CN113754455B - Multi-scale toughening layer structure wave-absorbing ceramic matrix composite and preparation method thereof - Google Patents

Multi-scale toughening layer structure wave-absorbing ceramic matrix composite and preparation method thereof Download PDF

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CN113754455B
CN113754455B CN202111154019.8A CN202111154019A CN113754455B CN 113754455 B CN113754455 B CN 113754455B CN 202111154019 A CN202111154019 A CN 202111154019A CN 113754455 B CN113754455 B CN 113754455B
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fiber cloth
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suction filtration
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CN113754455A (en
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罗瑞盈
崔光远
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Hubei Ruiyu Kongtian High Tech Co ltd
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Abstract

A multi-scale toughening paving structure wave-absorbing ceramic matrix composite and a preparation method thereof are disclosed, the preparation method comprises the following steps: deposition of an interface layer, introduction of a one-dimensional nano toughening phase, design of a layer structure preform, suction filtration and impregnation of the precursor, and cracking. The one-dimensional reinforcing phase is introduced in situ in the continuous fiber reinforced ceramic matrix composite, and the multistage toughening of the ceramic matrix composite is realized. The one-dimensional nano reinforcing phase is introduced through in-situ growth before the fiber preform is molded, so that the uniform distribution of the nano reinforcing phase in the ceramic matrix composite is realized while the strong binding force between the one-dimensional nano structure and the fiber is ensured, the designability of the microstructure of the composite is improved, and the preparation period is shortened. The nano wave absorbing agent is distributed in the composite material in a gradient manner by adopting a suction filtration dipping process, so that the material can be ensured to have excellent wave absorbing performance, and meanwhile, the special-shaped member can be designed and prepared by adopting a layering process to prepare the prefabricated body, so that the design requirement of the aerospace hot end member can be met.

Description

Multi-scale toughening layer structure wave-absorbing ceramic matrix composite and preparation method thereof
Technical Field
The invention relates to the field of materials, in particular to a multi-scale toughening layer structure wave-absorbing ceramic matrix composite material and a preparation method thereof.
Background
The radar stealth has important significance for improving the operational efficiency of the aerospace vehicle, and in order to meet the requirement of radar stealth performance of a hot end component of a new generation of aerospace vehicle in China, on the basis of designing a component structure, the radar stealth also provides the requirements of light weight, high strength, temperature resistance, oxidation resistance and the like for the material used by the hot end component, and meanwhile, the radar stealth has excellent wave-absorbing property, so that a wave-absorbing structure type material is urgently required to be researched and developed, has the functions of bearing and absorbing waves at the same time, and is an important development direction of the radar stealth aerospace vehicle material.
The continuous SiC fiber reinforced ceramic matrix composite has the characteristics of low density, high strength, high temperature resistance and oxidation resistance, and can be used as a hot end component material of an aerospace aircraft, so that the structural weight of the component can be greatly reduced while the reliability of the component is ensured, the thrust-weight ratio of the aircraft is improved, and in addition, the electromagnetic property of the material can be regulated and controlled through the design of the internal microstructure of the ceramic matrix composite, and the excellent wave-absorbing property of the material is realized.
The ceramic matrix composite prepared by the PIP process has the advantages of simple process, low preparation cost, low equipment requirement and the like, but the process needs a plurality of periodic dipping-cracking processes, so that the preparation period is greatly increased. In order to improve the electromagnetic wave-absorbing performance of the ceramic matrix composite, nano wave-absorbing filler can be selectively introduced into the material.
In order to further improve the mechanical property and the wave-absorbing property of the ceramic matrix composite, the one-dimensional nano material can be introduced into the material to realize multi-scale toughening of the material, the energy dissipation mechanism of the material in the loading process is increased by breaking and pulling out the one-dimensional nano material, but the addition of the one-dimensional nano filler is easy to form agglomeration in the material to influence the performance and the performance uniformity of the material. Even if the one-dimensional nano material is grown in situ in the material by adopting a chemical vapor deposition method, the one-dimensional nano material is unevenly distributed due to the distribution of pores in the prefabricated body and the difference of a gas concentration field and a temperature field in a deposition environment.
Disclosure of Invention
The invention aims to solve the defects of the prior art, so that the preparation method of the wave-absorbing ceramic matrix composite material with the multi-scale toughening layer structure is provided, the mechanical property of the composite material is improved, the excellent wave-absorbing characteristic of the material is realized, the preparation period is shortened, and the wave-absorbing structure type ceramic matrix composite material is prepared.
The invention also aims to provide the multi-scale toughened paving structure wave-absorbing ceramic matrix composite material prepared by the method.
A preparation method of a multi-scale toughening layer structure wave-absorbing ceramic matrix composite material comprises the following steps:
step 1: preparing a BN/SiC composite interface layer on the surface of the fibers in the single-layer fiber cloth layer to obtain primary fiber cloth; the single-layer fiber cloth layer takes silicon carbide fiber as a reinforcing phase, the weaving structure of the single-layer fiber cloth layer is plain weave, twill weave or satin weave, the thickness of a BN interface layer is 300-1500 nm, and the thickness of a SiC interface layer is 200-1000 nm;
step 2: introducing a catalyst into the primary fiber cloth prepared in the step 1, and growing a one-dimensional nano toughening phase on the surface of the BN/SiC composite interface layer in situ by adopting a chemical vapor deposition process to obtain secondary fiber cloth;
and step 3: laying the secondary fiber cloth obtained in the step (2) into a prefabricated body, and shaping by using a graphite mold;
and 4, step 4: and (3) densifying the preform obtained in the step (3) by adopting a suction filtration impregnation-cracking process, realizing gradient distribution of the nano carbon powder in the preform in the suction filtration impregnation process, and repeatedly densifying by adopting the suction filtration impregnation-cracking process until the weight gain rate of the preform after a single densification process is less than 1%.
In step 1, the preparation method of the BN/SiC composite interface layer specifically comprises the following steps:
placing a plurality of single-layer fiber cloth layers in a CVI deposition furnace, firstly adopting BCl3-NH3-Ar-H2Preparing a BN interface layer on the fiber surface of a single-layer fiber cloth layer by a precursor gas system, and then adopting MTS-Ar-H2Preparing a SiC interface layer on the surface of the BN interface layer;
BCl3-NH3-Ar-H2BCl in precursor gas system3And NH3The flow ratio is 1: 3-1: 5, and MTS-Ar-H2MTS with (Ar + H) in the system2) The gas flow ratio is 1: 10-1: 20.
In step 2, the catalyst is Co (NO)3)2·6H2O,Ni(NO3)2·6H2O or NiCl2·6H2And O is one of the compounds.
The step 2 is as follows: placing the primary fiber obtained in the step 1 in an ethanol solution of a catalyst for ultrasonic treatment, wherein the concentration of the ethanol solution of the catalyst is 0.2-1.0 mol/L, drying the ultrasonically treated primary fiber cloth, placing the dried primary fiber cloth in a CVI deposition furnace, and adopting MTS-Ar-H2The system grows a one-dimensional SiC nano structure MTS-Ar-H in situ in the primary fiber cloth2MTS with (Ar + H) in the system2) The gas flow ratio is 1: 40-1: 80.
The step 3 is: laying the secondary fiber cloth obtained in the step 2 layer by layer to obtain a fiber preform, clamping and shaping the preform by a graphite mold, wherein the density of the preform is 0.5-1.3 g/cm3
The shape and the size of the prefabricated body obtained by the laying in the step 3 can be designed according to the shape and the size of the component, a graphite mold is used for shaping, and air holes are formed in the surface of the graphite mold.
The single densification process comprises the whole process of suction filtration, impregnation and cracking, and specifically comprises the following steps: in the suction filtration and impregnation process, the prefabricated body clamped with the graphite mold obtained in the step 3 is placed in a suction filtration tank, after the pressure in the tank is vacuumized to be less than 100Pa, the prepared impregnation liquid is added, the impregnation liquid flows in from the upper layer of the graphite mold and flows out from the lower layer of the graphite mold, due to the filtering effect formed by the pore structure of the prefabricated body, the gradient distribution of the content of the nano carbon powder in the impregnation liquid is gradually reduced from the upper layer to the lower layer in the prefabricated body is realized, then the impregnated prefabricated body is dried and placed in a cracking furnace for cracking, the cracking temperature is 900-1300 ℃, and the heating rate is 2-5 ℃/min.
The dipping solution is a dimethylbenzene solution dissolved with nano carbon powder and a polysilazane precursor, the concentration of the nano carbon powder in the dipping solution is 0.1mol/L, and the mass fraction of the polysilazane is 20-50%.
The wave-absorbing ceramic matrix composite material with the multi-scale toughening layer structure is prepared by the method of the technical scheme.
The invention has the following excellent effects:
(1) in the invention, the one-dimensional nano material is introduced by adopting an in-situ growth method, and is firstly introduced into the single-layer fiber cloth, and then the prefabricated body is prepared. By adopting the method, the one-dimensional nano material and the fiber surface interface layer are strongly combined, the uniformity of the one-dimensional nano material in the material is realized, and the problems of agglomeration of the one-dimensional nano material and non-uniform distribution of the inside and the outside of the preform in the deposition process in the traditional process are solved.
(2) The BN/SiC composite interface is designed, the one-dimensional SiC nanowires are introduced to the surface of the interface, the BN interface and the SiC have moderate bonding strength, the realization of toughening mechanisms such as fiber extraction and crack deflection at the interface can be ensured, and the introduction of the SiC interface can protect the BN interface from being corroded by water and oxygen in the subsequent densification process and ensure the structural integrity of the BN interface. The SiC nanowires can consume energy through breakage and pulling out of the SiC nanowires in the material loading process, and fibers and a one-bit nanomaterial can cooperatively play a role in the material loading process, so that multi-scale toughening is realized, and the mechanical property and the bearing capacity of the material are improved.
(3) According to the invention, a precursor impregnation cracking method is adopted to prepare the ceramic matrix composite material, and the one-dimensional SiC nanowires are generated in situ on the interface of the fiber surface, so that the roughness of the fiber surface is greatly increased by introducing the nanowires, the wettability between the fiber surface and the impregnating solution is increased, the uniform distribution of the ceramic matrix generated after the polysilazane is cracked on the fiber surface is facilitated, meanwhile, the increase of the surface roughness enables the ceramic matrix to adsorb more impregnating solution after impregnation, the preparation cost is ensured to be low, and the preparation period is shortened.
(4) The invention adopts the suction filtration-impregnation process, and realizes the gradient distribution of the nano carbon powder in the material by utilizing the characteristics of the pore structure in the prefabricated part, so that the lower surface of the prepared composite material has better impedance matching property, and the electromagnetic wave can enter the material as much as possible. And the SiC nanowires and the high-concentration nano carbon powder in the material can realize electromagnetic loss, so that the material has good wave absorption characteristics.
Detailed Description
A preparation method of a multi-scale toughening layer structure wave-absorbing ceramic matrix composite material comprises the following specific steps:
step 1: and preparing a BN/SiC composite interface layer on the surface of the fiber in the single-layer fiber cloth layer, wherein the thickness of the BN interface layer is 300-1500 nm, and the thickness of the SiC interface layer is 200-1000 nm. The reinforcing fiber used by the single-layer fiber cloth layer is silicon carbide fiber, and the weaving structure of the fiber cloth is plain weave, twill weave or satin weave. The preparation method of the BN/SiC composite interface layer specifically comprises the following steps: placing a plurality of single-layer fiber cloth layers in a CVI deposition furnace, firstly adopting BCl3-NH3Preparing a BN interface layer, BCl on the fiber surface of the single-layer fiber cloth layer by using an-Ar-H2 precursor gas system3-NH3-Ar-H2BCl in precursor gas system3And NH3The flow ratio is 1: 3-1: 5; subsequently, preparing a SiC layer on the surface of the BN layer by adopting an MTS-Ar-H2 system, namely MTS-Ar-H2MTS with (Ar + H) in the system2) Gas flow ratio of1:10~1:20。
Step 2: introducing a catalyst into the primary fiber cloth prepared in the step 1, and growing a one-dimensional nano toughening phase on the surface of the BN/SiC composite interface layer in situ by adopting a chemical vapor deposition process to obtain the secondary fiber cloth. The catalyst is Co (NO)3)2·6H2O,Ni(NO3)2·6H2O or NiCl2·6H2And O, arranging the primary fiber obtained in the step 1 in an ethanol solution of a catalyst for ultrasonic treatment, wherein the concentration of the ethanol solution of the catalyst is 0.2-1.0 mol/L. Drying the ultrasonic primary fiber cloth, placing the dried fiber cloth in a CVI deposition furnace, and adopting MTS-Ar-H2The system grows a one-dimensional SiC nano structure MTS-Ar-H in situ in the fiber cloth2MTS with (Ar + H) in the system2) The gas flow ratio is 1: 40-1: 80.
And step 3: and (3) laying the secondary fiber cloth obtained in the step (2) into a prefabricated body, and shaping by adopting a graphite mould, wherein the secondary fiber cloth can be in a special-shaped structure. Setting the structure of the single-layer fiber cloth obtained in the step 2 according to the external dimension of the component, laying layer by layer to obtain a fiber preform, clamping and shaping the preform by adopting a graphite mold, wherein the density of the preform is 0.5-1.3 g/cm3And the surface of the graphite mould is provided with air holes.
And 4, step 4: and (3) rapidly densifying the preform obtained in the step (3) by adopting a suction filtration impregnation-cracking process. The dipping solution is xylene solution dissolved with nano carbon powder and polysilazane precursor. One densification cycle included suction filtration impregnation and subsequent cracking. The concentration of the nano carbon powder in the impregnation liquid is 0.1mol/L, and the mass fraction of the polysilazane is 20-50%. In the suction filtration and impregnation process, the prefabricated body clamped with the graphite mold obtained in the step 3 is placed in a suction filtration tank, after the pressure in the tank is vacuumized to be less than 100Pa, the prepared impregnation liquid is added, the impregnation liquid flows in from the upper layer of the graphite mold and flows out from the lower layer of the graphite mold, due to the filtering effect formed by the pore structure of the prefabricated body, the gradient distribution of the content of the nano carbon powder in the prefabricated body is gradually reduced from the upper layer to the lower layer, then the impregnated prefabricated body is dried and placed in a cracking furnace for cracking, the cracking temperature is 900-1300 ℃, and the heating rate is 2-5 ℃/min. And repeating the suction filtration, impregnation and cracking for a plurality of cycles until the weight gain of the composite material in a single densification cycle is less than 1%.
Example 1
Step 1: preparing a BN/SiC composite interface layer on the surface of the fiber inside the single-layer silicon carbide fiber cloth layer to obtain primary fiber cloth; the single-layer fiber cloth weaving structure is a plain weave structure, the thickness of a BN interface layer is 300nm, and the thickness of a SiC interface layer is 500 nm. BN interface adopts BCl3-NH3-Ar-H2The system is prepared on the surface of the fiber, BCl3-NH3-Ar-H2BCl in precursor gas system3And NH3The flow ratio is 1:3, and the SiC interface adopts MTS-Ar-H2The system is prepared on the surface of BN layer, MTS-Ar-H2MTS with (Ar + H) in the system2) The gas flow ratio was 1: 10.
Step 2: introducing a catalyst into the primary fiber cloth prepared in the step 1, and growing a one-dimensional nano toughening phase on the surface of the BN/SiC composite interface layer in situ by adopting a chemical vapor deposition process to obtain the secondary fiber cloth. The catalyst is Co (NO)3)2·6H2And O, arranging the primary fiber obtained in the step 1 in an ethanol solution of a catalyst for ultrasonic treatment, wherein the concentration of the ethanol solution of the catalyst is 0.2 mol/L. Drying the ultrasonic primary fiber cloth, placing the dried fiber cloth in a CVI deposition furnace, and adopting MTS-Ar-H2The system grows a one-dimensional SiC nano structure MTS-Ar-H in situ in the primary fiber cloth2MTS with (Ar + H) in the system2) The gas flow ratio was 1: 80.
And step 3: laying the secondary fiber cloth obtained in the step 2 layer by layer according to a set structure to obtain a fiber preform, clamping and shaping the preform by adopting a graphite mold, wherein the density of the preform is 1.3g/cm3And the surface of the graphite mould is provided with air holes.
And 4, step 4: and (3) rapidly densifying the preform obtained in the step (3) by adopting a suction filtration impregnation-cracking process. One densification cycle included suction filtration impregnation and subsequent cracking. The concentration of the nano carbon powder in the impregnation liquid is 0.1mol/L, and the mass fraction of the polysilazane is 25%. And in the suction filtration and impregnation process, placing the prefabricated body clamped with the graphite mold obtained in the step 3 into a suction filtration tank, vacuumizing until the pressure in the tank reaches 50Pa, adding prepared impregnation liquid to realize gradient distribution of the content of the nano carbon powder in the prefabricated body gradually reduced from the upper layer to the lower layer, drying the impregnated prefabricated body, and placing the dried prefabricated body into a cracking furnace for cracking, wherein the cracking temperature is 900 ℃, and the heating rate is 5 ℃/min. And repeating the suction filtration, impregnation and cracking for a plurality of cycles until the weight gain of the composite material in a single densification cycle is less than 1%.
The prepared composite material has room temperature bending strength of at least 565 MPa.
Example 2
Step 1: preparing a BN/SiC composite interface layer on the surface of the fiber inside the single-layer silicon carbide fiber cloth layer to obtain primary fiber cloth; the single-layer fiber cloth weaving structure is a twill structure, the thickness of a BN interface layer is 1500nm, and the thickness of a SiC interface layer is 500 nm. BN interface adopts BCl3-NH3-Ar-H2The system is prepared on the surface of the fiber, BCl3-NH3-Ar-H2BCl in precursor gas system3And NH3The flow ratio is 1:3, and the SiC interface adopts MTS-Ar-H2The system is prepared on the surface of BN layer, MTS-Ar-H2MTS with (Ar + H) in the system2) The gas flow ratio was 1: 20.
Step 2: introducing a catalyst into the primary fiber cloth prepared in the step 1, and growing a one-dimensional nano toughening phase on the surface of the BN/SiC composite interface layer in situ by adopting a chemical vapor deposition process to obtain the secondary fiber cloth. The catalyst is Ni (NO)3)2·6H2And O, arranging the single-layer fiber of the primary fiber cloth obtained in the step 1 in an ethanol solution of a catalyst for ultrasonic treatment, wherein the concentration of the ethanol solution of the catalyst is 1.0 mol/L. Drying the ultrasonic primary fiber cloth, placing the dried fiber cloth in a CVI deposition furnace, and adopting MTS-Ar-H2The system grows a one-dimensional SiC nano structure MTS-Ar-H in situ in the primary fiber cloth2MTS with (Ar + H) in the system2) The gas flow ratio was 1: 40.
And step 3: laying the single-layer fiber cloth obtained in the step 2 layer by layer according to a set structure to obtain a fiber preform, clamping and shaping the preform by adopting a graphite mold, wherein the density of the preform is 0.5g/cm3What is, what isThe surface of the graphite mould is provided with air holes.
And 4, step 4: and (3) rapidly densifying the preform obtained in the step (3) by adopting a suction filtration impregnation-cracking process. One densification cycle included suction filtration impregnation and subsequent cracking. The concentration of the nano carbon powder in the impregnation liquid is 0.1mol/L, and the mass fraction of the polysilazane is 25%. And in the suction filtration and impregnation process, placing the prefabricated body clamped with the graphite mold obtained in the step 3 into a suction filtration tank, vacuumizing until the pressure in the tank reaches 50Pa, adding prepared impregnation liquid to realize gradient distribution of the content of the nano carbon powder in the prefabricated body gradually reduced from the upper layer to the lower layer, drying the impregnated prefabricated body, and placing the dried prefabricated body into a cracking furnace for cracking, wherein the cracking temperature is 1300 ℃, and the heating rate is 2 ℃/min. And repeating the suction filtration, impregnation and cracking for a plurality of cycles until the weight gain of the composite material in a single densification cycle is less than 1%.
The prepared composite material has room temperature bending strength of at least 435 MPa.
Example 3
Step 1: preparing a BN/SiC composite interface layer on the surface of the fiber inside the single-layer silicon carbide fiber cloth layer to obtain primary fiber cloth; the single-layer fiber cloth weaving structure is a satin weave structure, the thickness of a BN interface layer is 1000nm, and the thickness of a SiC interface layer is 500 nm. BN interface adopts BCl3-NH3-Ar-H2The system is prepared on the surface of the fiber, BCl3-NH3-Ar-H2BCl in precursor gas system3And NH3The flow ratio is 1:3, and the SiC interface adopts MTS-Ar-H2The system is prepared on the surface of BN layer, MTS-Ar-H2MTS with (Ar + H) in the system2) The gas flow ratio was 1: 15.
Step 2: introducing a catalyst into the primary fiber cloth prepared in the step 1, and growing a one-dimensional nano toughening phase on the surface of the BN/SiC composite interface layer in situ by adopting a chemical vapor deposition process to obtain the secondary fiber cloth. The catalyst is NiCl2·6H2And O, arranging the primary fiber obtained in the step 1 in an ethanol solution of a catalyst for ultrasonic treatment, wherein the concentration of the ethanol solution of the catalyst is 0.5 mol/L. Drying the fiber cloth after ultrasonic treatment, placing the fiber cloth in a CVI deposition furnace, and adopting MTS-Ar-H2System is fineIn-situ growth of one-dimensional SiC nanostructure, MTS-Ar-H, in wibu2MTS with (Ar + H) in the system2) The gas flow ratio was 1: 50.
And step 3: laying the secondary fiber cloth obtained in the step 2 layer by layer according to a set structure to obtain a fiber preform, clamping and shaping the preform by adopting a graphite mold, wherein the density of the preform is 1.1g/cm3And the surface of the graphite mould is provided with air holes.
And 4, step 4: and (3) rapidly densifying the preform obtained in the step (3) by adopting a suction filtration impregnation-cracking process. One densification cycle included suction filtration impregnation and subsequent cracking. The concentration of the nano carbon powder in the impregnation liquid is 0.1mol/L, and the mass fraction of the polysilazane is 25%. And in the suction filtration and impregnation process, placing the preform clamped with the graphite mold obtained in the step 3 into a suction filtration tank, vacuumizing until the pressure in the tank reaches 50Pa, adding prepared impregnation liquid to realize gradient distribution of the content of the nano carbon powder in the preform gradually reduced from the upper layer to the lower layer, drying the impregnated preform, and placing the dried preform into a cracking furnace for cracking, wherein the cracking temperature is 1100 ℃, and the heating rate is 3 ℃/min. And repeating the suction filtration, impregnation and cracking for a plurality of cycles until the weight gain of the composite material in a single densification cycle is less than 1%.
The prepared composite material has room temperature bending strength of at least 698 MPa.

Claims (4)

1. A preparation method of a multi-scale toughening layer structure wave-absorbing ceramic matrix composite is characterized by comprising the following steps: the method comprises the following steps:
step 1: preparing a BN/SiC composite interface layer on the surface of the fibers in the single-layer fiber cloth layer to obtain primary fiber cloth; the single-layer fiber cloth layer takes silicon carbide fiber as a reinforcing phase, the weaving structure of the single-layer fiber cloth layer is plain weave, twill weave or satin weave, the thickness of a BN interface layer is 300-1500 nm, and the thickness of a SiC interface layer is 200-1000 nm; the preparation method of the BN/SiC composite interface layer comprises the following steps:
placing a plurality of single-layer fiber cloth layers in a CVI deposition furnace, firstly adopting BCl3-NH3-Ar-H2Preparing BN interface layer on fiber surface of single-layer fiber cloth layer by precursor gas systemFollowed by MTS-Ar-H2Preparing a SiC interface layer on the surface of the BN interface layer;
BCl3-NH3-Ar-H2BCl in precursor gas system3And NH3The flow ratio is 1: 3-1: 5, and MTS-Ar-H2MTS with (Ar + H) in the system2) The gas flow ratio is 1: 10-1: 20;
step 2: introducing a catalyst into the primary fiber cloth prepared in the step 1, and growing a one-dimensional nano toughening phase on the surface of the BN/SiC composite interface layer in situ by adopting a chemical vapor deposition process to obtain secondary fiber cloth; the catalyst is Co (NO)3)2·6H2O,Ni(NO3)2·6H2O or NiCl2·6H2One of O;
the preparation method of the step 2 comprises the following steps: placing the primary fiber obtained in the step 1 in an ethanol solution of a catalyst for ultrasonic treatment, wherein the concentration of the ethanol solution of the catalyst is 0.2-1.0 mol/L, drying the ultrasonically treated primary fiber cloth, placing the dried primary fiber cloth in a CVI deposition furnace, and adopting MTS-Ar-H2The system grows a one-dimensional SiC nano structure MTS-Ar-H in situ in the primary fiber cloth2MTS with (Ar + H) in the system2) The gas flow ratio is 1: 40-1: 80;
and step 3: laying the secondary fiber cloth obtained in the step (2) into a prefabricated body, and shaping by using a graphite mold;
and 4, step 4: adopting a suction filtration impregnation-cracking process to densify the prefabricated body obtained in the step 3, realizing gradient distribution of the nano carbon powder in the prefabricated body in the suction filtration impregnation process, and repeating the suction filtration impregnation-cracking process to densify until the weight gain rate is less than 1% after single densification;
the single densification process comprises the whole process of suction filtration, impregnation and cracking, and specifically comprises the following steps: in the suction filtration and impregnation process, the prefabricated body clamped with the graphite mold obtained in the step 3 is placed in a suction filtration tank, the tank is vacuumized until the pressure in the tank is less than 100Pa, the prepared impregnation liquid is added, then the impregnated prefabricated body is dried and placed in a cracking furnace for cracking, the cracking temperature is 900-1300 ℃, and the heating rate is 2-5 ℃/min;
the dipping solution is a dimethylbenzene solution dissolved with nano carbon powder and a polysilazane precursor, the concentration of the nano carbon powder in the dipping solution is 0.1mol/L, and the mass fraction of the polysilazane is 20-50%.
2. The preparation method of the multi-scale toughening paving structure wave-absorbing ceramic matrix composite material according to claim 1, characterized in that: the step 3 is: laying the secondary fiber cloth obtained in the step 2 layer by layer to obtain a fiber preform, clamping and shaping the preform by a graphite mold, wherein the density of the preform is 0.5-1.3 g/cm3
3. The preparation method of the multi-scale toughened ply structure wave-absorbing ceramic matrix composite material according to claim 1 or 2, characterized in that: the shape and the size of the prefabricated body obtained by the laying in the step 3 can be designed according to the shape and the size of the component, a graphite mold is used for shaping, and air holes are formed in the surface of the graphite mold.
4. The multi-scale toughened ply structure wave-absorbing ceramic matrix composite material prepared by the method of claim 1 or 2.
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