic as antioxidantThe protective layer and the impedance matching layer are used for oxidizing and decarbonizing residual carbon fiber to obtain Si with a bidirectional periodic pore structure 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramics. Si prepared by the invention 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 The complex phase ceramic has a bidirectional periodic pore structure, a large number of wave-transmitting/wave-absorbing nano heterogeneous interfaces and defects, when the thickness is only 2.45mm, the average effective absorption efficiency of the complex phase ceramic in an X wave band exceeds-10 dB, the strongest absorption reaches-24.5 dB, and the preparation process is simple, the thermal stability of the material is good, the operability is strong, and the preparation of the room/high temperature cooperative wave-absorbing complex phase ceramic is facilitated.
Description
Technical Field
The invention relates to the technical field of high-temperature wave-absorbing complex-phase ceramic preparation, in particular to wave-absorbing Si-C-N complex-phase ceramic with a bidirectional periodic pore structure and a preparation method thereof.
Background
Aiming at the urgent demands of the invisible tail spray component of the aeroengine on high-temperature resistant, oxidation resistant and broadband wave-absorbing materials, the Si-C-N complex phase ceramic not only can meet the demands, but also has the advantages of easy design, light weight, processability and the like, and becomes an important matrix material of the high-temperature bearing wave-absorbing integrated ceramic matrix composite material; the preparation process of the Si-C-N composite ceramic commonly used for the Si-C-N composite ceramic comprises a polymer conversion ceramic method and a chemical vapor deposition/chemical vapor infiltration method, wherein the polymer conversion ceramic has insufficient high-temperature stability and lower mechanical property, and the Si-C-N ceramic prepared by the chemical vapor deposition method can effectively solve the problems and has important research significance for preparing the carrier wave-absorbing integrated ceramic matrix composite material. The subject group adopts SiCl 4 -NH 3 -C 3 H 6 -H 2 Ar' system, si-C-N ceramic is prepared by regulating deposition temperature, gas flow and other parameters, and the obtained Si-C-N ceramic contains SiC (C) -Si 3 N 4 The Si-C-N ceramic has a low degree of crystallization at a preparation temperature (800 to 1000 ℃ C.), and is insufficient in electromagnetic wave absorption capacity. The Si-C-N ceramic is heat treated in Ar atmosphere at 1200-1500 ℃ and then good electromagnetic wave absorption performance can be obtained in the X wave band; but the above SiC (C) -Si 3 N 4 The co-deposited Si-C-N ceramic has great difficulty in regulating and controlling the parameters of the preparation process, and the phase components and the multi-scale structure of the Si-C-N ceramic are difficult to effectively regulate and control at a lower preparation temperature, so that a wider effective absorption frequency band is realized; therefore, a broadband wave-absorbing is exploredThe low-temperature preparation method of the Si-C-N complex phase ceramic has important research value.
The literature "J.M.Xue, X.W.Yin, et al, induced crystallization behavior EMW absorption properties of CVI Si-C-N ceramics modified with carbon nanowires [ J ]. Chem.Eng.J.), 378 (2019) 122213-122222," proposed to modify CVI Si-C-N ceramics with carbon nanowires to optimize the electromagnetic wave absorption performance at room temperature, and the content and uniformity of the carbon nanowires are difficult to control due to the fact that the carbon nanowires are prepared prior to CVI SiCN, and the Si-C-N ceramics have limited electromagnetic wave absorption performance, so that the basic requirements of "thin, light, wide and strong" are difficult to meet.
The invention patent with the publication number of CN107188596A discloses a preparation method of porous gradient silicon nitride-silicon carbide wave-absorbing complex phase, which takes diatomite and phenolic resin as raw materials to prepare diatomite blanks, and the gradual partial pressure is generated due to the consumption of nitrogen when the blanks are sintered, so that continuous gradient silicon carbide is formed in porous silicon nitride-silicon carbide ceramics; the method effectively reduces the reflection of the material surface to electromagnetic waves and improves the electromagnetic wave absorbing performance, but the material has lower dielectric constant due to the too high porosity, and the matching thickness of the material is larger.
In conclusion, the existing Si-C-N complex-phase ceramic has the problems of complex preparation process, difficult regulation and control of a multi-scale structure, difficult cooperation of high-temperature wave absorption of a room and the like, and limits the application of the Si-C-N complex-phase ceramic in the stealth tail spray part of the aeroengine. Therefore, the method for preparing the wave-absorbing Si-C-N complex phase ceramic with the periodic pore structure has important academic research and application demand value.
Disclosure of Invention
Aiming at the problems, the invention aims to develop a composite material with light weight, high temperature resistance, wide frequency band and strong absorption, and provides a preparation method of wave-absorbing Si-C-N complex phase ceramic with a bidirectional periodic pore structure, wherein a two-dimensional woven structure carbon fiber cloth is adopted to provide a bidirectional periodic pore structure skeleton, and SiC and Si are alternately deposited 3 N 4 Ceramic and method for multiple oxidation, in-situ construction of Si with bidirectional pore structure 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramic; the aim of the invention is mainly achieved by the following scheme:
the preparation method of the wave-absorbing Si-C-N complex phase ceramic with the bidirectional periodic pore structure is characterized by comprising the following steps of:
s1: preparation of Si 3 N 4 (C) A porous ceramic;
s2: using Si prepared in step S1 3 N 4 (C) Preparation of Si from porous ceramics 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Complex phase ceramic;
s3: using Si prepared in step S2 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Preparation of Si by Complex phase ceramic 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramics, i.e. Si-C-N complex phase ceramics.
Further, the specific operation of step S1 includes the following steps:
s11: adopting a chemical vapor infiltration method to deposit Si with the diameter of 1-2 mu m on the carbon fiber cloth with the two-dimensional weaving structure in situ 3 N 4 Ceramic matrix, obtain C f /Si 3 N 4 A composite material;
s12: at 600-700 deg.C for C f /Si 3 N 4 The composite material is oxidized and kept for 1 to 5 hours to obtain Si with a bidirectional periodic pore structure 3 N 4 (C) Porous ceramics.
Further, the specific operation of step S2 includes the following steps:
s21: si obtained in step S1 3 N 4 (C) Depositing 90-200 nm SiC interface layer on the porous ceramic in situ to obtain SiC/(Si) 3 N 4 (C) A) SiC complex phase ceramic;
s22: in SiC/(Si) 3 N 4 (C) 300-400 nm Si is deposited on the SiC complex phase ceramics in situ 3 N 4 An antioxidation layer to obtain Si 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Complex phase ceramics.
Further, the specific operation in step S3 is as follows:
for Si prepared in step S2 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Oxidizing the complex phase ceramic again, and maintaining the temperature at 600-700 ℃ for at least 8h to obtain the layered Si with the bidirectional periodic pore structure 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramics.
Further, the wave-absorbing Si-C-N complex phase ceramic with the bidirectional periodic pore structure is prepared by the preparation method.
Further, the Si-C-N complex phase ceramic comprises Si 3 N 4 Ceramic matrix, intermediate SiC interface layer and outer Si layer 3 N 4 An oxidation resistant layer.
Further, the Si is 3 N 4 The thickness of the ceramic matrix is about 1-2 mu m, the thickness of the SiC interface layer is about 90-200 nm, si 3 N 4 The thickness of the antioxidation layer is about 300-400 nm.
Further, the Si is 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 The volume density of the complex phase ceramic is 1.3-1.6 g/cm 3 The porosity is 73-77%.
Compared with the prior art, the invention has the beneficial effects that:
1. the porous wave-absorbing complex-phase ceramic prepared by the method is mainly polarization loss, has low density, wide absorption frequency band and stable high-temperature wave-absorbing performance, is a high-temperature wave-absorbing material with potential, and effectively solves the problems of high density, large thickness, insufficient wave-absorbing performance and the like of the existing high-temperature wave-absorbing ceramic;
2. the invention has simple process flow, a large number of periodic pore structures, defects, cracks and wave-transmitting/absorbing heterogeneous interfaces exist in the complex-phase ceramic, and the thickness and the distribution of the SiC layer in the complex-phase ceramic can be regulated and controlled; by forming Si with bi-directional periodic hole structure 3 N 4 (C) In ceramicsAlternate deposition of SiC and Si 3 N 4 A large number of wave-transmitting/absorbing heterogeneous interfaces are constructed in situ, so that the loss of the material to electromagnetic waves is effectively increased; by reacting Si with 3 N 4 (C) The oxidation degree (heat preservation time) of the ceramic regulates and controls the holes (transmission channels of CVI SiC gas phase precursors to the inside) in the ceramic, changes the size of a gas phase deposition diffusion channel in the CVI process, and realizes the control of the deposition content and thickness of a SiC interface layer, thereby optimizing a bidirectional periodic pore structure and a wave-transmitting/absorbing heterogeneous interface, and finally preparing Si 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 The dielectric property of the complex phase ceramic is adjustable, the wave absorbing property is excellent, and when the thickness is 2.45mm, the complex phase ceramic can almost realize effective absorption of X wave band;
3. adopting a two-dimensional woven structure carbon fiber cloth as a template to deposit Si 3 N 4 Preparation C f /Si 3 N 4 The composite material is oxidized to remove carbon fiber to form the bidirectional periodic pore structure Si 3 N 4 (C) The ceramic solves the problem of randomness of pores in the ceramic, and the prepared Si 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 The bi-directional periodic pore structure, defects, cracks, wave-transmitting/wave-absorbing nano heterogeneous interfaces and the like exist in the complex-phase ceramic, so that the polarization loss capacity of the complex-phase ceramic is effectively improved; the laminated forming of the two-dimensional woven structure carbon fiber cloth provides a bidirectional periodic pore structure for the complex phase ceramic, reduces the density of the homogeneous wave-absorbing ceramic, improves the wave-absorbing performance of the homogeneous wave-absorbing ceramic, and provides a new idea for preparing the thin, light, wide and strong electromagnetic wave-absorbing material.
Drawings
FIG. 1 is a process flow diagram of a Si-C-N complex phase ceramic;
FIG. 2 is a photograph of a cross-sectional microstructure of a Si-C-N complex phase ceramic in example 2;
FIG. 3 is a graph of complex permittivity versus frequency for a Si-C-N complex phase ceramic;
FIG. 4 is a graph showing the reflection coefficient of Si-C-N complex phase ceramics as a function of frequency.
Detailed Description
In order to enable those skilled in the art to better understand the technical solution of the present invention, the technical solution of the present invention is further described below with reference to the accompanying drawings and examples.
Example 1:
as shown in fig. 1, a method for preparing wave-absorbing Si-C-N complex phase ceramic having a bi-directional periodic pore structure, comprising the steps of,
s1: preparation of Si 3 N 4 (C) A porous ceramic;
specifically, S11: adopting a Chemical Vapor Infiltration (CVI) method to deposit amorphous Si on the carbon fiber cloth with a two-dimensional braided structure in situ 3 N 4 Ceramic matrix, i.e. two-dimensional woven carbon fiber (C f ) The cloth is subjected to lamination needling fixation, horizontally clamped by a graphite die and tightly screwed and fixed by four sides of a carbon bolt, so that a uniform and flat carbon fiber preform with the thickness of 3-5 mm is obtained; the preform is then placed in Si 3 N 4 The central position of the constant temperature zone of the deposition furnace adopts a CVI method, a gaseous precursor (ammonia gas is a nitrogen source, silicon tetrachloride is a silicon source, argon is a protective atmosphere, and hydrogen is a diluent gas) enters the reaction deposition furnace according to a certain proportion, and is mainly infiltrated into a porous fiber preform through diffusion, and the chemical reaction equation of in-situ deposition is as follows:
wherein, deposition temperature: 800-1000 ℃ and the heat preservation time is as follows: 100h, deposition pressure: 5000Pa, in situ deposition of amorphous Si on carbon fiber preform 3 N 4 Depositing the ceramic matrix (multilayer) five times to obtain C with thickness of about 1-2 μm f /Si 3 N 4 A composite material;
s12: at 650 ℃ for C f /Si 3 N 4 The composite material is subjected to oxidation treatment, namely C f /Si 3 N 4 Placing the composite material sample in a tubular furnace, and fully contacting air for heat preservation treatment for 1h to obtain Si with a tubular-like braided structure 3 N 4 (C) Porous ceramics.
S2: preparation of Si 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Complex phase ceramic;
specifically, S21: si obtained in step S1 3 N 4 (C) Depositing 90-200 nm SiC interface layer (single layer) on the porous ceramic in situ; namely Si with bidirectional periodic pore structure prepared in the step S1 3 N 4 (C) The porous ceramic is arranged at the central position of the constant temperature area of the phi 500SiC deposition furnace, and a CVI method is adopted, and a gaseous precursor (CH 3 SiCl 3 (MTS) is a carbon source, MTS is a reaction gas for chemical vapor deposition, hydrogen is taken as a diluent gas) enters a reaction deposition furnace according to a certain ratio, reactants exist in a gas form in the CVI process, can permeate into the porous ceramic and chemically react to generate a SiC interface layer, and the reaction equation is shown as follows, wherein the thickness of the SiC interface layer is about 90-200 nm after being deposited in a furnace.
To obtain SiC/Si 3 N 4 (C) The thickness of the SiC interface layer of the SiC complex phase ceramic is about 95nm;
s22: in SiC/(Si) 3 N 4 (C) In situ deposition of amorphous Si on a composite SiC ceramic 3 N 4 Depositing a ceramic antioxidation matching layer (single layer) for a furnace time with the thickness of about 300-400 nm to obtain Si 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Complex phase ceramics.
S3: preparation of Si 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramics.
Specifically, for Si prepared in step S2 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Oxidizing the composite ceramic again at 700 deg.c for 8 hr to eliminate residual carbon fiber to obtain layered ceramic with bi-directional periodic pore structureSi 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramic; the bulk density of the ceramic is about 1.29g/cm 3 The porosity was about 77.0%.
Example 2:
the difference from embodiment 1 is that for C in step S12 of this embodiment f /Si 3 N 4 When the composite material is subjected to oxidation treatment, the heat preservation time is 3 hours, and other operation methods and parameters are the same as those in the embodiment 1; the thickness of the SiC interface layer is about 105nm, and finally the Si is prepared 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 The bulk density of the composite ceramic is about 1.45g/cm 3 The porosity was about 75.6%.
Example 3
The difference from embodiment 2 is that for C in step S12 of this embodiment f /Si 3 N 4 When the composite material is subjected to oxidation treatment, the heat preservation time is 5 hours, and other operation methods and parameters are the same as those in the embodiment 2; the carbon fiber is nearly fully oxidized, the deposited SiC content is excessive, the thickness of the SiC interface layer reaches 181nm, and the volume density of the finally prepared Si-C-N complex phase ceramic is about 1.61g/cm 3 The porosity was about 73.7%.
FIG. 2 is a photograph of a cross-sectional microstructure of the Si-C-N composite ceramic of example 2. As can be seen from FIG. 2, two scale voids exist in the composite ceramic, and the periodic pore structure greatly optimizes the impedance matching. FIG. 2 (a) is Si 3 N 4 (C) The back scattering spectrum of the porous ceramic shows that the outer layer is bright and the thickness of the silicon nitride substrate is about 1-2 mu m, and the inside is irregular carbon fiber after oxidation treatment; FIG. 2 (b) is SiC/Si 3 N 4 (C) The SiC composite ceramic shows that the interface layers between the silicon nitride substrate and the carbon fiber and the silicon nitride substrate are SiC, the thickness of the SiC composite ceramic is about 100-150 nm, and the SiC composite ceramic is a thin nano interface layer and is also an electromagnetic wave absorption phase (loss layer); FIG. 2 (c) is Si 3 N 4 /SiC/Si 3 N 4 /SiC/Si 3 N 4 Complex phase ceramics, slaveIt can be seen that the silicon nitride matching layer is uniformly distributed in the outer surface layer and the periodic holes, and the thickness of the silicon nitride matching layer is about 300-400 nm. Observation shows that SiC and Si with good uniformity are alternately deposited in porous ceramics with periodic pore structures 3 N 4 The nano layer, which builds a wave-transparent/wave-absorbing double hetero interface system, will increase electromagnetic attenuation, and at the same time, the silicon nitride antioxidation layer and the silicon nitride matrix effectively separate the conductive phase silicon carbide.
FIG. 3 is a graph showing the complex permittivity of Si-C-N complex phase ceramics with frequency (C1, C2 and C3 are Si in example 1, example 2 and example 3, respectively 3 N 4 /SiC/Si 3 N 4 /SiC/Si 3 N 4 Complex phase ceramics); as can be seen from C1 in fig. 3, since the carbon fiber oxidation is insufficient in example 1, the voids between the carbon fiber and the silicon nitride matrix are too small, resulting in too low a deposited SiC content, essentially a low absorber content, resulting in lower real (epsilon ') and imaginary (epsilon ") parts of the dielectric constants (fig. 3 (a) and fig. 3 (b) are graphs of epsilon', epsilon" versus frequency, respectively);
FIG. 4 is a graph showing the relationship between the reflection coefficient of Si-C-N complex phase ceramics and the frequency (C1, C2 and C3 are Si in example 1, example 2 and example 3, respectively) 3 N 4 /SiC/Si 3 N 4 /SiC/Si 3 N 4 Complex-phase ceramic), as can be seen from C1 in FIG. 4, si in example 1 is not easily absorbed due to low dielectric loss of example 1 and difficulty in achieving effective absorption at low thickness 3 N 4 /SiC/Si 3 N 4 /SiC/Si 3 N 4 Complex phase ceramics have unsatisfactory electromagnetic properties;
when the oxidation degree of the carbon fiber is moderate, as shown by C2 in FIG. 3, the content of the deposited SiC in the embodiment 2 is moderate, the thickness of the SiC interface layer is about 105nm, the average value of the real part of the dielectric constant is greatly increased from 4.18 to 9.25, the average value of the real part of the dielectric constant is nearly doubled, the obvious dispersion phenomenon is shown, the average value of the imaginary part of the dielectric constant is doubled, the average value of the dielectric constant is increased from 2.37 to 4.51, a double heterogeneous interface system is formed by the silicon nitride of the insulating phase and the silicon carbide of the semiconductor phase, the dielectric constant can be effectively improved, medium loss is realized, the final antioxidation layer strengthens impedance matching, so that the wave absorbing performance is excellent, as shown in FIG. 4, the strongest absorption of C2 reaches-24.5 dB, and effective absorption can be almost realized in the whole X wave band.
As shown by C3 in fig. 3, the silicon carbide content in example 3 is too large, and although the real part of the dielectric constant is not greatly different from that in example 2, the imaginary part of the dielectric constant is too high, and the dielectric medium in example 2 is changed from the medium to the high loss, and the electromagnetic performance is deteriorated due to the impedance mismatch, as shown by C3 in fig. 4.
Conclusion: by forming Si with bi-directional periodic hole structure 3 N 4 (C) Alternate deposition of SiC and Si in ceramics 3 N 4 In-situ constructing a large number of wave-transmitting/absorbing nano heterogeneous interfaces, oxidizing and removing carbon to form a discontinuous conductive network structure, optimizing impedance matching and effectively increasing the loss of materials to electromagnetic waves, and finally obtaining Si 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex-phase ceramics can almost realize effective absorption (absorption efficiency exceeds-10 dB) of X wave band when the thickness is only 2.45mm, and the strongest absorption intensity reaches-24.5 dB. The structural design can also serve a high-temperature wave-absorbing material system in a good high-temperature environment.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The preparation method of the wave-absorbing Si-C-N complex phase ceramic with the bidirectional periodic pore structure is characterized by comprising the following steps of:
s1: preparation of Si 3 N 4 (C) A porous ceramic;
s2: using Si prepared in step S1 3 N 4 (C) PorousPreparation of Si from ceramics 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Complex phase ceramic;
s3: using Si prepared in step S2 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Preparation of Si by Complex phase ceramic 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramics, i.e. Si-C-N complex phase ceramics.
2. The method for preparing the wave-absorbing Si-C-N complex phase ceramic with the bidirectional periodic pore structure according to claim 1, wherein the specific operation of the step S1 comprises the following steps:
s11: adopting a chemical vapor infiltration method to deposit Si with the diameter of 1-2 mu m on the carbon fiber cloth with the two-dimensional weaving structure in situ 3 N 4 Ceramic matrix, obtain C f /Si 3 N 4 A composite material;
s12: at 600-700 deg.C for C f /Si 3 N 4 The composite material is oxidized and kept for 1 to 5 hours to obtain Si with a bidirectional periodic pore structure 3 N 4 (C) Porous ceramics.
3. The method for preparing the wave-absorbing Si-C-N complex phase ceramic with the bi-directional periodic pore structure according to claim 2, wherein the specific operation of the step S2 comprises the steps of:
s21: si obtained in step S1 3 N 4 (C) Depositing 90-200 nm SiC interface layer on the porous ceramic in situ to obtain SiC/(Si) 3 N 4 (C) A) SiC complex phase ceramic;
s22: in SiC/(Si) 3 N 4 (C) 300-400 nm Si is deposited on the SiC complex phase ceramics in situ 3 N 4 An antioxidation layer to obtain Si 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Complex phase ceramics.
4. The method for preparing the wave-absorbing Si-C-N composite ceramic with the bi-directional periodic pore structure according to claim 3, wherein the specific operation of the step S3 is as follows:
for Si prepared in step S2 3 N 4 /(SiC/Si 3 N 4 (C)/SiC)/Si 3 N 4 Oxidizing the complex phase ceramic again, and maintaining the temperature at 600-700 ℃ for at least 8h to obtain the layered Si with the bidirectional periodic pore structure 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 Complex phase ceramics.
5. The wave-absorbing Si-C-N complex phase ceramic with a bidirectional periodic pore structure prepared by the preparation method of any one of claims 1 to 4.
6. The wave-absorbing Si-C-N complex phase ceramic having a bi-directional periodic pore structure according to claim 5, wherein said Si-C-N complex phase ceramic comprises Si 3 N 4 Ceramic matrix, intermediate SiC interface layer and outer Si layer 3 N 4 An oxidation resistant layer.
7. The wave-absorbing Si-C-N complex phase ceramic having a bi-directional periodic pore structure according to claim 6, wherein said Si 3 N 4 The thickness of the ceramic matrix is about 1-2 mu m, the thickness of the SiC interface layer is about 90-200 nm, si 3 N 4 The thickness of the antioxidation layer is about 300-400 nm.
8. A bi-directional periodic pore structure wave-absorbing Si-C-N complex phase ceramic according to claim 6 or 7, wherein said Si 3 N 4 /(SiC/Si 3 N 4 /SiC)/Si 3 N 4 The volume density of the complex phase ceramic is 1.3-1.6 g/cm 3 The porosity is 73-77%.
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| CN108395267A (en) * | 2018-05-23 | 2018-08-14 | 西北工业大学 | The fiber reinforced SiBCN ceramic matric composites of SiC with function solenoid and preparation method |
| WO2022007377A1 (en) * | 2020-07-09 | 2022-01-13 | 南京航空航天大学 | Composite material enhanced by mixed woven fiber preform and preparation method therefor |
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| CN108395267A (en) * | 2018-05-23 | 2018-08-14 | 西北工业大学 | The fiber reinforced SiBCN ceramic matric composites of SiC with function solenoid and preparation method |
| WO2022007377A1 (en) * | 2020-07-09 | 2022-01-13 | 南京航空航天大学 | Composite material enhanced by mixed woven fiber preform and preparation method therefor |
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