CN109265189B - Method for rapidly preparing wave-absorbing ceramic matrix composite with electromagnetic impedance gradual change matrix - Google Patents

Method for rapidly preparing wave-absorbing ceramic matrix composite with electromagnetic impedance gradual change matrix Download PDF

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CN109265189B
CN109265189B CN201811199009.4A CN201811199009A CN109265189B CN 109265189 B CN109265189 B CN 109265189B CN 201811199009 A CN201811199009 A CN 201811199009A CN 109265189 B CN109265189 B CN 109265189B
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叶昉
殷小玮
李明星
莫然
成来飞
张立同
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Northwestern Polytechnical University
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Abstract

The invention relates to a method for rapidly preparing a wave-absorbing ceramic matrix composite material with an electromagnetic impedance gradual change matrix, which comprises the steps of firstly preparing a porous carbon matrix composite material by adopting a CVI (chemical vapor infiltration) or PIP (poly-p-phenylene oxide) process, then obtaining a C-SiC matrix composite material by adopting an RMI (reduced metal infiltration) process, and finally converting residual Si in the composite material into Si by adopting a nitriding process3N4The matrix phase composition obtained thereby is C → SiC → Si from inside to outside3N4The electromagnetic impedance matching performance with the free space is gradually improved; from outside to inside is Si3N4→ SiC → C, the ability of loss of electromagnetic wave is gradually enhanced. The invention has strong process controllability, and has short preparation period and low production cost compared with CVI and PIP methods. In the aspect of electromagnetic performance of the composite material, the impedance matching performance of the matrix material from inside to outside and the free space is gradually improved, the loss capacity of the matrix material to electromagnetic waves from outside to inside is gradually enhanced, and the wave absorbing performance of the composite material is favorably improved.

Description

Method for rapidly preparing wave-absorbing ceramic matrix composite with electromagnetic impedance gradual change matrix
Technical Field
The invention belongs to a preparation method of a ceramic matrix composite, and relates to a rapid preparation method of a wave-absorbing ceramic matrix composite with an electromagnetic impedance gradual change matrix.
Background
Ceramic matrix composites are widely used as high temperature structural materials for advanced equipment due to their good mechanical properties, thermophysical properties, environmental properties, and the like. With the development of aerospace and military science and technology, radar stealth technology becomes a key for improving the comprehensive performance of equipment, and the development of wave-absorbing ceramic matrix composite materials is imperative.
Two principles that the ceramic matrix composite material has excellent wave absorption performance are as follows: (1) matching with free space electromagnetic impedance; (2) the electromagnetic wave attenuation capability is strong. That is, when the wave impedance of the material is close to that of the free space and the electromagnetic impedance matching degree is high, the electromagnetic wave can enter the material to a large extent and then is attenuated and lost under the action of various wave absorbing mechanisms in the material. In the ceramic matrix composite, a matrix material is in direct contact with a free space, and the electromagnetic impedance matching characteristic of the matrix material and the free space and the attenuation capacity of the matrix material to electromagnetic waves directly determine the wave absorbing performance of the composite. The currently reported wave-absorbing ceramic matrix composite mainly adopts a single matrix material, and researches show that the matrix material with wave impedance similar to that of free space is generally insufficient in electromagnetic wave attenuation capability; the base material having high electromagnetic wave loss ability tends to have a large difference from the wave impedance of free space. Therefore, the ceramic matrix composite material with a single matrix has limited regulation and control of electromagnetic impedance matching performance and electromagnetic wave attenuation capability, which is not beneficial to improving the wave absorption performance of the composite material. If a base material with the internal and surface wave impedances gradually close to the free space wave impedance and the surface and internal electromagnetic wave attenuation capabilities gradually enhanced can be designed and prepared, the electromagnetic characteristics of the ceramic matrix composite material can be fundamentally changed, the two principles are cooperated, and the wave absorption performance of the composite material is effectively optimized. Meanwhile, in the densification process of the ceramic matrix composite, the commonly used Chemical Vapor Infiltration (CVI), polymer impregnation cracking (PIP) and other process periods are long, so that the preparation cost of the material is inevitably increased, and the wider application of the ceramic matrix composite is limited. Therefore, a rapid preparation method of the ceramic matrix composite material with the electromagnetic impedance gradual change matrix and excellent wave absorption performance is urgently needed to be developed.
The carbon material (C) is a commonly used high-conductivity loss material, and the wave impedance of the material is far smaller than that of a free space; silicon carbide (SiC) is a typical dielectric loss type semiconductor material, and has a wave impedance smaller than that of free space; silicon nitride (Si)3N4) The material is a well-known insulation type wave-transparent material, and the wave-starting impedance is close to the free space wave impedance. From C → SiC → Si3N4The electromagnetic impedance matching performance with the free space is gradually improved; from Si3N4→ SiC → C, the ability to lose electromagnetic waves is gradually enhanced. All three materials are excellent high temperature resistant matrix material candidates, especially for SiC and Si3N4The two materials also have excellent oxidation resistance, and can well protect the internal materials from being corroded by oxidizing atmosphere when being used as an outer layer matrix material. Xu Yongdong et al (Y.D.xu, L.F.Cheng, L.T.Zhang.carbon/silicon carbide compositions prepared by chemical vapor infiltration combining with silicon infiltration [ J.]Carbon,1999,37(8):1179-1187.) Carbon matrix was introduced into the Carbon fiber preform by PIP method, and then SiC was formed by infiltrating molten silicon into the porous Carbon matrix by Reaction Melt Infiltration (RMI). Bhatt et al (Bhatt R. mechanical properties of SiC fiber-reinforced interaction-bonded Si)3N4composites[M]// Tailoreng Multiphase and Composite ceramics. Springer US,1986:675-686.) Si in SiC fiber composites is nitrided by nitriding process to convert into Si3N4. The RMI method and the nitriding method are used for preparing SiC and Si with continuous and compact structures3N4The common method of the base material has strong process controllability, and has the advantages of short preparation period, low production cost and the like compared with the CVI method and the PIP method.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for quickly preparing a wave-absorbing ceramic matrix composite with an electromagnetic impedance gradual change matrix.
Technical scheme
A method for rapidly preparing a wave-absorbing ceramic matrix composite with an electromagnetic impedance gradual change matrix is characterized by comprising the following steps:
step 1, preparing a porous carbon-based composite material: firstly, preparing a boron nitride BN interface layer on the surface of a fiber in a preform by adopting a CVI (chemical vapor infiltration) process, and controlling the thickness of the interface layer to be 200-1500 nm by controlling the deposition time;
preparing a carbon matrix by adopting a CVI (chemical vapor infiltration) or PIP (PIP) process, and controlling the open porosity of the composite material to be about 30% by controlling the CVI deposition time or the PIP times to obtain the porous carbon-based composite material;
step 2, preparing the C-SiC-based composite material by an RMI process: placing the porous carbon-based composite material in a high-temperature vacuum furnace with the absolute pressure of 100-4000 Pa, taking Si powder as a raw material, heating to 1450-1600 ℃ at the heating rate of 3-30 ℃/min, preserving heat for 0.2-3 h, enabling Si to be molten and impregnated into pores of the porous carbon-based composite material, reacting with a carbon matrix to generate SiC, and cooling to room temperature at the cooling rate of 1-30 ℃/min to obtain the C-SiC-based composite material;
step 3, preparing Si by nitridation process3N4Matrix: putting the C-SiC-based composite material into a nitriding furnace for nitriding treatment, wherein the nitriding atmosphere is high-purity N of 0.1-0.5 MPa2Or NH3Or heating the mixed gas to 900-1100 ℃ at a heating rate of 3-30 ℃/min, then heating to 1350-1500 ℃ at a heating rate of 0.1-3 ℃/min, and preserving heat for 1-5 h; after the nitriding treatment, the residual Si on the surface layer of the composite material is converted into Si3N4Obtaining a matrix phase with the composition of carbon material → SiC → Si3N4The wave-absorbing ceramic matrix composite material is provided with an electromagnetic impedance gradient matrix; the mixed gas is N2Or NH3And H2And (3) mixing.
The fiber preform adopts a two-dimensional laminated preform, a two-dimensional semi-woven preform, a three-dimensional needling preform or a three-dimensional woven preform.
The fiber of the fiber preform adopts high-resistance SiC fiber and wave-transparent Si3N4Fibres or Al2O3A fiber.
The Si powder is an industrial raw material with the particle size of 2-100 mu m.
Advantageous effects
The invention provides a method for quickly preparing a wave-absorbing ceramic matrix composite material with an electromagnetic impedance gradual change matrix, which comprises the steps of firstly preparing a porous carbon matrix composite material by adopting a CVI (chemical vapor infiltration) or PIP (poly-p-phenylene oxide) process, then obtaining a C-SiC matrix composite material by adopting an RMI (reduced metal infiltration) process, and finally converting residual Si in the composite material by adopting a nitriding processIs Si3N4The matrix phase composition obtained thereby is C → SiC → Si from inside to outside3N4The electromagnetic impedance matching performance with the free space is gradually improved; from outside to inside is Si3N4→ SiC → C, the ability of loss of electromagnetic wave is gradually enhanced.
The invention has the beneficial effects that:
(1) the invention adopts the RMI process combined with the nitriding process to prepare the ceramic matrix composite material with continuous and compact matrix, has strong process controllability, and has the advantages of short preparation period, low production cost and the like compared with the CVI and PIP methods.
(2) The invention designs a wave-absorbing ceramic matrix composite with an electromagnetic impedance gradient matrix, wherein the matrix phase composition of the composite is C → SiC → Si from inside to outside3N4The matrix material has excellent high temperature resistance, and SiC and Si on the outer layer3N4And the coating also has excellent oxidation resistance, and is favorable for protecting the internal material from being corroded in high-temperature oxidizing atmosphere. In the aspect of electromagnetic performance, the impedance matching performance of the matrix material from inside to outside and the free space is gradually improved, the loss capacity of the matrix material to electromagnetic waves from outside to inside is gradually enhanced, and the wave absorbing performance of the composite material is favorably improved.
Drawings
FIG. 1 is a flow chart of the preparation process of the present invention
FIG. 2 is a schematic diagram of phase distribution of the composite material prepared by the present invention before and after the nitridation process
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1: a two-dimensional laminated high-resistance SiC fiber with the fiber volume fraction of 35% is used as a preform, and a uniform BN interface layer (with the thickness of 500nm) is prepared in/on the surface of the preform by a CVI method. Propylene is used as precursor gas, pyrolytic carbon is deposited on the prefabricated body with the prepared interface layer by a CVI method, the deposition temperature is 1000 ℃, the deposition time is 500 hours, and porous SiC with the open porosity of about 30 percent is preparedfa/C composite material. In the obtained SiCfComposite material tableCoating industrial silicon powder with the particle size of 10 mu m on the surface, putting the coated industrial silicon powder in a vacuum furnace with the absolute pressure of 1000Pa, heating to 1500 ℃ at the heating rate of 30 ℃/min, preserving the heat for 1h, and melting and impregnating the silicon into the porous SiCfAnd reacting the/C composite material preform with a C matrix to generate SiC, and cooling to room temperature at the speed of 10 ℃/min. The test shows that the obtained composite material has the open pore rate of 9 percent, and the composite material matrix consists of C, SiC and residual Si. Polishing and machining the composite material obtained after RMI, putting the composite material into a nitriding furnace after ultrasonic cleaning and drying, and introducing high-purity N with the pressure of 0.3MPa2Raising the temperature to 1100 ℃ at the heating rate of 5 ℃/min, then raising the temperature to 1450 ℃ at the heating rate of 2 ℃/min, preserving the temperature for 2 hours, and finally reducing the temperature to the room temperature at the cooling rate of 10 ℃/min. After the nitriding treatment, the residual Si on the surface layer of the composite material is converted into Si3N4. The final composite matrix was analyzed to be composed of C, SiC and Si3N4Composition, wherein the C content is 9 vol.%, the SiC content is 35 vol./%, and Si is3N4The content was 17 vol.%.
Example 2: adopting CVI process to obtain two-dimensional semi-permeable wave type Si with fiber volume fraction of 30%3N4A uniform BN interface layer (500 nm thickness) was prepared inside/on the surface of the fiber preform. Taking phenolic resin as an organic precursor of C, preparing a C matrix in the prefabricated body with the prepared interface layer by a PIP (poly-p-phenylene-imide) process to obtain porous Si with the open porosity of about 30 percent3N4fa/C composite material. In the obtained Si3N4fCoating industrial silicon powder with the particle size of 10 mu m on the surface of a/C composite material preform, putting the preform in a vacuum furnace with the absolute pressure of 1000Pa, heating to 1500 ℃ at the heating rate of 30 ℃/min, and preserving heat for 1h to ensure that the porous Si is infiltrated into the silicon melt3N4fAnd reacting the/C composite material preform with a C matrix to generate SiC, and cooling to room temperature at the speed of 10 ℃/min. The open porosity of the resulting composite was tested to be 12 vol.%, and the composite matrix consisted of C, SiC and residual Si. Polishing and machining the composite material obtained after RMI, putting the composite material into a nitriding furnace after ultrasonic cleaning and drying, and introducing high-purity N with the pressure of 0.2MPa2Heating to 1100 deg.C at a rate of 5 deg.C/min, and heating at a rate of 3 deg.C/minHeating to 1450 deg.C, maintaining for 2h, and cooling to room temperature at a cooling rate of 10 deg.C/min. After the nitriding treatment, the residual Si on the surface layer of the composite material is converted into Si3N4. The final composite matrix was analyzed to be composed of C, SiC and Si3N4Composition, wherein the C content is 10 vol.%, the SiC content is 32 vol./%, and Si is3N4The content was 18 vol.%.
Example 3: two-dimensional laminated transmission mode Al with fiber volume fraction of 45% by adopting CVI (chemical vapor infiltration) process2O3A uniform BN interface layer (500 nm thickness) was prepared inside/on the surface of the fiber preform. Placing the preform with the BN interface layer in a pyrolytic carbon deposition furnace, taking methane as precursor gas, preparing a pyrolytic carbon matrix at 1000 ℃ by a CVI method, and obtaining porous two-dimensional Al2O3fThe porosity of the/C composite material preform is about 35 vol.%, and the preform is subjected to ultrasonic cleaning and drying for later use. In the obtained SiCfCoating industrial silicon powder with the particle size of 20 mu m on the surface of a/PyC composite material preform, putting the preform in a vacuum furnace with the absolute pressure of 1000Pa, heating to 1500 ℃ at the heating rate of 30 ℃/min, and preserving the heat for 0.5h to ensure that porous Al is melted and impregnated by silicon2O3fAnd reacting the C/C preform with a C matrix to generate SiC, and cooling to room temperature at the speed of 10 ℃/min. The open porosity of the resulting composite was tested to be 10 vol.%, and the composite matrix consisted of C, SiC and residual Si. Polishing and machining the composite material obtained after RMI, ultrasonically cleaning and drying the composite material, putting the composite material into a nitriding furnace, and introducing high-purity H of 0.1MPa2+N2Mixed gas (H)2The flow accounts for 5 percent of the total flow of the gas), the temperature is raised to 1100 ℃ at the heating rate of 10 ℃/min, then the temperature is raised to 1350 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 2h, and finally the temperature is lowered to the room temperature at the cooling rate of 10 ℃/min. After the nitriding treatment, the residual Si on the surface layer of the composite material is converted into Si3N4. The final composite matrix was analyzed to be composed of C, SiC and Si3N4Composition, wherein the C content is 5 vol.%, the SiC content is 32 vol./%, and Si is3N4The content was 15 vol.%.
Example 4: two-dimensional semi-transparent wave with fiber volume fraction of 30% by adopting CVI (chemical vapor infiltration) processForm Si3N4A uniform BN interface layer (800 nm thickness) was prepared inside/on the surface of the fiber preform. Methane is used as precursor gas, pyrolytic carbon is deposited on the prefabricated body with the prepared interface layer by a CVI method, the deposition temperature is 1000 ℃, the deposition time is 500h, and porous Si with the open porosity of about 30 percent is prepared3N4fa/C composite material. In the obtained Si3N4fCoating industrial silicon powder with the particle size of 10 mu m on the surface of a/C composite material preform, putting the preform in a vacuum furnace with the absolute pressure of 1000Pa, heating to 1500 ℃ at the heating rate of 30 ℃/min, and preserving heat for 1h to ensure that the porous Si is infiltrated into the silicon melt3N4fAnd reacting the/C composite material preform with a C matrix to generate SiC, and cooling to room temperature at the speed of 10 ℃/min. The open porosity of the resulting composite was tested to be 10 vol.%, and the composite matrix consisted of C, SiC and residual Si. Polishing and machining the composite material obtained after RMI, ultrasonically cleaning and drying the composite material, putting the composite material into a nitriding furnace, and introducing high-purity H of 0.1MPa2+N2Mixed gas (H)2The flow accounts for 5 percent of the total flow of the gas), the temperature is raised to 1100 ℃ at the heating rate of 10 ℃/min, then the temperature is raised to 1450 ℃ at the heating rate of 3 ℃/min, the temperature is kept for 2h, and finally the temperature is lowered to the room temperature at the cooling rate of 10 ℃/min. After the nitriding treatment, the residual Si on the surface layer of the composite material is converted into Si3N4. The final composite matrix was analyzed to be composed of C, SiC and Si3N4Composition, wherein the C content is 10 vol.%, the SiC content is 35 vol./%, and Si is3N4The content was 15 vol.%.

Claims (4)

1. A method for rapidly preparing a wave-absorbing ceramic matrix composite with an electromagnetic impedance gradual change matrix is characterized by comprising the following steps:
step 1, preparing a porous carbon-based composite material: firstly, preparing a boron nitride BN interface layer on the surface of a fiber in a preform by adopting a CVI (chemical vapor infiltration) process, and controlling the thickness of the interface layer to be 200-1500 nm by controlling the deposition time;
then preparing a carbon matrix by adopting a CVI (chemical vapor infiltration) or PIP (PIP) process, and controlling the open porosity of the composite material to be 30% by controlling the CVI deposition time or the PIP times to obtain the porous carbon-based composite material;
step 2, preparing the C-SiC-based composite material by an RMI process: placing the porous carbon-based composite material in a high-temperature vacuum furnace with the absolute pressure of 100-4000 Pa, taking Si powder as a raw material, heating to 1450-1600 ℃ at the heating rate of 3-30 ℃/min, preserving heat for 0.2-3 h, enabling Si to be molten and impregnated into pores of the porous carbon-based composite material, reacting with a carbon matrix to generate SiC, and cooling to room temperature at the cooling rate of 1-30 ℃/min to obtain the C-SiC-based composite material;
step 3, preparing Si by nitridation process3N4Matrix: putting the C-SiC-based composite material into a nitriding furnace for nitriding treatment, wherein the nitriding atmosphere is high-purity N of 0.1-0.5 MPa2Or NH3Or heating the mixed gas to 900-1100 ℃ at a heating rate of 3-30 ℃/min, then heating to 1350-1500 ℃ at a heating rate of 0.1-3 ℃/min, and preserving heat for 1-5 h; after the nitriding treatment, the residual Si on the surface layer of the composite material is converted into Si3N4Obtaining a matrix phase with the composition of carbon material → SiC → Si3N4The wave-absorbing ceramic matrix composite material is provided with an electromagnetic impedance gradient matrix; the mixed gas is N2Or NH3And H2And (3) mixing.
2. The method for rapidly preparing the wave-absorbing ceramic matrix composite with the electromagnetic impedance gradual change matrix according to claim 1, is characterized in that: the prefabricated body adopts a two-dimensional laminated prefabricated body, a two-dimensional semi-woven prefabricated body, a three-dimensional needling prefabricated body or a three-dimensional woven prefabricated body.
3. The method for rapidly preparing the wave-absorbing ceramic matrix composite with the electromagnetic impedance gradual change matrix according to claim 2, is characterized in that: the fiber of the fiber preform adopts high-resistance SiC fiber and wave-transparent Si3N4Fibres or Al2O3A fiber.
4. The method for rapidly preparing the wave-absorbing ceramic matrix composite with the electromagnetic impedance gradual change matrix according to claim 1, is characterized in that: the Si powder is an industrial raw material with the particle size of 2-100 mu m.
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CN111205106B (en) * 2020-01-11 2021-05-28 西安交通大学 Silicon nitride @ carbon wave-absorbing foam and preparation method and application thereof
CN112374901B (en) * 2020-11-19 2022-08-05 航天特种材料及工艺技术研究所 Ablation-resistant modified C/SiC composite material and preparation method thereof
CN113754455B (en) * 2021-09-29 2022-04-08 湖北瑞宇空天高新技术有限公司 Multi-scale toughening layer structure wave-absorbing ceramic matrix composite and preparation method thereof
CN115490529A (en) * 2022-09-16 2022-12-20 江苏华中新材料有限公司 Ceramic matrix composite with electromagnetic impedance gradual change set
CN116217253A (en) * 2023-01-17 2023-06-06 西安交通大学 Impedance gradual change layered gradient composite aerogel and preparation method and application thereof

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103724035B (en) * 2013-07-23 2016-02-03 太仓派欧技术咨询服务有限公司 A kind of density method of fibre reinforced silicon nitride-silicon carbide ceramic composite
CN105481429B (en) * 2016-01-11 2018-06-19 山东理工大学 A kind of preparation method of silicon nitride-silicon carbide-carbon fiber friction material
CN106495702B (en) * 2016-10-14 2019-06-25 湖南工业大学 It is a kind of to prepare carbon fiber/silicon nitride structure absorbing material process

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Carbon/silicon carbide composites prepared by chemical vapor infiltration combined with silicon melt infiltration;Yongdong Xu et al.;《Carbon》;19991231;第37卷;全文 *
Effects of thermal cycling on thermal expansion and mechanical properties of SiC fibre-reinforced reaction-bonded Si3N4 composites;R.T. BHATT et al.;《Journal of Materials Science》;19971231;第32卷;全文 *

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