CN111592371A - Titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and preparation method thereof - Google Patents

Titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and preparation method thereof Download PDF

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CN111592371A
CN111592371A CN202010508372.0A CN202010508372A CN111592371A CN 111592371 A CN111592371 A CN 111592371A CN 202010508372 A CN202010508372 A CN 202010508372A CN 111592371 A CN111592371 A CN 111592371A
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彭雨晴
徐海明
魏子涵
朱界
李爱军
刘立起
张方舟
白瑞成
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Shaoxing Institute Of Shanghai University
University of Shanghai for Science and Technology
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Abstract

The invention discloses a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and a preparation method thereof.A silicon carbide fiber preform is placed in a CVD furnace constant-temperature area, and a titanium silicon carbon interface layer is deposited on the surface of silicon carbide fiber by adopting a chemical vapor infiltration method within a proper temperature range; and then the ceramic matrix composite is placed into slurry containing polycarbosilane and titanium silicon carbon for dipping, and a precursor dipping pyrolysis method (PIP) is adopted to prepare the ceramic matrix composite. The invention prepares the titanium-containing alloy3SiC2The SiCf/SiC composite material of the interface has simple process and low cost, effectively regulates and controls the dielectric constant of the wave-absorbing composite material and achieves good wave-absorbing effect.

Description

Titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and preparation method thereof
Technical Field
The invention relates to the field of wave absorption of silicon carbide composite materials, in particular to a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and a preparation method thereof.
Background
The wave-absorbing material has wide application in daily life and national defense science and technology. With the continuous development of modern radar and microwave electronic technology, human bodies and equipment are increasingly affected by electromagnetic waves. In the military field, various weapons also face serious threats in battle, detection by using radar is a common military means, and the radar is suitable for rapid development of modern detection technology and is of great importance in researching stealth function of weapons in order to improve survival probability of fighters, naval vessels, tanks, missiles and other combat weapons. The stealth technology generally has two means of appearance design and wave-absorbing material selection, changes the direction of reflected waves by designing a complex polyhedron appearance, but has higher difficulty, so the common method is to select the wave-absorbing material with high absorption to electromagnetic waves. The microwave absorbing material can convert electromagnetic waves into heat energy through loss to dissipate, so that the survival probability of the weapon can be improved, and the harm of the electromagnetic waves to human bodies can be reduced.
The ideal electromagnetic wave-absorbing material has the characteristics of wide absorption frequency band, light weight, thin thickness, strong wave-absorbing performance and the like. The silicon carbide used as the wave-absorbing material can simultaneously meet the requirements of light weight, high temperature resistance and the like, and is one of wave-absorbing materials which are developed rapidly at home and abroad. The SiCf/SiC composite material has high strength, oxidation resistance and adjustable conductivity, and is the most potential high-temperature ceramic matrix structure wave-absorbing material. Titanium silicon carbon (Ti)3SiC2) The composite material has the advantages of good conductivity, good high-temperature oxidation resistance, good thermal stability and small density, and can improve the wave-absorbing performance when being applied to the composite material. Duan S(Duan S,et al.Enhanced mechanical andmicrowave absorption properties of SiCf/SiC composite using aluminum powderas active filler[J]Literature), the SiCf/SiC composite material prepared by the PIP process (precursor impregnation pyrolysis method) has the reflection coefficient of more than-10 dB in the frequency range of 8.2-12.4GHz, cannot achieve 90% of electromagnetic wave absorption, and has poor wave absorption performance.
Fan X(Fan X,et al.Mechanical and Electromagnetic InterferenceShielding Behavior of C/SiC Composite Containing Ti3SiC2[J]Literature) adding Ti3SiC2The composite material is introduced into the C/SiC composite material, so that the electromagnetic shielding effectiveness of the composite material in the frequency range of 8.2-12.8GHz is increased, and great potential is shown for the application of multifunctional materials. Gao H (Gao H, et al. improved mechanical and microwave adsorption properties of SiC fiber/mullite composite using hybrid SiC/Ti3SiC2fillers[J]Literature) adding a suitable amount of Ti to a SiCf/Mu composite containing SiC filler3SiC2Due to Ti3SiC2Has higher dielectric constant, so the dielectric constant of the composite material is also increased, and the microwave absorption performance is improved.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material and a preparation method thereof, and prepared titanium silicon carbon (Ti)3SiC2) The interface can effectively regulate and control the dielectric property of the composite material and improve the electromagnetic wave-absorbing property.
In order to achieve the purpose, the invention can be realized by the following technical scheme:
a Ti-Si-C interface modified SiCf/SiC wave-absorbing composite material is prepared by depositing Ti on SiC fiber preform by chemical vapor infiltration3SiC2Interfacial coating, then coating with Ti3SiC2SiC fiber preform with interface coating impregnated in PCS/Ti3SiC2In the slurry, a precursor polymerization impregnation cracking method is adopted to prepare the SiCf/SiC wave-absorbing composite material.
Further, the composite material can realize the reflection efficiency of less than-10 dB at 8-18 GHz.
The invention also provides a preparation method of the titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material, which comprises the following steps:
(1) preparing Ti on the surface of SiC fiber fabric by adopting a chemical vapor infiltration process3SiC2An interface phase forming a SiC fiber fabric reinforcement containing the interface phase;
(2) dissolving polycarbosilane solid particles in dimethylbenzene to form a solution, and adding a certain amount of Ti3SiC2Filler, as a slurry for the first impregnation, Ti3SiC2Introducing into a SiC matrix;
(3) putting the reinforcement body in the step (1) into an impregnation kettle, and preparing Ti by using the slurry in the step (2) and adopting a PIP (poly-p-phenylene-imide) process3SiC2(p)-SiC ceramic matrix until the sample weight gain is less than 1 wt%, the sample preparation is completed, and Ti-containing ceramic matrix is obtained3SiC2An interface modified SiCf/SiC composite material.
Further, the SiC fiber fabric in the step (1) is a 2D laminate or 2.5 or 3D4D or 3D 5D.
Further: the preparation of Ti in the step (1)3SiC2Interfacial phase of TiCl4And H2As a precursor system, Ar is used as a diluent gas and a protective gas, and is introduced into a chemical vapor deposition furnace to deposit for 1 to 10 hours under the conditions of the temperature of 1000 to 1400 ℃ and the pressure of 4 to 10kPa to obtain the Ti3SiC2An interfacial phase.
Further, said H2And TiCl4The molar ratio of (A) to (B) is 10 to 20.
Further, Ti in the first dipping slurry in the step (2)3SiC2The addition amount of the filler accounts for 5-20 wt% of the polycarbosilane and xylene solution.
Further, in the step (2), the polycarbosilane solid particles are dissolved in a solution formed by dimethylbenzene, and the mass fraction of the polycarbosilane is 30-60 wt%.
Further, it is characterized byTi in the above step (2)3SiC2The particle size is 0.015-5 μm.
Further, in the step (3), Ti is contained3SiC2The interface modified SiCf/SiC composite material can realize 8-18GHz and has reflection efficiency less than-10 dB.
Has the advantages that: doping Ti with conventional PIP process3SiC2Compared with particles, the invention firstly uses a CVI process to prepare TiCl4And H2Is used as a precursor system and is introduced into a chemical vapor deposition furnace to obtain more uniform and compact Ti on the silicon carbide fiber3SiC2Interface, effective in reducing Ti3SiC2The agglomeration phenomenon of the particles is strong in combination with the fibers, and is beneficial to the load transfer of the composite material in the loading process. The combination of CVI + PIP process can avoid the defects of long period of single CVI process and the like, and also avoid the defects of multiple holes, multiple cracks and the like caused by single PIP process, and Ti is added in the PIP process3SiC2The filler can inhibit the volume shrinkage of products in the cracking process, and can also adjust the dielectric constant and dielectric loss of the composite material by changing the content of titanium, silicon and carbon, so as to achieve good wave-absorbing performance. The process is simple, has good repeatability, and the prepared material is compact, and has the advantages of high temperature resistance, oxidation resistance and the like.
Drawings
FIG. 1 is a flow chart of a preparation process provided in examples 1-3 of the present invention;
FIG. 2 shows Ti-containing alloy prepared in example 2 of the present invention3SiC2Scanning electron microscope pictures of silicon carbide fibers on the interface;
FIG. 3 is a scanning electron microscope image of the surface topography of the composite material prepared in example 3 of the present invention.
Detailed Description
The technical solution of the present invention will be described in further detail with reference to examples.
Example 1
A preparation method of a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material comprises the following steps (as shown in figure 1):
step 1, extractingPreparation of Ti on surface of 3D4D silicon carbide fiber fabric by chemical vapor infiltration process3SiC2Interfacial phase of TiCl4And H2As a precursor system, Ar as a dilution gas and a protective gas is introduced into a chemical vapor deposition furnace, wherein H2And TiCl4Is 20, the hydrogen flow is 500sccm, the argon flow is 500sccm, and the silicon carbide fiber fabric reinforcement containing the interface phase is formed by deposition for 5 hours at the temperature of 1100 ℃ and the pressure of 8 kPa.
Step 2, dissolving polycarbosilane solid particles in dimethylbenzene to form a solution, and adding a certain amount of Ti3SiC2Filler, as a slurry for the first impregnation, Ti3SiC2Is introduced into the SiC matrix. The addition amount of the titanium silicon carbon filler accounts for 10 wt% of the polycarbosilane and xylene solution, impregnation liquid used in the subsequent impregnation-cracking process is a solution of polycarbosilane dissolved in xylene, and the mass fraction of polycarbosilane in the polycarbosilane solution is 50 wt%.
Step 3, putting the prefabricated body in the step 1 into an impregnation kettle, using the slurry in the step 2, and preparing Ti by a PIP (poly-p-phenylene-imide) process3SiC2(p)-SiC ceramic matrix until the sample weight gain is less than 1 wt%, the sample preparation is completed, and Ti-containing ceramic matrix is obtained3SiC2An interface modified SiCf/SiC composite material.
Step 4, adopting a waveguide method to carry out the treatment on Ti-containing materials3SiC2The dielectric property test of the interface modified SiCf/SiC composite material is carried out, the test frequency is 8-18GHz, and the wave-absorbing performance is less than-10 dB.
Example 2
A preparation method of a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material comprises the following steps:
step 1, preparing Ti on the surface of the 2D laminated silicon carbide fiber fabric by adopting a chemical vapor infiltration process3SiC2Interfacial phase of TiCl4And H2As a precursor system, Ar as a dilution gas and a protective gas is introduced into a chemical vapor deposition furnace, wherein H2And TiCl4The molar ratio of (2) is 10, the hydrogen flow is 350sccm, the argon flow is 450sccm, and the temperature isDepositing for 7h at 1200 ℃ and under the pressure of 6kPa a to form the silicon carbide fiber fabric reinforcement containing the interface phase.
Step 2, dissolving polycarbosilane solid particles in dimethylbenzene to form a solution, and adding a certain amount of Ti3SiC2Filler, as a slurry for the first impregnation, Ti3SiC2Is introduced into the SiC matrix. The adding amount of the titanium silicon carbon filler accounts for 15 wt% of the polycarbosilane and xylene solution, impregnation liquid used in the subsequent impregnation-cracking process is a solution of polycarbosilane dissolved in xylene, and the mass fraction of polycarbosilane in the polycarbosilane solution is 40 wt%.
Step 3, putting the prefabricated body in the step 1 into an impregnation kettle, using the slurry in the step 2, and preparing Ti by a PIP (poly-p-phenylene-imide) process3SiC2(p)-SiC ceramic matrix until the sample weight gain is less than 1 wt%, the sample preparation is completed, and Ti-containing ceramic matrix is obtained3SiC2An interface modified SiCf/SiC composite material. The Ti-containing alloy thus prepared is shown in FIG. 23SiC2Scanning electron microscope pictures of silicon carbide fibers at the interface.
Step 4, adopting a waveguide method to carry out the treatment on Ti-containing materials3SiC2The dielectric property test of the interface modified SiCf/SiC composite material is carried out, the test frequency is 8-18GHz, and the wave-absorbing performance is less than-10 dB.
Example 3
A preparation method of a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material comprises the following steps:
step 1, preparing Ti on the surface of 2.5D silicon carbide fiber fabric by adopting a chemical vapor infiltration process3SiC2Interfacial phase of TiCl4And H2As a precursor system, Ar as a dilution gas and a protective gas is introduced into a chemical vapor deposition furnace, wherein H2And TiCl4Is 10, the hydrogen flow is 700sccm, the argon flow is 800sccm, and the silicon carbide fiber fabric reinforcement containing the interface phase is formed by deposition for 9 hours under the conditions of the temperature of 900 ℃ and the pressure of 4kPa
Step 2, dissolving polycarbosilane solid particles in dimethylbenzene to form a solution, and adding a certain amount of Ti3SiC2The filler is filled in the inner cavity of the shell,as a slurry for the first dipping, Ti was added3SiC2Is introduced into the SiC matrix. The addition amount of the titanium silicon carbon filler accounts for 20 wt% of the polycarbosilane and xylene solution, impregnation liquid used in the subsequent impregnation-cracking process is a solution of polycarbosilane dissolved in xylene, and the mass fraction of polycarbosilane in the polycarbosilane solution is 30 wt%.
Step 3, putting the prefabricated body in the step 1 into an impregnation kettle, using the slurry in the step 2, and preparing Ti by a PIP (poly-p-phenylene-imide) process3SiC2(p)-SiC ceramic matrix until the sample weight gain is less than 1 wt%, the sample preparation is completed, and Ti-containing ceramic matrix is obtained3SiC2An interface modified SiCf/SiC composite material. Referring to fig. 3, a scanning electron microscope image of the surface topography of the prepared composite material is shown, and the following embodiments are provided to illustrate the embodiments of the present invention, other advantages and effects of the present invention will be apparent to those skilled in the art from the disclosure of the present specification.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. A titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material is characterized in that Ti is deposited on a SiC fiber preform by adopting a chemical vapor infiltration process3SiC2Interfacial coating, then coating with Ti3SiC2SiC fiber preform with interface coating impregnated in PCS/Ti3SiC2In the slurry, a precursor polymerization impregnation cracking method is adopted to prepare the SiCf/SiC wave-absorbing composite material.
2. The titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material of claim 1, wherein the composite material can achieve a reflection efficiency of less than-10 dB at 8-18 GHz.
3. A preparation method of a titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material is characterized by comprising the following steps:
(1) preparing Ti on the surface of SiC fiber fabric by adopting a chemical vapor infiltration process3SiC2An interface phase forming a SiC fiber fabric reinforcement containing the interface phase;
(2) dissolving polycarbosilane solid particles in dimethylbenzene to form a solution, and adding a certain amount of Ti3SiC2Filler, as a slurry for the first impregnation, Ti3SiC2Introducing into a SiC matrix;
(3) putting the reinforcement body in the step (1) into an impregnation kettle, and preparing Ti by using the slurry in the step (2) and adopting a PIP (poly-p-phenylene-imide) process3SiC2(p)-SiC ceramic matrix until the sample weight gain is less than 1 wt%, the sample preparation is completed, and Ti-containing ceramic matrix is obtained3SiC2An interface modified SiCf/SiC composite material.
4. The preparation method of the titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material according to claim 3, which is characterized by comprising the following steps: the SiC fiber fabric in the step (1) is 2D laminated or 2.5 or 3D4D or 3D 5D.
5. The preparation method of the titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material according to claim 3, which is characterized by comprising the following steps: the preparation of Ti in the step (1)3SiC2Interfacial phase of TiCl4And H2As a precursor system, Ar is used as a diluent gas and a protective gas, and is introduced into a chemical vapor deposition furnace to deposit for 1 to 10 hours under the conditions of the temperature of 1000 to 1400 ℃ and the pressure of 4 to 10kPa to obtain the Ti3SiC2An interfacial phase.
6. The preparation method of the titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material according to claim 5, which is characterized by comprising the following steps: said H2And TiCl4The molar ratio of (A) to (B) is 10 to 20.
7. The preparation method of the titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material of claim 3The preparation method is characterized by comprising the following steps: ti in the first dipping slurry in the step (2)3SiC2The addition amount of the filler accounts for 5-20 wt% of the polycarbosilane and xylene solution.
8. The preparation method of the titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material according to claim 3, which is characterized by comprising the following steps: in the step (2), the polycarbosilane solid particles are dissolved in a solution formed by dimethylbenzene, and the mass fraction of the polycarbosilane is 30-60 wt%.
9. The preparation method of the titanium silicon carbon interface modified SiCf/SiC wave-absorbing composite material according to claim 3, which is characterized by comprising the following steps: ti in the step (2)3SiC2The particle size is 0.015-5 μm.
10. The method for preparing the titanium-silicon-carbon interface modified SiCf/SiC wave-absorbing composite material as claimed in claim 3, wherein the Ti-containing composite material obtained in the step (3)3SiC2The interface modified SiCf/SiC composite material can realize 8-18GHz and has reflection efficiency less than-10 dB.
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CN112479718A (en) * 2020-11-20 2021-03-12 航天特种材料及工艺技术研究所 Ti3SiC2MAX phase interface layer modified SiC/SiC composite material and preparation method thereof
CN112521156A (en) * 2021-02-18 2021-03-19 中国人民解放军国防科技大学 Hybrid matrix SiCf/SiC composite material and preparation method thereof
CN113185299A (en) * 2021-04-06 2021-07-30 中国航空制造技术研究院 Preparation method of multilayer wave-absorbing ceramic matrix composite
CN114315394A (en) * 2021-12-21 2022-04-12 西北工业大学 By using Ti3SiC2Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material
CN115259878A (en) * 2022-09-01 2022-11-01 上海大学 Suction filtration doping process
CN116239384A (en) * 2023-02-20 2023-06-09 北京航空航天大学 MAX phase ceramic particle modified SiCf/SiC composite material and preparation method thereof
CN116836002A (en) * 2023-05-26 2023-10-03 西北工业大学 Be used for SiC f Ti-Si-C composite coating on SiC surface and preparation method thereof
CN118175828A (en) * 2024-05-16 2024-06-11 浙江大华技术股份有限公司 Wave-absorbing material, preparation method and device
CN118175826A (en) * 2024-05-16 2024-06-11 浙江大华技术股份有限公司 Composite wave-absorbing material, preparation method and device

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CN112479718A (en) * 2020-11-20 2021-03-12 航天特种材料及工艺技术研究所 Ti3SiC2MAX phase interface layer modified SiC/SiC composite material and preparation method thereof
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CN114315394B (en) * 2021-12-21 2023-03-10 西北工业大学 By using Ti 3 SiC 2 Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material
CN114315394A (en) * 2021-12-21 2022-04-12 西北工业大学 By using Ti3SiC2Preparation method of three-dimensional network porous prefabricated body reinforced SiC ceramic matrix composite material
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CN116239384A (en) * 2023-02-20 2023-06-09 北京航空航天大学 MAX phase ceramic particle modified SiCf/SiC composite material and preparation method thereof
CN116239384B (en) * 2023-02-20 2024-06-07 北京航空航天大学 MAX phase ceramic particle modified SiCf/SiC composite material and preparation method thereof
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CN116836002B (en) * 2023-05-26 2024-04-30 西北工业大学 Be used for SiCfTi-Si-C composite coating on SiC surface and preparation method thereof
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