CN116606155A - Wave-absorbing ceramic matrix composite material with three-dimensional prism periodic structure and preparation method thereof - Google Patents
Wave-absorbing ceramic matrix composite material with three-dimensional prism periodic structure and preparation method thereof Download PDFInfo
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- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 69
- 239000000463 material Substances 0.000 title abstract description 28
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 93
- 239000000919 ceramic Substances 0.000 claims abstract description 31
- 239000011159 matrix material Substances 0.000 claims abstract description 29
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 26
- 230000008569 process Effects 0.000 claims description 17
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000005336 cracking Methods 0.000 claims description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 13
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 10
- 230000008595 infiltration Effects 0.000 claims description 10
- 238000001764 infiltration Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 9
- 239000004917 carbon fiber Substances 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 9
- 229920000642 polymer Polymers 0.000 claims description 9
- 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 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
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- 239000005049 silicon tetrachloride Substances 0.000 claims description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
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- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 238000004088 simulation Methods 0.000 claims description 5
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- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 239000012700 ceramic precursor Substances 0.000 claims description 4
- 239000003085 diluting agent Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- -1 polysiloxane Polymers 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- 239000012495 reaction gas Substances 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 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 claims description 2
- 229910052863 mullite Inorganic materials 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 229920001709 polysilazane Polymers 0.000 claims description 2
- 238000010008 shearing Methods 0.000 claims description 2
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000000197 pyrolysis 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
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Abstract
The invention discloses a three-dimensional prism periodic structure wave-absorbing ceramic matrix composite and a preparation method thereof, wherein the ceramic matrix composite comprises a dielectric layer, a wave-absorbing unit formed on the dielectric layer in situ, and a ceramic matrix filled in gaps between the dielectric layer and the wave-absorbing unit; the wave absorbing unit is formed by stacking conductive fibers and is in a three-dimensional prismatic shape. The invention provides a discrete periodic wave-absorbing unit of a three-dimensional prism periodic structure, which is formed in situ on ceramic fiber cloth (namely a dielectric layer) with a certain thickness, wherein a ceramic matrix is filled in a gap between the dielectric layer and the wave-absorbing unit, and finally, the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material with the porosity less than 10% is obtained; the ceramic matrix composite material effectively improves the ultra-wideband wave absorbing performance of the ceramic matrix composite material at 4-18GHz, and solves the bottleneck problem of low-frequency and wideband wave absorbing of the ceramic matrix composite material.
Description
Technical Field
The invention relates to the technical field of bearing wave-absorbing ceramic matrix composite materials, in particular to a wave-absorbing ceramic matrix composite material with a three-dimensional prism periodic structure 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. Currently, in order to improve the high-temperature broadband wave absorbing performance of CMC, multi-layer impedance matching design and surface periodic structure design are mostly adopted.
Prior art "patent number CN112939619B, patent name: the elevator degree distribution silicon carbide fiber reinforced ceramic-based ultra-wideband wave-absorbing composite material comprises a first high-resistance silicon carbide fiber reinforced ceramic-based composite material layer, a first high-resistance silicon carbide fiber array reinforced ceramic-based composite material layer, a second high-resistance silicon carbide fiber array reinforced ceramic-based composite material layer, a third high-resistance silicon carbide fiber array reinforced ceramic-based composite material layer and a fourth high-resistance silicon carbide fiber reinforced ceramic-based composite material layer in sequence; the consumed silicon carbide fiber array is formed by two-dimensional fiber cloth patch units which are arranged in a periodic array, the periodic units are the same in size, the patch sizes are sequentially increased, and the sheet resistances are sequentially reduced; the technology obtains excellent wave absorbing performance in the 3-40 GHz wave band.
Prior art "patent number CN115190756a, patent name: a three-dimensional lattice structure high-temperature wave-absorbing material and a preparation method thereof are disclosed, wherein the wave-absorbing material sequentially comprises a continuous fiber reinforced ceramic matrix composite lower panel, a three-dimensional loss type continuous silicon carbide fiber reinforced ceramic matrix composite lattice structure and a high-resistance type continuous silicon carbide fiber reinforced ceramic matrix composite panel from bottom to top. The three-dimensional lattice structure high-temperature wave absorbing material in the technology has excellent broadband wave absorbing performance, and the wave absorbing frequency band covers 1-18 GHz.
Although the multi-layer design and the surface periodic structure in the prior art can effectively improve the broadband wave absorbing performance of the material, the requirements on the electrical performance of the dielectric layer and the absorption layer are high, the thickness and the electrical performance of each layer need to be strictly controlled, and the combination of the absorption layer and the dielectric layer can influence the interlayer combination property and the integrity of the composite material.
Therefore, the method can solve the problems that the traditional Ceramic Matrix Composite (CMC) has a narrow wave absorption frequency band and a periodic structure wave absorption unit in the CMC is difficult to form, and has important academic research and application demand values.
Disclosure of Invention
In order to solve the problems that the wave absorption frequency band of the traditional ceramic matrix composite is narrow and the molding difficulty of a periodic structure wave absorption unit in CMC is high, one of the purposes of the invention is to provide a three-dimensional prism periodic structure wave absorption ceramic matrix composite.
The technical scheme for solving the technical problems is as follows:
a three-dimensional prism periodic structure wave-absorbing ceramic matrix composite comprises a dielectric layer, a periodic structure wave-absorbing unit formed on the dielectric layer in situ, and a ceramic matrix filled in gaps of the dielectric layer and the periodic structure wave-absorbing unit; the periodic structure wave absorbing unit is formed by stacking conductive fibers and is in a three-dimensional prismatic shape.
Based on the technical scheme, the invention can also be improved as follows:
further, the dielectric layer is continuous ceramic fiber with a dielectric constant less than or equal to 6, the ceramic matrix is a ceramic matrix with a dielectric constant less than 10, and the conductivity of the conductive fiber is 10 3 ～10 6 S/m. Preferably, the continuous ceramic fiber in the invention mainly refers to continuous ceramic fiber with medium and low loss and dielectric constant less than or equal to 6; the ceramic matrix mainly refers to a medium-low loss ceramic matrix with a dielectric constant less than 10.
Further, the continuous ceramic fiber comprises Al 2 O 3 Fiber, si 3 N 4 Fibers, siO 2 At least one of a fiber, mullite fiber and SiC fiber.
Further, the ceramic matrix comprises SiOC, si 3 N 4 、SiCN、SiBCN、SiO 2 And Al 2 O 3 At least one of them.
Further, the conductive fibers include carbon fibers or silicon carbide fibers.
Further, the porosity of the ceramic matrix composite is less than 10%.
The second object of the invention is to provide a preparation method of the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material, which comprises the following steps:
step 1, simulating the thickness of a dielectric layer and the size and distribution of a periodic structure wave absorbing unit by adopting electromagnetic simulation software;
step 2, shearing the dielectric layer into a required size according to the simulation of the step 1, and then carrying out oxidation treatment to remove the sizing agent on the surface of the dielectric layer;
step 3, conducting fibers are formed on the dielectric layer in situ according to the size and the distribution of the wave absorbing units with the simulated periodic structures in the step 1, and a fiber preform containing the wave absorbing units with the three-dimensional prism periodic structures is prepared;
and 4, preparing a ceramic matrix in the fiber preform obtained in the step 3 by adopting a chemical vapor infiltration process and/or a polymer impregnation cracking process, and repeating the step 4 until the porosity of the finally obtained ceramic matrix composite is less than 10%.
Further, the chemical vapor infiltration process comprises the steps of: placing the fiber preform or the fiber preform treated by the polymer impregnation cracking process into a deposition furnace, vacuumizing to a pressure less than 300Pa, introducing diluent gas and reaction gas into the deposition furnace at 800-1100 ℃, and generating a ceramic matrix through chemical reaction; wherein the diluent gas comprises argon or hydrogen, and the reaction gas comprises silicon tetrachloride and ammonia.
Further, the polymer impregnation pyrolysis process comprises the steps of: firstly, dissolving a ceramic precursor in an organic solvent to form a mixture, putting a fiber preform or the fiber preform treated by a chemical vapor infiltration process into the mixture, then, continuously carrying out vacuum or pressurization to 0.8-1 Mpa for 0.5-1 h, and finally, sequentially carrying out curing and cracking in an inert atmosphere to prepare a ceramic matrix;
the organic solvent comprises dimethylbenzene or methylbenzene, the ceramic precursor comprises any one of polysiloxane, polysilazane and polysilborazine, the inert atmosphere is nitrogen or argon, the curing condition is 200-300 ℃ for curing for 1-2 h, and the cracking condition is 800-1000 ℃ for cracking for 2-3 h.
Further, the conditions of the oxidation treatment in step 2 are: and heat-treating in 500-600 deg.c air for 5-6 hr.
The invention has the following beneficial effects:
1. the invention provides a three-dimensional prism periodic structure wave-absorbing unit formed in situ on a medium-low loss ceramic fiber cloth (medium layer) with a certain thickness, and a ceramic matrix is filled in a gap between the medium layer and the periodic structure wave-absorbing unit, so that a three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material with a porosity of less than 10% is finally obtained; the ceramic matrix composite material with the three-dimensional prism periodic structure effectively improves the ultra-wideband wave-absorbing performance of the ceramic matrix composite material at 4-18GHz, and solves the bottleneck problem of low-frequency and wideband wave-absorbing of the ceramic matrix composite material; and according to subsequent test analysis, the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material has smaller reflection coefficient, and the absorption bandwidth of the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material in the range of 4-18GHz is almost lower than-5 dB.
In addition, the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite can effectively attenuate electromagnetic waves in a wider frequency range on the premise of keeping the mechanical properties of the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite, and the broadband wave-absorbing properties of CMC are obviously improved under the condition of thinner thickness, thus providing a new idea for the integrated design and preparation of the high-temperature bearing broadband wave-absorbing ceramic matrix composite for aerospace.
2. The invention provides a method for preparing uniform and compact interfaces and matrixes by adopting conductive fiber bundles to form a discrete periodic structure wave absorbing unit on a middle-low-loss ceramic fiber cloth in situ and adopting a Chemical Vapor Infiltration (CVI) process and/or a Polymer Impregnation Pyrolysis (PIP) process, so that the original structure of the fiber and the integrity of the original structure of the fiber are cooperatively protected, the wave absorbing and mechanical properties of a ceramic matrix composite material are further improved, and the difficult problem that the ceramic matrix composite material is difficult to be compatible with radar stealth is solved.
3. The invention provides a discrete periodic structure wave-absorbing unit (namely, the periodic structure wave-absorbing units are discontinuously and non-coincidently arranged on a dielectric layer) manufactured by adopting conductive fibers (such as carbon fibers) with stable high-temperature electrical property and thermal property, and meanwhile, a uniform and compact interface and a matrix (namely, a ceramic matrix) are used for protecting the fibers; therefore, the invention avoids the problem that the conductivity of the conductive fiber can be increased along with the temperature rise, thereby causing the electrical property of the ceramic matrix composite to be too high and finally causing the reduction of the wave absorbing property; therefore, the invention realizes the cooperative wave absorption of the ceramic matrix composite in the room/high temperature, and solves the problem of the attenuation of the high-temperature wave absorption performance of the ceramic matrix composite.
4. The three-dimensional prism periodic structure wave-absorbing material adopts the conductive fiber as the discrete periodic structure wave-absorbing unit, has the advantages of strong designability, various forms, easy molding, no damage to the reinforcement fiber cloth and the like, can realize the integrated preparation of the low-frequency and broadband wave-absorbing ceramic matrix composite under the condition of thinner thickness, and solves the problem of high molding difficulty of the periodic wave-absorbing structure in the broadband wave-absorbing CMC in the prior art.
5. The discrete periodic structure wave-absorbing unit in the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material has the advantages of simple molding process, short preparation period, wide wave-absorbing frequency band and excellent mechanical property, and is a very potential broadband wave-absorbing ceramic matrix composite material.
Drawings
FIG. 1 is a schematic diagram of a three-dimensional prism periodic structure wave-absorbing unit according to the present invention;
FIG. 2 is a graph showing the wave absorbing performance of a ceramic matrix composite material with triangular prism-shaped wave absorbing units with three-dimensional prism periodic structures in the 4-18GHz frequency band;
FIG. 3 is a graph showing the wave absorbing performance of a ceramic matrix composite material with a triangular prism-shaped wave absorbing unit with a three-dimensional prism periodic structure in the 4-18GHz frequency band;
FIG. 4 is a graph showing the wave absorbing performance of a ceramic matrix composite material with hexagonal prism shaped wave absorbing units in the 4-18GHz frequency band.
Detailed Description
A three-dimensional prism periodic structure wave-absorbing 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
A preparation method of a three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material comprises the following steps:
step 1, al with low loss 2 O 3 The fiber cloth is used as a medium layer, and electromagnetic simulation software (namely HFSS software) is adopted to simulate the thickness of the medium layer and the size and distribution of the triangular prism periodic structure wave absorbing units; the dielectric constant of the dielectric layer is set to 5.8, the loss value is set to 0.2 in simulation, and the conductivity is set to 10 5 S/m carbon fiber is used as a wave absorbing unit to simulate electromagnetic performance, and finally the simulated wave absorbing unit structure is as follows: two layers of triangles and are triangular prism-shaped.
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 put into a box-type furnace, and is heat treated for 5 hours in air with the temperature of 550 ℃ to remove sizing agent on the surface of the fiber.
Step 3, forming the carbon fiber in situ on Al after the treatment of the step 2 according to the wave-absorbing unit structure simulated in the step 1 2 O 3 Fiber cloth for preparing Al containing triangular prism periodic structure wave absorbing unit 2 O 3 A fiber preform.
Step 4, using a polymer impregnation cracking (PIP) process to carry out the preparation of the Al obtained in the step 3 2 O 3 The fiber preform is densified by a matrix, specifically: al containing triangular prism periodic structure 2 O 3 The fiber preform was immersed in a mixture of polysiloxane and toluene and held under vacuum for 1h; then fishing out the fiber preform, curing for 1.5 hours under the condition of nitrogen atmosphere and 250 ℃, and cracking for 2 hours under the condition of nitrogen atmosphere and 950 ℃ after curing; repeating the step 4 until Al with triangular prism periodic structure wave absorbing unit is obtained 2 O 3f The porosity of the SiOC ceramic matrix composite is less than 10%, and finally Al of the triangular prism periodic structure wave absorbing unit with the thickness of 8mm is obtained 2 O 3f SiOC ceramic matrix composites.
Example 2
A preparation method of a three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material comprises the following steps:
step 1, al with low loss 2 O 3 The fiber cloth is used as a medium layer, and electromagnetic simulation software (namely HFSS software) is adopted to simulate the thickness of the medium layer and the size and distribution of the triangular prism periodic structure wave absorbing units; the dielectric constant of the dielectric layer is set to be 6, the loss value is set to be 0.2, and the conductivity is set to be 10 during simulation 5 The S/m carbon fiber is used as a wave absorbing unit to simulate electromagnetic performance, and the wave absorbing unit is finally simulated as follows: four layers of squares and in the shape of a quadrangular prism.
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 put into a box-type furnace, and is heat treated for 6 hours in the air with the temperature of 500 ℃ to remove sizing agent on the surface of the fiber.
Step 3, forming the carbon fiber in situ on Al after the treatment of the step 2 according to the wave-absorbing unit structure simulated in the step 1 2 O 3 Fiber cloth for preparing Al containing quadrangular periodic structure wave absorbing unit 2 O 3 A fiber preform.
Step 4, adopting a Chemical Vapor Infiltration (CVI) process to perform the Chemical Vapor Infiltration (CVI) on the Al obtained in the step 3 2 O 3 The fiber preform is densified by a matrix, specifically: placing the fiber preform in a deposition furnace, vacuumizing until the vacuum degree is less than 300Pa, introducing mixed gas consisting of argon, hydrogen, silicon tetrachloride and ammonia into the deposition furnace at 800 ℃, 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; repeating the step 4 until Al with quadrangular periodic structure wave absorbing unit is obtained 2 O 3f /Si 3 N 4 The porosity of the ceramic matrix composite is less than 10%, and finally Al with a thickness of 10mm and a quadrangular periodic structure wave absorbing unit is obtained 2 O 3f /Si 3 N 4 Ceramic matrix composite。
Example 3
A preparation method of a three-dimensional prism periodic structure wave-absorbing ceramic matrix composite material comprises the following steps:
step 1, al with low loss 2 O 3 The fiber cloth is used as a medium layer, and electromagnetic simulation software (namely HFSS software) is adopted to simulate the thickness of the medium layer and the size and distribution of the hexagonal prism periodic structure wave absorbing units; the dielectric constant of the dielectric layer is set to 5.5, the loss value is set to 0.25 during simulation, and the conductivity is set to 10 5 The S/m carbon fiber is used as a wave absorbing unit to simulate electromagnetic performance, and the wave absorbing unit is finally simulated as follows: three layers of regular hexagons and in the shape of a six-prism.
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 Placing the fiber cloth into a box-type furnace, performing heat treatment for 5 hours in the air at 600 ℃, and removing sizing agent on the surface of the fiber.
Step 3, forming the carbon fiber in situ on Al after the treatment of the step 2 according to the wave-absorbing unit structure simulated in the step 1 2 O 3 Fiber cloth for preparing Al containing hexagonal prism periodic structure wave absorbing unit 2 O 3 A fiber preform.
Step 4, combining Chemical Vapor Infiltration (CVI) with polymer impregnation cracking (PIP) to obtain Al in step 3 2 O 3 The fiber preform is densified by a matrix, specifically:
firstly, placing a fiber preform in a deposition furnace, vacuumizing until the vacuum degree is less than 300Pa, introducing mixed gas consisting of argon, hydrogen, silicon tetrachloride and ammonia into the deposition furnace at 800 ℃, 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;
then immersing the fiber preform subjected to CVI treatment into a mixture formed by polysiloxane and toluene, and maintaining the mixture for 1h under the condition of vacuum; then fishing out the fiber preform, curing for 1.5 hours under the condition of nitrogen atmosphere and 250 ℃, and cracking for 2 hours under the condition of 950 ℃ in the nitrogen atmosphere after curing;
repeating the step 4 until Al with hexagonal prism periodic structure wave-absorbing structure is obtained 2 O 3f /Si 3 N 4 The porosity of the SiOC ceramic matrix composite is less than 10%, and finally Al with a hexagonal prism periodic structure wave-absorbing unit with a thickness of 7mm is obtained 2 O 3f /Si 3 N 4 SiOC ceramic matrix composites.
Test analysis:
the composite materials (Al) of the periodic structure-free wave-absorbing units of example 1, example 2, example 3 2 O 3 SiOC composite material), the test results of which are shown in fig. 2, 3 and 4, respectively.
Wherein, FIG. 2 is a graph showing the wave absorbing performance results of the ceramic matrix composite material prepared in example 1 and the composite material without the periodic structure wave absorbing unit; as can be seen from fig. 2, the reflection coefficient of the composite material of the wave absorbing unit without the periodic structure is about-1 dB; by introducing the triangular prism periodic structure wave absorbing unit, the wave absorbing performance is improved, the minimum reflection coefficient can reach minus 32dB, and the absorption bandwidth in the range of 4-18GHz is almost lower than minus 5dB.
FIG. 3 is a graph showing the results of the wave absorbing performance of the ceramic matrix composite and the composite without the periodic structure wave absorbing unit prepared in example 2; as can be seen from fig. 3, the reflection coefficient of the composite material of the wave absorbing unit without the periodic structure is about-1 dB; by introducing the quadrangular periodic structure wave absorbing unit, the wave absorbing performance is improved, the minimum reflection coefficient can reach-17 dB, and the absorption bandwidth in the range of 4-18GHz is almost lower than-5 dB.
FIG. 4 is a graph showing the results of the wave absorbing performance of the ceramic matrix composite and the composite without the periodic structure wave absorbing unit prepared in example 3; as can be seen from fig. 3, the reflection coefficient of the composite material of the wave absorbing unit without the periodic structure is about-1 dB; by introducing the hexagonal prism periodic structure wave-absorbing unit, the wave-absorbing performance is improved, the minimum reflection coefficient can reach-14 dB, and the absorption bandwidth in the range of 4-18GHz is almost lower than-5 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 three-dimensional prism periodic structure wave-absorbing ceramic matrix composite is characterized by comprising a dielectric layer, a periodic structure wave-absorbing unit formed on the dielectric layer in situ and a ceramic matrix filled in gaps of the dielectric layer and the periodic structure wave-absorbing unit; the periodic structure wave absorbing unit is formed by stacking conductive fibers and is in a three-dimensional prismatic shape.
2. The three-dimensional prism periodic structure wave-absorbing ceramic matrix composite according to claim 1, wherein the dielectric layer is continuous ceramic fiber with dielectric constant less than or equal to 6, the ceramic matrix is ceramic matrix with dielectric constant less than 10, and the conductivity of the conductive fiber is 10 3 ～10 6 S/m。
3. The three-dimensional prismatic periodic structure wave absorbing ceramic matrix composite according to claim 2, wherein the continuous ceramic fibers comprise Al 2 O 3 Fiber, si 3 N 4 Fibers, siO 2 At least one of a fiber, mullite fiber and SiC fiber.
4. The three-dimensional prismatic periodic structure wave absorbing ceramic matrix composite according to claim 2, wherein the ceramic matrix comprises SiOC, si 3 N 4 、SiCN、SiBCN、SiO 2 And Al 2 O 3 At least one of them.
5. The three-dimensional prismatic periodic structure wave absorbing ceramic matrix composite of claim 2, wherein the conductive fibers comprise carbon fibers or silicon carbide fibers.
6. The three-dimensional prismatic periodic structure wave absorbing ceramic matrix composite according to any of claims 1-5, wherein the ceramic matrix composite has a porosity of less than 10%.
7. The method for preparing the three-dimensional prism periodic structure wave-absorbing ceramic matrix composite according to any one of claims 1 to 6, comprising the following steps:
step 1, simulating the thickness of a dielectric layer and the size and distribution of a periodic structure wave absorbing unit by adopting electromagnetic simulation software;
step 2, shearing the dielectric layer into a required size according to the simulation of the step 1, and then carrying out oxidation treatment to remove the sizing agent on the surface of the dielectric layer;
step 3, conducting fibers are formed on the dielectric layer in situ according to the size and the distribution of the wave absorbing units with the simulated periodic structures in the step 1, and a fiber preform containing the wave absorbing units with the three-dimensional prism periodic structures is prepared;
and 4, preparing a ceramic matrix in the fiber preform obtained in the step 3 by adopting a chemical vapor infiltration process and/or a polymer impregnation cracking process, and repeating the step 4 until the porosity of the finally obtained ceramic matrix composite is less than 10%.
8. The method of claim 7, wherein the chemical vapor infiltration process comprises the steps of:
placing the fiber preform or the fiber preform treated by the polymer impregnation cracking process into a deposition furnace, vacuumizing to a pressure less than 300Pa, introducing diluent gas and reaction gas into the deposition furnace at 800-1100 ℃, and generating a ceramic matrix through chemical reaction; wherein the diluent gas comprises argon or hydrogen, and the reaction gas comprises silicon tetrachloride and ammonia.
9. The method of claim 7, wherein the polymer impregnation cleavage process comprises the steps of:
firstly, dissolving a ceramic precursor in an organic solvent to form a mixture, immersing a fiber preform or the fiber preform treated by a chemical vapor infiltration process into the mixture, then continuously carrying out vacuum or pressurization to 0.8-1 Mpa for 0.5-1 h, and finally sequentially carrying out curing and cracking in an inert atmosphere to prepare a ceramic matrix;
the organic solvent comprises dimethylbenzene or methylbenzene, the ceramic precursor comprises any one of polysiloxane, polysilazane and polysilborazine, the inert atmosphere is nitrogen or argon, the curing condition is 200-300 ℃ for curing for 1-2 h, and the cracking condition is 800-1000 ℃ for cracking for 2-3 h.
10. The method according to claim 7, wherein the conditions of the oxidation treatment in step 2 are: and heat-treating in 500-600 deg.c air for 5-6 hr.
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| CN109413974A (en) * | 2018-11-02 | 2019-03-01 | 合肥工业大学 | A kind of multi-layer structured wave absorbing material and preparation method thereof |
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