CN114149272A - High-temperature wide-band wave-absorbing Al2O3fReinforced ceramic matrix composite material and integrated preparation method - Google Patents
High-temperature wide-band wave-absorbing Al2O3fReinforced ceramic matrix composite material and integrated preparation method Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 title abstract description 11
- 239000000835 fiber Substances 0.000 claims abstract description 100
- 239000002131 composite material Substances 0.000 claims abstract description 46
- 239000004744 fabric Substances 0.000 claims abstract description 44
- 239000011159 matrix material Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 25
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- 239000002243 precursor Substances 0.000 claims abstract description 17
- 239000011226 reinforced ceramic Substances 0.000 claims abstract description 17
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- 238000000197 pyrolysis Methods 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 37
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- 229910010271 silicon carbide Inorganic materials 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
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- 238000004513 sizing Methods 0.000 claims description 7
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- 238000000280 densification Methods 0.000 claims description 3
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- 229910052786 argon Inorganic materials 0.000 description 5
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Abstract
The invention relates to a high-temperature broadband wave-absorbing Al2O3fA reinforced ceramic matrix composite and an integrated preparation method are used for solving the technical problem that the high-temperature wave-absorbing frequency band of the existing ceramic matrix composite is narrow. The technical scheme is that Al is optimally designed through HFSS software2O3fThe wave-absorbing structure unit in the fiber prefabricated body is formed on Al by adopting a manual sewing process2O3fPreparing conductive carbon fiber with a certain periodic structure on fiber cloth, and then adopting a precursor impregnation pyrolysis method (PIP method) to prepare the conductive carbon fiber with the periodic structureAl2O3fPreparing ceramic matrix in the fiber preform to obtain the broadband wave-absorbing Al2O3fa/SiOC composite material. The method can directly carry out periodic structural design and content regulation and control on the wave-absorbing unit of the composite material, does not need to chemically synthesize a wave-absorbing agent, and has the advantages of simple preparation process, short period and no damage to the fiber of the composite material. By reacting with Al2O3fThe periodic wave absorbing unit and the wave absorbing agent of the reinforced composite material are regulated and controlled, so that the broadband wave absorbing performance of the composite material can be effectively improved, and the reinforced composite material has the potential of becoming an excellent broadband wave absorbing ceramic matrix composite material.
Description
Technical Field
The invention belongs to the technical field of bearing wave-absorbing ceramic matrix composite materials, and relates to a high-temperature broadband wave-absorbing Al2O3fA reinforced ceramic matrix composite material and an integrated preparation method.
Background
With the development of the omnibearing radar detection technology, the radar stealth problem of the hot-end part of the aircraft engine needs to be solved urgently. The fiber reinforced ceramic matrix composite has the advantages of high strength, high temperature resistance, oxidation resistance, designable electromagnetic property and the like, and has good development potential in the aspect of bearing and absorbing waves. Al (Al)2O3The fiber has the advantages of high melting point, corrosion resistance, high temperature resistance, excellent mechanical property and the like, and is a good wave-transmitting material. With Al2O3The fiber is used as a reinforcement to prepare the composite material, and excellent wave-absorbing performance can be obtained only by introducing a wave-absorbing phase and regulating and controlling the content and the structure of the wave-absorbing phase. Compared with other wave-absorbing fibers, the fiber has the advantages of simple process, short period and the like.
Document 1 "invar and worth, chuangmei, hanmeikang, etc. Al (Al)2O3fPreparation method of SiOC radar absorbing composite material, China, CN 105503229[ A ]]2015 "discloses a process for preparing Al2O3fA method for producing SiOC absorption type composite material. According to the method, a catalyst is introduced into a polysiloxane precursor, Fe element is bonded into a precursor molecular chain, and a wave absorbing agent is separated out at a low temperature. The wave absorbing performance is adjusted by controlling the content of the catalyst. The method realizes better wave-absorbing performance of the X wave band. The existing structural wave-absorbing material gradually develops towards directions of strong absorption, broadband and the like, and to obtain better broadband wave-absorbing performance, the structural wave-absorbing material is not easy to realize only by depending on the electromagnetic performance of the material, and is usually realized by introducing a periodic structure.
At present, the structural design of the wave-absorbing ceramic matrix composite material mainly takes SiC fiber as a main material. Document 2, "liuhai taotao, sun son, huangwen, etc., an elevator distribution silicon carbide fiber reinforced ceramic-based ultra-wideband wave-absorbing composite material and a preparation method thereof, and china, CN 112939619[ a ] 2021" discloses an elevator distribution silicon carbide fiber reinforced ceramic-based ultra-wideband wave-absorbing composite material and a preparation method thereof. According to the method, the periodic structure unit is etched on the two-dimensional silicon carbide cloth through a laser processing technology, and an impedance matching structure is designed, so that good broadband wave absorbing performance is obtained. However, the laser etching periodic structure has certain damage to the continuous fiber and has influence on the overall mechanical property of the composite material; and the conductivity of the SiC fiber at high temperature can be increased, which can cause impedance mismatch and reduced wave-absorbing performance.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a high-temperature broadband wave-absorbing Al2O3fThe reinforced ceramic matrix composite and the integrated preparation method improve the broadband wave-absorbing performance of the ceramic matrix composite. The method adopts HFSS software to design the broadband wave absorption performance of the composite material, and adopts wave-transparent Al2O3Discrete conductive fibers with periodic structures are formed on the fiber cloth and used as wave absorbing units, a nano wave absorbing phase modified ceramic matrix is prepared by a modified polymer impregnation pyrolysis Method (MPIP), the densification process of the matrix is optimized, and the broadband wave absorbing Al is obtained2O3fA reinforced ceramic matrix composite. The method designs and forms the composite material from a micro-mesoscopic-macroscopic scale, the structural size of the wave-absorbing unit, the structural form and content of the wave-absorbing unit, the microstructure and content of the wave-absorbing agent and the like are all controllable and adjustable, and the broadband wave-absorbing performance of the ceramic matrix composite material can be effectively improved.
Technical scheme
High-temperature broadband wave-absorbing Al2O3fThe reinforced ceramic matrix composite is characterized in that: in wave-transparent Al2O3A wave absorbing unit with a periodic structure is formed on the fiber cloth and is composed of discrete conductive fibers, and a nano wave absorbing phase modified ceramic matrix is prepared by a modified polymer impregnation pyrolysis method to obtain the broadband wave absorbing Al2O3fA reinforced ceramic matrix composite.
The high-temperature broadband wave-absorbing Al2O3fReinforced ceramic matrixThe preparation method of the composite material is characterized by comprising the following steps:
step 1: mixing Al2O3Cutting the fiber cloth into required size, putting the fiber cloth into a box type furnace, and performing heat treatment for 5-6 h in the air at 600-700 ℃ to remove the sizing agent on the surface of the fiber to obtain Al2O3Fiber cloth;
step 2: using HFSS software on Al2O3The fiber cloth is provided with a periodic wave absorbing unit, and the conductive fiber is sewed to the Al according to the designed wave absorbing unit2O3Obtaining Al containing periodic wave absorbing units on the fiber cloth2O3Fibers;
and step 3: al containing the periodic wave absorbing unit in the step 22O3Fibers and Al in step 12O3Stacking fiber cloth, and shaping to obtain wave-absorbing Al2O3A fiber preform;
and 4, step 4: taking a polymer precursor solution as an impregnation solution, and carrying out a precursor impregnation cracking process on the Al obtained in the step 32O3Impregnating, cracking and repeatedly densifying the fiber preform, and machining to a test size to obtain Al with a periodic structure2O3fReinforcing the ceramic matrix composite;
the precursor impregnation cracking process parameters are as follows: the vacuum impregnation time is not less than 1h, and the pressure is not more than-0.1 MPa; the pyrolysis temperature is 800-900 ℃, the time is not less than 2h, and the densification time is not less than 8 times.
The conductive fibers include, but are not limited to, SiC fibers or C fibers.
The polymer precursor includes, but is not limited to, silicon carbide, silicon boron carbon nitride, silicon oxygen carbon, silicon carbon nitride, or silicon boron nitrogen.
Advantageous effects
The invention provides a high-temperature broadband wave-absorbing Al2O3fA reinforced ceramic matrix composite and an integrated preparation method are used for solving the technical problem that the high-temperature wave-absorbing frequency band of the existing ceramic matrix composite is narrow. The technical scheme is that Al is optimally designed through HFSS software2O3fFiber preformThe wave-absorbing structure unit is arranged on Al by adopting a manual sewing process2O3fPreparing conductive carbon fiber with a certain periodic structure on fiber cloth, and then adopting a precursor impregnation pyrolysis method (PIP method) to prepare Al with a periodic structure2O3fPreparing ceramic matrix in the fiber preform to obtain the broadband wave-absorbing Al2O3fa/SiOC composite material. The method can directly carry out periodic structural design and content regulation and control on the wave-absorbing unit of the composite material, does not need to chemically synthesize a wave-absorbing agent, and has the advantages of simple preparation process, short period and no damage to the fiber of the composite material. By reacting with Al2O3fThe periodic wave absorbing unit and the wave absorbing agent of the reinforced composite material are regulated and controlled, so that the broadband wave absorbing performance of the composite material can be effectively improved, and the reinforced composite material has the potential of becoming an excellent broadband wave absorbing ceramic matrix composite material.
Compared with the prior art, the invention has the following beneficial effects:
1. high-temperature broadband wave-absorbing Al in the invention2O3fThe reinforced ceramic matrix composite material adopts conductive fibers as a periodic structure and is sewn on the wave-transparent Al2O3The designability among fibers is strong, the form, size and content of the wave-absorbing unit are simple and easy to adjust, and Al is treated2O3The fiber preform is not damaged and is synthesized without chemical reaction.
2. The broadband wave-absorbing performance is realized by designing the shape (square, cross, honeycomb and the like) of the periodic wave-absorbing unit, regulating and controlling the content of the conductive fiber (the size of the wave-absorbing unit, the wall thickness of the wave-absorbing unit and the like) and changing the thickness of the wave-absorbing fiber layer.
3. The ceramic matrix composite material has simple design and forming method and short preparation period, and is potential high-temperature broadband wave-absorbing Al2O3fa/SiOC composite material.
Drawings
FIG. 1 is a process flow diagram of the process of the present invention.
FIG. 2 shows the fibers C in single Al layer in examples 1 and 22O3Schematic representation of the structure on the fiber.
FIG. 3 shows Al in example 12O3fThe wave absorbing performance curve of the/SiOC composite material is 2-18 GHz.
FIG. 4 shows Al in practical example 22O3fThe wave absorbing performance curve of the/SiOC composite material is 2-18 GHz.
FIG. 5 shows Al prepared in example 12O3fthe/SiOC composite material sample.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1 was carried out:
(1) mixing Al2O3Putting the fiber cloth into a box type furnace, and carrying out heat treatment for 5-6 h in the air at the temperature of 600-700 ℃ to remove the sizing agent on the surface of the fiber;
(2) a single layer of Al2O3Cutting the fiber cloth into 200mm × 200mm, sewing C fiber on single layer Al according to the size of honeycomb wave-absorbing unit in FIG. 2a2O3On a fiber cloth, wherein the conductivity of the C fiber is about 105S/m；
(3) Al in step 22O3The upper layer and the lower layer of the fiber cloth are respectively provided with 5 layers of wave-transparent Al2O3Stacking fiber cloth into a sandwich structure, and fixing by a graphite grinding tool to obtain Al2O3A fiber preform;
(4) mixing the above Al2O3Vacuum soaking the fiber preform in a polysiloxane precursor solution for 0.5h, and cracking at 900 ℃ for 2h under the protection of inert atmosphere (argon or nitrogen) to prepare SiOC matrix to obtain broadband wave-absorbing Al2O3fa/SiOC composite material.
FIG. 3 contains Al of the present embodiment2O3fThe wave absorbing performance curve of the/SiOC composite material at 2-18GHz, wherein Al of C fiber is not added2O3fThe reflection coefficient of the/SiOC composite material is about-1 dB; by adding the C fiber, the wave absorbing performance is improved, and particularly, the minimum reflection coefficient can reach-7 dB under high frequency; FIG. 5 is a sample prepared in this example.
Example 2 was carried out:
(1) mixing Al2O3Fiber cloth is put intoCarrying out heat treatment for 5-6 h in air at 600-700 ℃ in a box type furnace to remove a sizing agent on the surface of the fiber;
(2) a single layer of Al2O3Cutting the fiber cloth into 200mm × 200mm, sewing C fiber on single layer Al according to the size of honeycomb wave-absorbing unit in FIG. 2a2O3On a fiber cloth, wherein the conductivity of the C fiber is about 105S/m；
(3) Al with the wave absorbing unit in the step 22O3The fiber cloth is arranged at the uppermost layer, and 10 layers of wave-transparent Al are stacked below the fiber cloth2O3Fiber cloth and fixing by graphite grinding tool to obtain Al2O3A fiber preform;
(4) mixing the above Al2O3Vacuum soaking the fiber preform in a polysiloxane precursor solution for 0.5h, and cracking at 900 ℃ for 2h under the protection of inert atmosphere (argon or nitrogen) to prepare SiOC matrix to obtain broadband wave-absorbing Al2O3fa/SiOC composite material.
FIG. 4 shows Al contained in the present embodiment2O3fThe wave absorbing performance curve of the/SiOC composite material at 2-18GHz, wherein Al of C fiber is not added2O3fThe reflection coefficient of the/SiOC composite material is about-1 dB; it can be seen that Al containing the wave absorbing element2O3When the fiber is arranged on the uppermost layer, the wave absorbing performance of the composite material is greatly improved, two resonance peaks appear at 8GHz and 18GHz, and the minimum reflection coefficient can reach-13 dB.
Example 3 of implementation:
(1) mixing Al2O3Putting the fiber cloth into a box type furnace, and carrying out heat treatment for 5-6 h in the air at the temperature of 600-700 ℃ to remove the sizing agent on the surface of the fiber;
(2) a single layer of Al2O3Cutting the fiber cloth into 200mm × 200mm, sewing C fiber on single layer Al according to the size of honeycomb wave-absorbing unit in FIG. 2b2O3On a fiber cloth, wherein the conductivity of the C fiber is about 105S/m；
(3) Al in step 22O3The upper layer and the lower layer of the fiber cloth are respectively provided with 5 layers of wave-transparent Al2O3Fiber cloth, stacked intoSandwich structure, and fixing with graphite grinding tool to obtain Al2O3A fiber preform;
(4) mixing the above Al2O3Vacuum soaking the fiber preform in a polysiloxane precursor solution for 0.5h, and cracking at 900 ℃ for 2h under the protection of inert atmosphere (argon or nitrogen) to prepare SiOC matrix to obtain broadband wave-absorbing Al2O3fa/SiOC composite material.
FIG. 3 contains Al of the present embodiment2O3fThe wave-absorbing performance curve of the/SiOC composite material at 2-18GHz is similar to that of the embodiment example 1.
Example 4 of implementation:
(1) mixing Al2O3Putting the fiber cloth into a box type furnace, and carrying out heat treatment for 5-6 h in the air at the temperature of 600-700 ℃ to remove the sizing agent on the surface of the fiber;
(2) a single layer of Al2O3Cutting the fiber cloth into 200mm × 200mm, sewing the C fiber on the single-layer Al according to the size of the cross wave-absorbing unit2O3On a fiber cloth, wherein the conductivity of the C fiber is about 105S/m；
(3) Al in step 22O3The upper layer and the lower layer of the fiber cloth are respectively provided with 5 layers of wave-transparent Al2O3Stacking fiber cloth into a sandwich structure, and fixing by a graphite grinding tool to obtain Al2O3A fiber preform;
(4) mixing the above Al2O3Vacuum soaking the fiber preform in a polysiloxane precursor solution for 0.5h, and cracking at 900 ℃ for 2h under the protection of inert atmosphere (argon or nitrogen) to prepare SiOC matrix to obtain broadband wave-absorbing Al2O3fa/SiOC composite material.
Example 5 was carried out:
(1) mixing Al2O3Putting the fiber cloth into a box type furnace, and carrying out heat treatment for 5-6 h in the air at the temperature of 600-700 ℃ to remove the sizing agent on the surface of the fiber;
(2) a single layer of Al2O3Cutting the fiber cloth into 200mm × 200mm, sewing SiC fiber on single layer Al according to the size of the cross wave-absorbing unit2O3FiberOn cloth, wherein the conductivity of the C fiber is about 102S/m；
(3) Al in step 22O3The upper layer and the lower layer of the fiber cloth are respectively provided with 5 layers of wave-transparent Al2O3Stacking fiber cloth into a sandwich structure, and fixing by a graphite grinding tool to obtain Al2O3A fiber preform;
(4) mixing the above Al2O3Vacuum soaking the fiber preform in a polysiloxane precursor solution for 0.5h, and cracking at 900 ℃ for 2h under the protection of inert atmosphere (argon or nitrogen) to prepare SiOC matrix to obtain broadband wave-absorbing Al2O3fa/SiOC composite material.
Claims (4)
1. High-temperature broadband wave-absorbing Al2O3fThe reinforced ceramic matrix composite is characterized in that: in wave-transparent Al2O3A wave absorbing unit with a periodic structure is formed on the fiber cloth and is composed of discrete conductive fibers, and a nano wave absorbing phase modified ceramic matrix is prepared by a modified polymer impregnation pyrolysis method to obtain the broadband wave absorbing Al2O3fA reinforced ceramic matrix composite.
2. The high-temperature broadband absorption Al of claim 12O3fThe preparation method of the reinforced ceramic matrix composite material is characterized by comprising the following steps:
step 1: mixing Al2O3Cutting the fiber cloth into required size, putting the fiber cloth into a box type furnace, and performing heat treatment for 5-6 h in the air at 600-700 ℃ to remove the sizing agent on the surface of the fiber to obtain Al2O3Fiber cloth;
step 2: using HFSS software on Al2O3The fiber cloth is provided with a periodic wave absorbing unit, and the conductive fiber is sewed to the Al according to the designed wave absorbing unit2O3Obtaining Al containing periodic wave absorbing units on the fiber cloth2O3Fibers;
and step 3: al containing the periodic wave absorbing unit in the step 22O3Fibers and Al in step 12O3FiberStacking and shaping cloth to obtain wave-absorbing Al2O3A fiber preform;
and 4, step 4: taking a polymer precursor solution as an impregnation solution, and carrying out a precursor impregnation cracking process on the Al obtained in the step 32O3Impregnating, cracking and repeatedly densifying the fiber preform, and machining to a test size to obtain Al with a periodic structure2O3fReinforcing the ceramic matrix composite;
the precursor impregnation cracking process parameters are as follows: the vacuum impregnation time is not less than 1h, and the pressure is not more than-0.1 MPa; the pyrolysis temperature is 800-900 ℃, the time is not less than 2h, and the densification time is not less than 8 times.
3. The high-temperature broadband absorption Al of claim 12O3fThe preparation method of the reinforced ceramic matrix composite material is characterized by comprising the following steps: the conductive fibers include, but are not limited to, SiC fibers or C fibers.
4. The high-temperature broadband absorption Al of claim 12O3fThe preparation method of the reinforced ceramic matrix composite material is characterized by comprising the following steps: the polymer precursor includes, but is not limited to, silicon carbide, silicon boron carbon nitride, silicon oxygen carbon, silicon carbon nitride, or silicon boron nitrogen.
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| CN116606148A (en) * | 2023-05-12 | 2023-08-18 | 西北工业大学 | Ceramic matrix composite material with three-dimensional gradient periodic structure and preparation method thereof |
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