CN115745647B - Preparation method of ceramic matrix composite wave-absorbing honeycomb - Google Patents
Preparation method of ceramic matrix composite wave-absorbing honeycomb Download PDFInfo
- Publication number
- CN115745647B CN115745647B CN202211288369.8A CN202211288369A CN115745647B CN 115745647 B CN115745647 B CN 115745647B CN 202211288369 A CN202211288369 A CN 202211288369A CN 115745647 B CN115745647 B CN 115745647B
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- wave
- honeycomb
- ceramic
- boron nitride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 89
- 239000000835 fiber Substances 0.000 claims abstract description 62
- 238000000151 deposition Methods 0.000 claims abstract description 41
- 229910052582 BN Inorganic materials 0.000 claims abstract description 32
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011159 matrix material Substances 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 20
- 239000000919 ceramic Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 15
- 230000008595 infiltration Effects 0.000 claims abstract description 14
- 238000001764 infiltration Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000000853 adhesive Substances 0.000 claims abstract description 12
- 230000001070 adhesive effect Effects 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000010521 absorption reaction Methods 0.000 claims abstract description 9
- 238000009941 weaving Methods 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- 230000008021 deposition Effects 0.000 claims description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims description 22
- 239000012700 ceramic precursor Substances 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 15
- 239000004744 fabric Substances 0.000 claims description 14
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 14
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 10
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000003085 diluting agent Substances 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 6
- 229920001709 polysilazane Polymers 0.000 claims description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 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 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 239000003365 glass fiber Substances 0.000 claims description 5
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 5
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 5
- 229920003257 polycarbosilane Polymers 0.000 claims description 5
- 239000005049 silicon tetrachloride Substances 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- -1 polysiloxane Polymers 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000009954 braiding Methods 0.000 claims 1
- 239000004760 aramid Substances 0.000 description 5
- 229920003235 aromatic polyamide Polymers 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000011184 SiC–SiC matrix composite Substances 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000009958 sewing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Ceramic Products (AREA)
Abstract
The invention relates to a silicon carbide ceramic matrix composite honeycomb with high-temperature electromagnetic wave absorption performance and a preparation method thereof. Weaving silicon carbide fibers into corrugated plate-shaped fiber preformed bodies by using a die, preparing and depositing a boron nitride interface layer on the surfaces of the silicon carbide fibers by using a chemical vapor infiltration process, depositing a composite material matrix on the surfaces of the boron nitride interface layer by using the chemical vapor infiltration process, bonding the corrugated plates of the silicon carbide ceramic matrix composite material into honeycomb preformed bodies by using a ceramic slurry adhesive, and finally depositing the matrix to obtain the silicon carbide ceramic matrix composite material wave-absorbing honeycomb. The prepared wave-absorbing honeycomb has good high temperature resistance, high strength and excellent room temperature and high temperature wave-absorbing performance, and has potential application prospect in the field of high temperature wave absorption.
Description
Technical Field
The invention relates to a preparation method of a high-temperature-resistant ceramic matrix composite wave-absorbing honeycomb.
Background
With the continuous development of radar detection technology, the requirements of aircrafts on stealth performance are continuously improved. The honeycomb wave-absorbing material is used as a structural wave-absorbing material, has the characteristics of light weight, high strength, good wave-absorbing performance and the like, and is widely applied to airplanes, radars and some civil fields. The wave-absorbing honeycomb mainly used at present is an aramid paper honeycomb composite material, and is prepared by impregnating the aramid paper honeycomb with wave-absorbing paint. Because the temperature resistance of the aramid paper is low, the aramid honeycomb structure is widely used for wings, tail wings and the like of an aircraft in the aerospace field, so that the wave absorbing performance of a hot end part (such as an engine tail nozzle) of the aircraft is poor, and the integral stealth effect is influenced. The ceramic matrix composite has a series of advantages of low density, high specific strength, oxidation resistance, high temperature resistance and the like, and if the skeleton of the wave-absorbing honeycomb is replaced by the ceramic matrix wave-absorbing composite by aramid paper, the service temperature of the wave-absorbing honeycomb can be effectively increased, the wave-absorbing performance of a hot end part of an aircraft is obviously improved, and the whole stealth effect is improved.
The patent CN108794046B, an alumina ceramic matrix composite honeycomb and a preparation method thereof, discloses a high-temperature-resistant alumina ceramic matrix composite honeycomb and a preparation method thereof, and the alumina ceramic fiber cloth prepreg is cut, molded, dried, bonded and sintered to obtain the ceramic matrix composite honeycomb. However, the aluminum oxide fiber and the matrix are both wave-transparent materials, and the composite material honeycomb taking the aluminum oxide fiber and the matrix as a framework cannot effectively absorb electromagnetic waves. In addition, the solid-phase powder sintering method tends to have higher sintering temperature, and the fiber is greatly damaged by the excessively high temperature, so that the mechanical and wave-absorbing properties of the fiber are affected.
Disclosure of Invention
The invention aims to provide a preparation method of a ceramic matrix composite wave-absorbing honeycomb with high-temperature electromagnetic wave absorption performance, which is used for solving the problems of low high temperature resistance and low strength in the existing wave-absorbing honeycomb.
The invention provides the following technical scheme: a silicon carbide ceramic matrix composite wave-absorbing honeycomb having high-temperature electromagnetic wave absorption properties, the wave-absorbing honeycomb comprising:
a silicon carbide fiber preform woven from silicon carbide fibers;
the boron nitride interface layer is prepared through a chemical vapor infiltration process and deposited on the surface of the silicon carbide fiber;
the composite material matrix is prepared by a chemical vapor infiltration process and deposited on the surface of the boron nitride interface layer.
In the silicon carbide ceramic matrix composite wave-absorbing honeycomb provided by the invention, silicon carbide fibers are used as a semiconductor material, the dielectric property is adjustable, and the silicon carbide ceramic matrix composite wave-absorbing honeycomb is a dielectric loss type wave-absorbing material, so that the absorption capacity of the honeycomb to electromagnetic waves is determined.
The boron nitride interface layer has better oxidation resistance, thermal shock resistance and chemical stability, and has lower dielectric constant and dielectric loss, so that the interface binding force between the fiber and the matrix can be effectively improved while the wave absorbing performance of the honeycomb is not influenced, and the mechanical property of the composite honeycomb is obviously improved.
The Chemical Vapor Infiltration (CVI) process can prepare a uniform and compact composite material matrix at a lower temperature, and the residual stress in the material is small, so that the fiber is hardly damaged, and the strength of the honeycomb can be remarkably improved. In addition, the composite material matrix is made of medium-low dielectric materials, electromagnetic waves can be prevented from being reflected on the surface of the material, more electromagnetic waves can enter the composite material, the wave absorbing function of the silicon carbide fiber is fully exerted, and the wave absorbing performance of the composite material honeycomb is improved.
The medium-low dielectric matrix comprises a silicon nitride matrix and a silicon carbide matrix.
The invention also provides a preparation method of the silicon carbide ceramic matrix composite wave-absorbing honeycomb with high-temperature electromagnetic wave absorption performance, which comprises the following steps:
step 1, weaving silicon carbide fibers into corrugated plate-shaped fiber preforms: weaving continuous silicon carbide fiber tows into plain silicon carbide fiber cloth, then cutting the silicon carbide fiber cloth into corresponding sizes according to the size of a corrugated plate die, and stacking the silicon carbide fiber cloth layer by layer, wherein the stacking layer is determined by the thickness of honeycomb walls; then, stitching the corrugated plate-shaped silicon carbide fiber preform along the thickness direction by using continuous glass fibers to obtain the corrugated plate-shaped silicon carbide fiber preform;
in the step 1, the width of the fiber cloth is 10-30 mm, and the stacking layer number is 4-8.
Step 2, preparing a boron nitride interface layer by a chemical vapor infiltration process: placing the silicon carbide fiber preform in the step 1 into a vacuum furnace, introducing argon, hydrogen, boron trichloride and ammonia gas, reacting at high temperature and high pressure to generate boron nitride, and depositing a boron nitride interface layer on the surface of the silicon carbide fiber preform;
in the step 2, the pressure in the vacuum furnace is 100-400 Pa, the temperature is 600-800 ℃, argon in the gas is used as diluent gas, hydrogen is used as carrier gas, boron trichloride provides boron source, ammonia gas provides nitrogen source, boron trichloride reacts with ammonia gas, a boron nitride interface layer is deposited on the surface of the silicon carbide fiber preform for 20-50 h, and the thickness of the boron nitride interface layer is 200-600 nm.
Step 3, preparing a composite material matrix by a chemical vapor infiltration process: placing the preform of which the boron nitride interface layer is deposited in the step 2 into a deposition furnace, introducing argon, hydrogen and gases corresponding to different matrixes into the deposition furnace, reacting at high temperature and high pressure, and depositing the matrixes on the surface of the boron nitride interface layer to obtain the silicon carbide ceramic matrix composite corrugated plate;
in the step 3, the pressure in the deposition furnace is 100-400 Pa, the temperature is 700-1000 ℃, argon in the gas is used as diluent gas, hydrogen is used as carrier gas, the substrate is silicon nitride or silicon carbide, and the deposition time is 100-150 h.
And 4, connecting the corrugated plates of the silicon carbide ceramic matrix composite material obtained in the step 3 together by using a ceramic slurry adhesive, and then carrying out matrix deposition under the same deposition conditions as those of the step 2 to obtain the silicon carbide ceramic matrix composite material wave-absorbing honeycomb.
In the step 4, the ceramic slurry adhesive consists of ceramic powder and ceramic precursor solution, wherein the mass ratio is 1:5-1:10;
the ceramic powder is silicon nitride or silicon carbide;
the solvent in the ceramic precursor solution is any one of dimethylbenzene, cyclohexane and tetrahydrofuran, the ceramic precursor is any one of Polyborosilazane (PBSN), polysiloxane (PSO) and Polysilazane (PSN), and the volume ratio of the solvent to the ceramic precursor is 1:2-1:4.
the invention has the beneficial effects that:
the invention adopts a chemical vapor infiltration method to prepare the silicon carbide ceramic matrix composite corrugated plate at a lower temperature, and the corrugated plate is bonded together by utilizing a ceramic slurry adhesive and a deposition matrix to obtain the silicon carbide ceramic matrix composite wave-absorbing honeycomb. The prepared wave-absorbing honeycomb has good high temperature resistance, high strength and excellent room temperature and high temperature wave-absorbing performance.
Drawings
FIG. 1 is a flow chart of a process for preparing a silicon carbide ceramic matrix composite wave-absorbing honeycomb;
FIG. 2 is a photograph of a corrugated board fiber preform;
FIG. 3 is a photograph of a wave-absorbing honeycomb of a silicon carbide ceramic matrix composite;
FIG. 4 is a graph of the room temperature wave absorbing performance of a silicon carbide ceramic matrix composite wave absorbing honeycomb.
Detailed Description
The embodiment provides a preparation method of a silicon carbide ceramic matrix composite wave-absorbing honeycomb with high-temperature electromagnetic wave absorption performance, as shown in fig. 1, comprising the following steps:
step 1, weaving silicon carbide fibers into corrugated plate-shaped fiber preforms: weaving continuous silicon carbide fiber tows into plain silicon carbide fiber cloth, then cutting the silicon carbide fiber cloth into corresponding sizes according to the size of a corrugated plate die, and stacking the silicon carbide fiber cloth layer by layer, wherein the stacking layer is determined by the thickness of honeycomb walls; then, stitching the corrugated plate-shaped silicon carbide fiber preform along the thickness direction by using continuous glass fibers to obtain the corrugated plate-shaped silicon carbide fiber preform;
step 2, preparing a boron nitride interface layer by a chemical vapor infiltration process: placing the silicon carbide fiber preform in the step 1 into a vacuum furnace, introducing argon, hydrogen, boron trichloride and ammonia gas, reacting at high temperature and high pressure to generate boron nitride, and depositing a boron nitride interface layer on the surface of the silicon carbide fiber preform;
step 3, preparing a composite material matrix by a chemical vapor infiltration process: placing the preform of which the boron nitride interface layer is deposited in the step 2 into a deposition furnace, introducing argon, hydrogen and gases corresponding to different matrixes into the deposition furnace, reacting at high temperature and high pressure, and depositing the matrixes on the surface of the boron nitride interface layer to obtain the silicon carbide ceramic matrix composite corrugated plate;
and 4, connecting the corrugated plates of the silicon carbide ceramic matrix composite material obtained in the step 3 together by using a ceramic slurry adhesive, and then carrying out matrix deposition under the same deposition conditions as those of the step 2 to obtain the silicon carbide ceramic matrix composite material wave-absorbing honeycomb.
In the step 1, the width of the fiber cloth is 10-30 mm, and the stacking layer number is 4-8.
In the step 2, the pressure in the vacuum furnace is 100-400 Pa, the temperature is 600-800 ℃, argon in the gas is used as diluent gas, hydrogen is used as carrier gas, boron trichloride provides boron source, ammonia gas provides nitrogen source, the flow of argon is 3-5L/min, the flow of hydrogen is 7-10L/min, the flow of boron trichloride is 4-6L/min, the flow of ammonia is 5-7L/min, boron trichloride reacts with ammonia gas, the deposition time is 20-50 h, and the thickness of a boron nitride interface layer is 200-600 nm.
In the step 3, the pressure in the deposition furnace is 100-400 Pa, the temperature is 700-1000 ℃, argon in the gas is used as diluent gas, hydrogen is used as carrier gas, reaction gas is silicon tetrachloride and ammonia (silicon nitride is used as a matrix) or methyltrichlorosilane (silicon carbide is used as a matrix), the flow rate of argon is 3-5L/min, the flow rate of hydrogen is 7-10L/min, the flow rate of silicon tetrachloride is 2-4L/min, the flow rate of ammonia is 3-5L/min, the flow rate of methyltrichlorosilane is 5-7L/min, and the deposition time is 100-150 h.
In the step 4, the ceramic slurry adhesive consists of ceramic powder and ceramic precursor solution, wherein the mass ratio is 1:5-1:10. the ceramic powder is silicon nitride or silicon carbide. The solvent in the ceramic precursor solution is any one of dimethylbenzene, cyclohexane and tetrahydrofuran, the ceramic precursor is any one of Polyborosilazane (PBSN), polysiloxane (PSO), polysilazane (PSN) and Polycarbosilane (PCS), and the volume ratio of the solvent to the ceramic precursor is 1:2-1:4.
example 1
And step 1, cutting the silicon carbide fiber cloth into strips with the width of 30mm and the length of 310mm, stacking four layers in a corrugated plate die, and then sewing with continuous glass fibers along the thickness direction to obtain a corrugated plate-shaped silicon carbide fiber preform.
Step 2, placing the corrugated plate-shaped silicon carbide fiber preform in the step 1 into a vacuum furnace, introducing argon, hydrogen, boron trichloride and ammonia gas, wherein the temperature is 700 ℃, the pressure is 200Pa, the argon flow is 4L/min, the hydrogen flow is 9L/min, the boron trichloride flow is 5L/min, the ammonia gas flow is 6L/min, and reacting for 40 hours, and depositing a boron nitride interface layer on the surface of the silicon carbide fiber preform;
step 3, preparing Si by chemical vapor infiltration process 3 N 4 A substrate: putting the preform of which the boron nitride interface layer is deposited in the step 2 into a deposition furnace, introducing argon, hydrogen, silicon tetrachloride and ammonia gas into the deposition furnace, wherein the temperature is 800 ℃, the pressure is 300Pa, the argon flow is 4L/min, the hydrogen flow is 9L/min, the silicon tetrachloride flow is 3L/min, the ammonia flow is 4L/min, reacting for 120 hours, and depositing a silicon nitride matrix on the surface of the boron nitride interface layer to obtain SiC/Si 3 N 4 Corrugated sheet of composite material, as shown in fig. 2;
step 4, siC/Si obtained in the step 3 is processed 3 N 4 The composite corrugated plates are connected together by using a ceramic slurry adhesive, and the ceramic slurry adhesive is prepared from silicon nitride powder and a ceramic precursor solution according to a mass ratio of 1:7, mixing and stirring to prepare the ceramic precursor solution, wherein the volume ratio of the dimethylbenzene to the polyborosilazane is 1:3, preparing. Then Si is carried out again 3 N 4 Depositing a matrix, wherein the deposition conditions are the same as those of the step 2, and obtaining SiC/Si 3 N 4 The composite wave-absorbing honeycomb is shown in fig. 3.
The obtained SiC/Si 3 N 4 The composite material wave-absorbing honeycomb is subjected to wave-absorbing performance test, the room temperature wave-absorbing performance is shown in figure 4, the effective wave-absorbing bandwidth (smaller than-10 dB) can reach 14GHz in the frequency range of 2-18 GHz, and the total frequency of 2-4GHz at low frequency is smaller than-10 dB, so that the composite material wave-absorbing honeycomb has excellent low-frequency and broadband wave-absorbing performance. In addition, the wave-absorbing honeycomb has good wave-absorbing performance at 1000 ℃, and the wave-absorbing honeycomb can reach full frequency-6 dB in 2-18 GHz.
Example 2
And step 1, cutting the silicon carbide fiber cloth into strips with the width of 25mm and the length of 330mm, stacking four layers in a corrugated plate die, and then sewing with continuous glass fibers along the thickness direction to obtain a corrugated plate-shaped silicon carbide fiber preform.
Step 2, placing the corrugated plate-shaped silicon carbide fiber preform in the step 1 into a vacuum furnace, introducing argon, hydrogen, boron trichloride and ammonia gas, wherein the temperature is 700 ℃, the pressure is 200Pa, the argon flow is 4L/min, the hydrogen flow is 9L/min, the boron trichloride flow is 5L/min, the ammonia gas flow is 6L/min, and reacting for 40 hours, and depositing a boron nitride interface layer on the surface of the silicon carbide fiber preform;
step 3, preparing a silicon carbide matrix by a chemical vapor infiltration process: placing the preform of which the boron nitride interface layer is deposited in the step 2 into a deposition furnace, introducing argon, hydrogen and methyltrichlorosilane into the deposition furnace, wherein the temperature is 900 ℃, the pressure is 400Pa, the argon flow is 5L/min, the hydrogen flow is 10L/min, the methyltrichlorosilane flow is 7L/min, reacting for 140 hours, and depositing a silicon carbide substrate on the surface of the boron nitride interface layer to obtain the SiC/SiC composite corrugated plate;
step 4, connecting the SiC/SiC composite material corrugated plates obtained in the step 3 together by using a ceramic slurry adhesive, wherein the ceramic slurry adhesive comprises silicon carbide powder and a ceramic precursor solution according to a mass ratio of 1:6, mixing and stirring to prepare the ceramic precursor solution, wherein the ceramic precursor solution is prepared from dimethylbenzene and polycarbosilane according to the volume ratio of 1:4, preparing. And then depositing a silicon carbide substrate, wherein the deposition conditions are the same as those of the step 2, and obtaining the SiC/SiC composite material wave-absorbing honeycomb.
And (3) performing a wave absorbing performance test on the obtained silicon carbide/silicon carbide composite material wave absorbing honeycomb, wherein the effective wave absorbing bandwidth (less than-10 dB) of the room temperature wave absorbing performance within the frequency range of 2-18 GHz is 11GHz. In addition, the wave-absorbing honeycomb can reach full frequency-4 dB at 1000 ℃ within 2-18 GHz.
Claims (2)
1. A preparation method of a silicon carbide ceramic matrix composite wave-absorbing honeycomb with high-temperature electromagnetic wave absorption performance is characterized in that the honeycomb takes a silicon carbide ceramic matrix composite as a framework;
the silicon carbide ceramic matrix composite includes:
a silicon carbide fiber preform woven from silicon carbide fibers;
the boron nitride interface layer is prepared through a chemical vapor infiltration process and deposited on the surface of the silicon carbide fiber;
the composite material matrix is prepared by a chemical vapor infiltration process and deposited on the surface of the boron nitride interface layer;
the composite material matrix comprises a silicon nitride matrix and a silicon carbide matrix;
the silicon carbide ceramic matrix composite wave-absorbing honeycomb with high-temperature electromagnetic wave absorption performance is prepared according to the following steps:
step 1, weaving silicon carbide fibers into corrugated plate-shaped fiber preforms;
step 2, placing the silicon carbide fiber preform in the step 1 into a vacuum furnace, introducing argon, hydrogen, boron trichloride and ammonia gas, reacting at high temperature and high pressure to generate boron nitride, and depositing a boron nitride interface layer on the surface of the silicon carbide fiber preform;
step 3, placing the preform of which the boron nitride interface layer is deposited in the step 2 into a deposition furnace, introducing argon, hydrogen and gases corresponding to different matrixes into the deposition furnace, reacting at high temperature and high pressure, and depositing the matrixes on the surface of the boron nitride interface layer to obtain the silicon carbide ceramic matrix composite corrugated plate;
step 4, connecting the corrugated plates of the silicon carbide ceramic matrix composite material obtained in the step 3 together by using a ceramic slurry adhesive, and then carrying out matrix deposition, wherein the deposition conditions are the same as those of the step 2, so as to obtain the silicon carbide ceramic matrix composite material wave-absorbing honeycomb;
in the step 2, the pressure in the vacuum furnace is 100-400 Pa, the temperature is 600-800 ℃, argon in the gas is used as diluent gas, hydrogen is used as carrier gas, boron trichloride provides a boron source, ammonia gas provides a nitrogen source, boron trichloride reacts with ammonia gas, a boron nitride interface layer is deposited on the surface of the silicon carbide fiber preform for 20-50 h, and the thickness of the boron nitride interface layer is 200-600 nm;
in the step 3, the pressure in the deposition furnace is 100-400 Pa, the temperature is 700-1000 ℃, argon in the gas is used as diluent gas, hydrogen is used as carrier gas, when the substrate is silicon nitride, the reaction gas is silicon tetrachloride and ammonia, or when the substrate is silicon carbide, the reaction gas is methyltrichlorosilane, and the deposition time is 100-150 h;
in the step 4, the ceramic slurry adhesive consists of ceramic powder and ceramic precursor solution, wherein the mass ratio is 1:5-1:10; the ceramic powder is silicon nitride or silicon carbide; the solvent in the ceramic precursor solution is any one of dimethylbenzene, cyclohexane and tetrahydrofuran, the ceramic precursor is any one of Polyborosilazane (PBSN), polysiloxane (PSO), polysilazane (PSN) and Polycarbosilane (PCS), and the volume ratio of the solvent to the ceramic precursor is 1:2-1:4.
2. the method of manufacturing according to claim 1, wherein in the step 1, braiding silicon carbide fibers into corrugated plate-like fiber preform comprises:
weaving continuous silicon carbide fiber tows into plain silicon carbide fiber cloth, then cutting the silicon carbide fiber cloth into corresponding sizes according to the size of a corrugated plate die, and stacking the silicon carbide fiber cloth layer by layer, wherein the stacking layer is determined by the thickness of honeycomb walls; and then stitching the corrugated plate-shaped silicon carbide fiber preform along the thickness direction by using continuous glass fibers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211288369.8A CN115745647B (en) | 2022-10-20 | 2022-10-20 | Preparation method of ceramic matrix composite wave-absorbing honeycomb |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211288369.8A CN115745647B (en) | 2022-10-20 | 2022-10-20 | Preparation method of ceramic matrix composite wave-absorbing honeycomb |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115745647A CN115745647A (en) | 2023-03-07 |
| CN115745647B true CN115745647B (en) | 2024-02-09 |
Family
ID=85352325
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211288369.8A Active CN115745647B (en) | 2022-10-20 | 2022-10-20 | Preparation method of ceramic matrix composite wave-absorbing honeycomb |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115745647B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5851403A (en) * | 1995-01-04 | 1998-12-22 | Northrop Grumman Corporation | Ceramic honeycomb and method |
| CN108440007A (en) * | 2018-04-24 | 2018-08-24 | 苏州宏久航空防热材料科技有限公司 | A kind of control of two-dimensional braided silicon carbide fibre fabric enhancing composite material of silicon carbide filter plate |
| CN109703136A (en) * | 2019-01-23 | 2019-05-03 | 大连理工大学 | A kind of segmented wave structure inhales wave cellular composite material and preparation method thereof |
| CN111943721A (en) * | 2019-05-17 | 2020-11-17 | 深圳光启高端装备技术研发有限公司 | Preparation method and application of high-temperature-resistant wave-absorbing composite material |
| CN112876273A (en) * | 2021-03-17 | 2021-06-01 | 中南大学 | High-temperature-resistant wave-absorbing structure integrated ceramic matrix composite and preparation method thereof |
| CN114014680A (en) * | 2021-11-19 | 2022-02-08 | 西北工业大学 | Ceramic matrix composite material turbine outer ring and preparation method thereof |
-
2022
- 2022-10-20 CN CN202211288369.8A patent/CN115745647B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5851403A (en) * | 1995-01-04 | 1998-12-22 | Northrop Grumman Corporation | Ceramic honeycomb and method |
| CN108440007A (en) * | 2018-04-24 | 2018-08-24 | 苏州宏久航空防热材料科技有限公司 | A kind of control of two-dimensional braided silicon carbide fibre fabric enhancing composite material of silicon carbide filter plate |
| CN109703136A (en) * | 2019-01-23 | 2019-05-03 | 大连理工大学 | A kind of segmented wave structure inhales wave cellular composite material and preparation method thereof |
| CN111943721A (en) * | 2019-05-17 | 2020-11-17 | 深圳光启高端装备技术研发有限公司 | Preparation method and application of high-temperature-resistant wave-absorbing composite material |
| CN112876273A (en) * | 2021-03-17 | 2021-06-01 | 中南大学 | High-temperature-resistant wave-absorbing structure integrated ceramic matrix composite and preparation method thereof |
| CN114014680A (en) * | 2021-11-19 | 2022-02-08 | 西北工业大学 | Ceramic matrix composite material turbine outer ring and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Electromagnetic wave absorption and mechanical properties of silicon carbide fibers reinforced silicon nitride matrix composites;Ran Mo等;《Journal of the European Ceramic Society》;第1-30页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115745647A (en) | 2023-03-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Nag et al. | High temperature ceramic radomes (HTCR)–A review | |
| CN112341229B (en) | Gradient C/ZrC-SiC superhigh temperature ceramic matrix composite and preparation method thereof | |
| CN113773098B (en) | High electromagnetic wave shielding silicon carbide ceramic matrix composite material and preparation method thereof | |
| CN103253938B (en) | Chemical vapor deposition method of Si-B-C-N amorphous ceramic | |
| EP0799809B1 (en) | Ceramic matrix composites | |
| CN101503305A (en) | Process for preparing self-sealing silicon carbide ceramic based composite material | |
| CN111592371B (en) | Titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and preparation method thereof | |
| CN103922776B (en) | Silicon carbide fiber reinforced silicon carbide composite material microwave-absorbing ceramic and preparation method thereof | |
| CN112341228B (en) | C/ZrC-SiC superhigh temperature ceramic matrix composite and preparation method thereof | |
| CA2299603C (en) | Method for manufacturing ceramic-based composite material | |
| CN108101566B (en) | Method for preparing silicon carbide ceramic matrix composite component with assistance of RTM (resin transfer molding) process | |
| Ding et al. | Influence of pyrolytic carbon coatings on complex permittivity and microwave absorbing properties of Al2O3 fiber woven fabrics | |
| CN113045325B (en) | Preparation method of high-strength carbon/carbon-silicon carbide composite material | |
| CN114315394B (en) | By using Ti 3 SiC 2 Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material | |
| CN114716258B (en) | Preparation method of carbon fiber reinforced boron carbide composite material | |
| CN115745647B (en) | Preparation method of ceramic matrix composite wave-absorbing honeycomb | |
| CN106588124A (en) | Low-temperature preparation method of ceramic coating absorbing waves in frequency band of 8-18 GHz | |
| CN108395267A (en) | The fiber reinforced SiBCN ceramic matric composites of SiC with function solenoid and preparation method | |
| CN114988901A (en) | Rapid preparation method of high-density SiC/SiC composite material | |
| WO2020104959A1 (en) | Process for obtaining composite, ultra-refractory, fibre-reinforced ceramic materials | |
| Shimoda et al. | Novel production route for SiC/SiC ceramic-matrix composites using sandwich prepreg sheets | |
| CN114621728A (en) | High-temperature-resistant broadband wave-absorbing structure composite material and preparation method thereof | |
| CN115417685B (en) | SiC/Si with electromagnetic wave absorption performance 3 N 4 Composite and method for producing same | |
| EP4201915A1 (en) | Introduction of metallic particles to enable formation of metallic carbides in a matrix | |
| KR100829711B1 (en) | Fabrication method of high density silicon carbide fiber reinforced silicon carbide composite materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |