CN116606148A - Ceramic matrix composite material with three-dimensional gradient periodic structure and preparation method thereof - Google Patents
Ceramic matrix composite material with three-dimensional gradient periodic structure and preparation method thereof Download PDFInfo
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- CN116606148A CN116606148A CN202310541057.1A CN202310541057A CN116606148A CN 116606148 A CN116606148 A CN 116606148A CN 202310541057 A CN202310541057 A CN 202310541057A CN 116606148 A CN116606148 A CN 116606148A
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- 230000000737 periodic effect Effects 0.000 title claims abstract description 51
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000835 fiber Substances 0.000 claims abstract description 100
- 239000004744 fabric Substances 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims description 40
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 28
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 239000002131 composite material Substances 0.000 claims description 24
- 238000005336 cracking Methods 0.000 claims description 17
- 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 15
- 239000005049 silicon tetrachloride Substances 0.000 claims description 15
- 238000009826 distribution Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 239000013306 transparent fiber Substances 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 11
- 238000005470 impregnation Methods 0.000 claims description 10
- 230000008595 infiltration Effects 0.000 claims description 10
- 238000001764 infiltration Methods 0.000 claims description 10
- 229920000642 polymer Polymers 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 238000011065 in-situ storage Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- -1 polysiloxane Polymers 0.000 claims description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- 239000012700 ceramic precursor Substances 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000003475 lamination Methods 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 4
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 238000000280 densification Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229920001709 polysilazane Polymers 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 abstract description 4
- 229920000049 Carbon (fiber) Polymers 0.000 description 16
- 239000004917 carbon fiber Substances 0.000 description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- 230000008021 deposition Effects 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000004088 simulation Methods 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000010147 laser engraving Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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Abstract
The invention discloses a three-dimensional gradient periodic structure ceramic matrix composite and a preparation method thereof. The preparation method has the advantages of strong designability, various forms, easy molding, no damage to wave-transmitting fiber cloth and the like, and can realize the integrated preparation of the low-frequency and broadband wave-absorbing ceramic matrix composite material under the condition of thinner thickness.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a three-dimensional gradient periodic structure ceramic matrix composite material and a preparation method thereof.
Background
With the rapid development of all-round, all-weather and multi-band radar detection technology, the improvement of the flying speed and stealth capability of stealth aircraft is urgently needed. The engine tail spray component is used as an important radar scattering source of a stealth fighter, and because of high service temperature, a high-temperature radar wave absorbing material is needed to be adopted on the basis of the appearance stealth design to improve the stealth performance of the engine tail spray component. The ceramic material has excellent performances of high temperature resistance, oxidation resistance, corrosion resistance, high strength, high modulus, low density, low dielectric constant and the like, and is a key thermal structure material for engine tail spray parts. However, the brittle nature of ceramic materials makes them susceptible to catastrophic failure when loaded, and the mechanical properties of ceramics can be effectively improved by Ceramic Matrix Composites (CMC) prepared from continuous fiber toughened ceramics. The CMC consists of a fiber preform, an interface and a matrix, and the electrical properties of the interface and the matrix are effectively regulated and controlled by reasonably designing the structure (periodic structure) of the fiber preform, so that the broadband wave absorbing performance of the CMC is improved. At present, the high-temperature broadband wave absorbing performance of CMC is mainly improved through a multilayer impedance matching design and a surface periodic structure design.
At present, the periodic structure design of the ceramic matrix composite material is biased to adopt methods such as electrochemical etching, laser engraving, numerical control processing and the like, so that the continuity of the fiber is destroyed, and the bearing capacity of the fiber is influenced. Therefore, the integrated preparation method for the ultra-wideband wave-absorbing gradient periodic structure ceramic matrix composite material has important academic research and application demand values.
Disclosure of Invention
In order to solve the problem that the continuity of fibers is damaged in the existing ceramic matrix composite preparation process, one of the purposes of the invention is to provide a preparation method of a ceramic matrix composite with a three-dimensional gradient periodic structure.
The technical scheme for solving the technical problems is as follows:
the preparation method of the ceramic matrix composite with the three-dimensional gradient periodic structure comprises the following steps:
step 1, simulating the thickness of a medium layer and the size and distribution of a wave absorbing unit of a gradient periodic structure by adopting electromagnetic simulation software, wherein the medium layer is wave-transmitting fiber cloth;
step 2, cutting the wave-transparent fiber cloth according to the thickness of the medium layer simulated in the step 1, and oxidizing the cut wave-transparent fiber cloth to remove impurities on the wave-transparent fiber cloth; preferably, the oxidation treatment is aimed at removing the gum layer on the wave-transparent fiber cloth.
Step 3, forming conductive fiber cloth on the wave-transmitting fiber cloth processed in the step 2 in situ according to the size and the distribution of the wave-absorbing unit of the gradient periodic structure simulated in the step 1, so as to obtain a fiber preform;
and 4, densifying the fiber preform, and generating a ceramic matrix in the fiber preform to prepare the ceramic matrix composite material with the three-dimensional gradient periodic structure.
The beneficial effects of the invention are as follows: according to the invention, the thickness of a dielectric layer is simulated according to the dielectric constant and the loss value of the wave-transparent fiber cloth, and the size and the distribution of the wave-absorbing units of the gradient periodic structure are simulated according to the conductivity of the conductive fiber cloth; in the simulation process, the thickness of the dielectric layer (changing the dielectric constant and the loss value) and the wave absorbing unit of the gradient periodic structure (changing the conductivity, distribution, size and other structural parameters of the conductive fiber cloth) are changed so as to obtain the ceramic matrix composite material with the three-dimensional gradient periodic structure and better performance;
therefore, the preparation method provided by the invention has the advantages of strong designability, various forms, easiness in forming, no damage to the wave-transmitting fiber cloth and the like, and can realize the integrated preparation of the low-frequency and broadband wave-absorbing ceramic matrix composite material under the condition of thinner thickness.
Based on the technical scheme, the invention can also be improved as follows:
further, the dielectric constant of the wave-transparent fiber is less than or equal to 6; preferably, the wave-transparent fiber cloth is Al 2 O 3 Fiber, si 3 N 4 Fibers, siO 2 Any one of a fiber and a mullite fiber.
Further, the condition of the oxidation treatment of the wave-transparent fiber cloth in the step 2 is as follows: air atmosphere, temperature 500-600 deg.c and oxidation time 5-6 hr.
Further, the conductive fiber cloth has conductivity of 10 3 ～10 6 S/m fibers; preferably, the conductive fiber cloth is carbon fiber or silicon carbide fiber.
Further, the dielectric constant of the ceramic matrix in step 4 is less than 10.
Further, the ceramic matrix is SiOC, si 3 N 4 At least one of SiCN and SiBCN.
Further, the densification process in step 4 includes: a polymer impregnation pyrolysis process and/or a chemical vapor infiltration process;
the polymer impregnation and pyrolysis process comprises the following steps: immersing the fiber preform or the fiber preform treated by the chemical vapor infiltration process in a mixture of a ceramic precursor, and then sequentially curing and cracking in an inert atmosphere; preferably, the mixture is obtained by dispersing the ceramic precursor in an organic solvent, wherein the organic solvent is xylene or toluene.
The chemical vapor infiltration process comprises the following steps: placing the fiber preform or the fiber preform treated by the polymer impregnation cracking process into a mixed gas containing silicon tetrachloride and ammonia gas, and generating Si at 800-1100 DEG C 3 N 4 A substrate. Preferably, when the chemical vapor infiltration process is carried out, the fiber preform or the fiber preform after the polymer impregnation and pyrolysis process is firstly placed in a deposition furnace with vacuum of 300Pa, and then mixed gas containing silicon tetrachloride and ammonia is introduced.
The beneficial effect of adopting above-mentioned technical scheme: when the polymer impregnation cracking process and the chemical vapor infiltration process are combined to densify the fiber preform, the sequence can be exchanged according to actual conditions; the densified fiber preform has better high temperature resistance, realizes the cooperative wave absorption of the ceramic matrix composite at room temperature/high temperature, and solves the problem of the attenuation of the high temperature wave absorption performance of the ceramic matrix composite.
Further, preferably Si 3 N 4 The thickness of the matrix is 30-100 mu m.
Further, the ceramic precursor is polysiloxane, polysilazane or polysilabozane;
the dipping conditions are as follows: immersing in vacuum or pressurizing to 0.8-1.0 Mpa for 0.5-1 h.
The curing conditions are as follows: solidifying for 1-2 h at 200-300 ℃; preferably, the curing conditions are: curing for 2h at 200 ℃;
the cracking conditions are as follows: cracking for 2-3 h at 900-1000 ℃; preferably, the cleavage conditions are: cracking for 2 hours at 900 ℃;
the inert atmosphere is: nitrogen or argon;
the mixed gas also comprises argon and hydrogen; the volumes of silicon tetrachloride, ammonia, hydrogen and argon in the mixed gas are as follows: 1-1.5:1-1.5:5-8:5-8. Preferably, the volumes of silicon tetrachloride, ammonia, hydrogen and argon in the mixed gas are as follows: 1:1:5:7.
The second purpose of the invention is to provide a ceramic matrix composite with a three-dimensional gradient periodic structure.
The beneficial effects of the invention are as follows: the gradient periodic structure wave-absorbing unit in the composite material has the advantages of simple molding process, short preparation period, wide wave-absorbing frequency band and good mechanical property.
Further, the porosity of the ceramic matrix composite with the three-dimensional gradient periodic structure is less than 10%;
the wave absorbing units of the gradient periodic structure in the composite material are in gradient distribution along the lamination direction of the conductive fiber cloth;
the area of the conductive fiber cloth of the wave absorbing unit of the gradient periodic structure in the composite material is gradually decreased from top to bottom in the lamination process, so that a three-dimensional gradient structure is formed.
The invention has the following beneficial effects:
1. the invention provides an in-situ forming gradient periodic structure wave absorbing unit on a medium layer wave-transmitting fiber cloth, and a fiber preform is formed by laminating conductive fiber cloth on wave-transmitting fibers, so that the wave absorbing performance of a ceramic matrix composite material with a three-dimensional gradient periodic structure at 4-40GHz ultra-wideband is effectively improved, the bottleneck problems of low-frequency and broadband wave absorption of the ceramic matrix composite material are solved, in addition, the preparation method also avoids the damage to the continuity of the conductive fibers and the wave-transmitting fibers, and the influence on the bearing capacity of the composite material is small.
2. The invention provides a method for forming discrete periodic wave absorbing units on a medium layer wave-transmitting fiber cloth in situ by adopting conductive fiber cloth (namely, each wave absorbing unit is discontinuously and not overlapped on the medium layer), and densifying an in-situ formed fiber preform by a polymer impregnation cracking (PIP) process and/or a Chemical Vapor Infiltration (CVI) process, thereby forming uniform and compact interfaces and matrixes in gaps of the fiber preform, cooperatively improving the wave absorbing and mechanical properties of a ceramic matrix composite material, and solving the problem that the ceramic matrix composite material is difficult to bear and be compatible with radar stealth.
3. According to the invention, carbon fiber or silicon carbide fiber with stable high-temperature electrical property and thermal property is used as a wave-absorbing unit forming material, and a uniform and compact interface and matrix formed by a polymer impregnation cracking (PIP) process and/or a Chemical Vapor Infiltration (CVI) process are used for protecting the fiber in the fiber preform, so that the ceramic matrix composite material can cooperatively absorb waves at room temperature/high temperature, and the problem of attenuation of the high-temperature wave-absorbing property of the ceramic matrix composite material is solved.
4. The ceramic matrix composite material with the three-dimensional gradient periodic structure solves the problem that the traditional ceramic matrix Composite Material (CMC) has narrow wave absorption frequency band; the molding difficulty of the periodic wave-absorbing structure in the broadband wave-absorbing CMC is high; the low-frequency and broadband wave-absorbing CMC has large thickness and the like. The three-dimensional gradient periodic structure ceramic matrix composite material can effectively attenuate electromagnetic waves in a wide frequency range on the premise of keeping the mechanical properties of the ceramic matrix composite material, has excellent wide-frequency wave absorbing performance under the condition of thinner thickness, and provides a new idea for integrated design and preparation of high-temperature bearing wide-frequency wave absorbing ceramic matrix composite materials for aerospace.
Drawings
FIG. 1 is a flow chart of a preparation process of a ceramic matrix composite material with a three-dimensional gradient periodic structure;
FIG. 2 is a graph showing the wave-absorbing performance of the ceramic matrix composite with the three-dimensional gradient periodic structure prepared in example 1 at 4-40 GHz;
FIG. 3 is a graph showing the wave-absorbing performance of the ceramic matrix composite with the three-dimensional gradient periodic structure prepared in example 2 at 4-40 GHz;
FIG. 4 is a graph showing the wave-absorbing performance of the ceramic matrix composite with the three-dimensional gradient periodic structure prepared in example 3 at 4-40 GHz.
Detailed Description
A three-dimensional gradient periodic structure ceramic matrix composite and a method for preparing the same according to the present invention will be described below with reference to examples.
This invention may, however, be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein, but rather should be construed in order that the invention will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
Examples
Example 1
The preparation method of the ceramic matrix composite with the three-dimensional gradient periodic structure comprises the following steps:
step 1, simulating the thickness of a dielectric layer and the size and distribution of a wave absorbing unit of a gradient periodic structure by adopting electromagnetic simulation software (namely HFSS software) according to the dielectric constant, the loss value and the conductivity of conductive fibers of the dielectric layer; wherein the dielectric layer is Al 2 O 3 The fiber cloth is characterized in that the conductive fibers are carbon fibers, and the conductivity of the carbon fibers is 10 5 S/m。
In simulation, the dielectric constant of the dielectric layer is set to 5.5, the loss value is set to 0.05, and the conductivity of the conductive fiber is 10 5 S/m, and finally simulating to obtain a gradient periodic structure wave absorbing unit with 7 layers of carbon fiber stacks, gradually decreasing from top to bottom and in a square ring, wherein the wave absorbing unit is three-dimensionalGradient structure.
Step 2, simulating the thickness of the dielectric layer to Al according to the step 1 2 O 3 Cutting the fiber cloth, and then cutting the cut Al 2 O 3 The fiber cloth is heat treated in air at 550 ℃ for 5 hours, and sizing agent on the surface of the fiber is removed.
Step 3, in-situ forming the carbon fiber according to the size and distribution of the gradient periodic structure wave absorbing unit simulated in the step 1, and processing the carbon fiber in the step 2 to obtain Al 2 O 3 And (5) obtaining a fiber preform on the fiber cloth.
Step 4, densifying the fiber preform, including the following steps:
step S1, placing a fiber preform in a deposition furnace, vacuumizing, introducing mixed gas consisting of argon, hydrogen, silicon tetrachloride and ammonia into the deposition furnace, and reacting the silicon tetrachloride with the ammonia at 800 ℃ to generate Si in gaps of the fiber preform 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the volume ratio of silicon tetrachloride, ammonia, argon and hydrogen in the mixed gas is as follows: 1:1:5:7;
step S2, placing the fiber preform treated in the step S1 into a mixture containing polysiloxane under vacuum condition for soaking for 0.5h, wherein the mixture consists of polysiloxane and toluene; then in nitrogen atmosphere, curing at 200 ℃ for 2 hours, then cracking at 900 ℃ for 2 hours, generating SiOC in gaps of the fiber preform treated in the step S1 in the cracking process, and obtaining Al 2 O 3f /Si 3 N 4 -SiOC composite material;
repeating the step 4 until Al 2 O 3f /Si 3 N 4 The porosity of the SiOC composite is less than 10%, finally obtaining Al with a thickness of 9mm 2 O 3f /Si 3 N 4 SiOC composite material.
Example 2
Step 1, simulating the thickness of a dielectric layer and the size and distribution of a wave absorbing unit of a gradient periodic structure by adopting electromagnetic simulation software (namely HFSS software) according to the dielectric constant, the loss value and the conductivity of conductive fibers of the dielectric layer; wherein the dielectric layer is Al 2 O 3 The fiber cloth is characterized in that the conductive fibers are carbon fibers, and the conductivity of the carbon fibers is 10 5 S/m。
In simulation, the dielectric constant of the dielectric layer is set to 6, the loss value is set to 0.2, and the conductivity of the conductive fiber is 10 5 S/m, and finally simulating to obtain a gradient periodic structure wave-absorbing unit which is 4 layers of carbon fiber stacks, gradually decreases from top to bottom and is in a circular ring shape, wherein the wave-absorbing unit is in a three-dimensional gradient structure.
Step 2, simulating the thickness of the dielectric layer to Al according to the step 1 2 O 3 Cutting the fiber cloth, and then cutting the cut Al 2 O 3 The fiber cloth is heat treated in the air at 600 ℃ for 5 hours, and the sizing agent on the surface of the fiber is removed.
Step 3, in-situ forming the carbon fiber according to the size and distribution of the gradient periodic structure wave absorbing unit simulated in the step 1, and processing the carbon fiber in the step 2 to obtain Al 2 O 3 And (5) obtaining a fiber preform on the fiber cloth.
Step 4, densifying the fiber preform, including the following steps:
step S1, placing a fiber preform in a deposition furnace, vacuumizing, introducing mixed gas consisting of argon, hydrogen, silicon tetrachloride and ammonia into the deposition furnace, and reacting the silicon tetrachloride with the ammonia at 800 ℃ to generate Si in gaps of the fiber preform 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Wherein the volume ratio of silicon tetrachloride, ammonia, argon and hydrogen in the mixed gas is as follows: 1:1:7:7;
step S2, placing the fiber preform treated in the step S1 into a mixture containing polysiloxane for soaking for 1h under the vacuum condition, wherein the mixture consists of polysiloxane and dimethylbenzene; then in nitrogen atmosphere, curing at 200 ℃ for 2 hours, then cracking at 900 ℃ for 2 hours, generating SiOC in the gaps of the fiber preform treated in the step S1 in the cracking process, and obtaining Al 2 O 3f /Si 3 N 4 SiOC composite material.
Repeating the step 4 until Al 2 O 3f /Si 3 N 4 The porosity of the SiOC composite is less than 10%, finally Al with a thickness of 3.5mm is obtained 2 O 3f /Si 3 N 4 SiOC composite material.
Example 3:
step 1, simulating the thickness of a dielectric layer and the size and distribution of a wave absorbing unit of a gradient periodic structure by adopting electromagnetic simulation software (namely HFSS software) according to the dielectric constant, the loss value and the conductivity of conductive fibers of the dielectric layer; wherein the dielectric layer is Al 2 O 3 The fiber cloth is characterized in that the conductive fibers are carbon fibers, and the conductivity of the carbon fibers is 10 4 S/m。
In simulation, the dielectric constant of the dielectric layer is set to 6.5, the loss value is set to 0.1, and the conductivity of the conductive fiber is 10 4 S/m, and finally simulating to obtain a gradient periodic structure wave-absorbing unit which is 5 layers of carbon fiber stacks, gradually decreases from top to bottom and is in an equilateral triangle shape, wherein the wave-absorbing unit is in a three-dimensional gradient structure.
Step 2, simulating the thickness of the dielectric layer to Al according to the step 1 2 O 3 Cutting the fiber cloth, and then cutting the cut Al 2 O 3 The fiber cloth is heat treated in the air at 600 ℃ for 6 hours, and the sizing agent on the surface of the fiber is removed.
Step 3, molding the carbon fiber into Al after being processed in the step 2 according to the size and the distribution of the gradient periodic structure wave absorbing unit simulated in the step 1 2 O 3 And (5) obtaining a fiber preform on the fiber cloth.
Step 4, performing densification treatment on the fiber preform, placing the fiber preform in a deposition furnace, vacuumizing, introducing mixed gas consisting of argon, hydrogen, silicon tetrachloride and ammonia into the deposition furnace, and reacting the silicon tetrachloride with the ammonia at 800 ℃ to generate Si at gaps and surfaces of the fiber preform 3 N 4 Finally obtain Al 2 O 3f /Si 3 N 4 The composite material comprises silicon tetrachloride, ammonia, argon and hydrogen in the mixed gas in the volume ratio of: 1:1:6:8.
Repeating the step 4 until Al 2 O 3f /Si 3 N 4 The porosity of the composite material is less than 10 percent, and finally Al with the thickness of 5.9mm is obtained 2 O 3f /Si 3 N 4 A composite material.
Test analysis:
the composite materials prepared in examples 1 to 3 were subjected to test analysis, and the test results are shown in fig. 2 to 4, respectively.
FIG. 2 shows the Al prepared in example 1 2 O 3f /Si 3 N 4 -graph of the wave absorbing properties of SiOC composite material at 4-40 GHz; as can be seen from fig. 2, the minimum reflection coefficient of the composite material is-30 dB, the absorption bandwidth with the reflection coefficient smaller than-8 dB reaches 30GHz, and the average reflection coefficient of 4-40GHz is-10.2 dB, so that the composite material shows excellent ultra-wideband wave absorbing performance.
FIG. 3 is Al prepared in example 2 2 O 3f /Si 3 N 4 -the wave absorbing performance curve of SiOC composites at 4-40 GHz. As can be seen from FIG. 3, the minimum reflection coefficient of the composite material is-46 dB, the absorption bandwidth with the reflection coefficient smaller than-5 dB reaches 34GHz, the absorption bandwidth with the reflection coefficient smaller than-8 dB reaches 21GHz, the average reflection coefficient of 4-40GHz reaches-10.29 dB, and the composite material shows excellent ultra-wideband wave absorbing performance and has thinner sample thickness (3.5 mm).
FIG. 4 is Al prepared in example 3 2 O 3f The wave absorbing performance curve of the SiCN composite material at 4-40 GHz; as can be seen from FIG. 4, the minimum reflection coefficient of the composite material is-28 dB, the absorption bandwidth with the reflection coefficient smaller than-5 dB reaches 17GHz, and the average reflection coefficient of 4-40GHz is-7.8 dB.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The preparation method of the ceramic matrix composite with the three-dimensional gradient periodic structure is characterized by comprising the following steps of:
step 1, simulating the thickness of a medium layer and the size and distribution of a wave absorbing unit of a gradient periodic structure by adopting electromagnetic simulation software, wherein the medium layer is wave-transmitting fiber cloth;
step 2, cutting the wave-transparent fiber cloth according to the thickness of the medium layer simulated in the step 1, and oxidizing the cut wave-transparent fiber cloth to remove impurities on the wave-transparent fiber cloth;
step 3, forming conductive fiber cloth on the wave-transmitting fiber cloth processed in the step 2 in situ according to the size and the distribution of the wave-absorbing unit of the gradient periodic structure simulated in the step 1, so as to obtain a fiber preform;
and 4, densifying the fiber preform, and generating a ceramic matrix in the fiber preform to prepare the ceramic matrix composite material with the three-dimensional gradient periodic structure.
2. The method of claim 1, wherein the wave-transparent fiber has a dielectric constant of 6 or less.
3. The method according to claim 1, wherein the oxidizing conditions of the wave-transparent fiber cloth in step 2 are as follows: air atmosphere, temperature 500-600 deg.c and oxidation time 5-6 hr.
4. The method according to claim 1, wherein the conductive fiber cloth has an electrical conductivity of 10 3 ～10 6 S/m.
5. The method of claim 1, wherein the ceramic matrix in step 4 has a dielectric constant of less than 10.
6. The method according to claim 5, wherein the ceramic matrix is SiOC, si 3 N 4 At least one of SiCN and SiBCN.
7. The method according to claim 6, wherein the densification process in step 4 comprises: a polymer impregnation pyrolysis process and/or a chemical vapor infiltration process;
the polymer impregnation cracking process comprises the following steps: immersing the fiber preform or the fiber preform treated by the chemical vapor infiltration process into a mixture of a ceramic precursor, and then sequentially curing and cracking in an inert atmosphere to generate a ceramic matrix;
the chemical vapor infiltration process comprises the following steps: placing the fiber preform or the fiber preform treated by the polymer impregnation cracking process into a mixed gas containing silicon tetrachloride and ammonia gas, and generating Si at 800-1100 DEG C 3 N 4 A substrate.
8. The method according to claim 7, wherein,
the ceramic precursor is polysiloxane, polysilazane or polysilabozane;
the dipping conditions are as follows: immersing for 0.5-1 h in vacuum or pressurized to 0.8-1 Mpa;
the curing conditions are as follows: solidifying for 1-2 h at 200-300 ℃;
the cracking conditions are as follows: cracking for 2-3 h at 900-1000 ℃;
the inert atmosphere is: nitrogen or argon;
the mixed gas also comprises argon and hydrogen; the volumes of silicon tetrachloride, ammonia, hydrogen and argon in the mixed gas are as follows: 1-1.5:1-1.5:5-8:5-8.
9. The three-dimensional gradient periodic structure ceramic matrix composite material prepared according to any one of claims 1 to 8.
10. The three-dimensional gradient periodic structure ceramic matrix composite of claim 9, wherein the porosity of the three-dimensional gradient periodic structure ceramic matrix composite is less than 10%;
the wave absorbing units of the gradient periodic structure in the composite material are in gradient distribution along the lamination direction of the conductive fiber cloth;
the area of the conductive fiber cloth of the wave absorbing unit of the gradient periodic structure in the composite material is gradually decreased from top to bottom in the lamination process, so that a three-dimensional gradient structure is formed.
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