CN107226707B - Preparation method of SiC/Si-B-C-Zr ceramic matrix composite material - Google Patents

Preparation method of SiC/Si-B-C-Zr ceramic matrix composite material Download PDF

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CN107226707B
CN107226707B CN201710500824.9A CN201710500824A CN107226707B CN 107226707 B CN107226707 B CN 107226707B CN 201710500824 A CN201710500824 A CN 201710500824A CN 107226707 B CN107226707 B CN 107226707B
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fiber preform
silicon carbide
polymer precursor
temperature
vacuum
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陈明伟
邱海鹏
谢巍杰
刘善华
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AVIC Composite Corp Ltd
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Abstract

The invention belongs to a preparation technology of a continuous fiber reinforced ultrahigh-temperature ceramic matrix composite, and particularly relates to a preparation method of a SiC/Si-B-C-Zr ceramic matrix composite. The dipping solution adopted by the invention is polycarbosilane, a zirconium boride precursor and xylene, the solubility of the polycarbosilane, the zirconium boride precursor and the xylene is high, and the polymer precursor can be uniformly dispersed in the solution. The invention adopts polymer precursor dipping solutions with different zirconium boride precursor weight percentages to carry out vacuum dipping and high-temperature cracking successively, which is beneficial to preparing ceramic substrates with controllable element composition gradient distribution. According to the invention, B, Zr element is introduced into the original matrix, so that the synergistic oxidation resistance of the oxidation reaction products of diboron trioxide, borosilicate, zirconium dioxide and the like of the Si-B-C-Zr matrix component in different temperature ranges is fully exerted, and the high-temperature oxidation resistance and ablation resistance of the material are improved by utilizing the characteristics of high melting point and excellent ablation resistance of the Si-B-C-Zr matrix component.

Description

Preparation method of SiC/Si-B-C-Zr ceramic matrix composite material
Technical Field
The invention belongs to a preparation technology of a continuous fiber reinforced ultrahigh-temperature ceramic matrix composite, and particularly relates to a preparation method of a SiC/Si-B-C-Zr ceramic matrix composite.
Background
With the gradual increase of the flying Mach number of the aerospace vehicle, the thermal protection component of the aerospace vehicle can bear strong pneumatic heating and strong pneumatic load impact when in service. The severe service environment puts higher requirements on the material, such as low density, excellent ablation resistance, oxidation resistance, mechanical property, high-temperature stability and low thermal expansion coefficient.
At present, the thermal protection component material of the aircraft is mainly a carbon fiber reinforced carbon-based composite material (C/C composite material) and a carbon fiber reinforced silicon-boron-carbon-zirconium ceramic-based composite material (C/Si-B-C-Zr composite material). The C/C composite material has poor oxidation resistance because the fiber and the matrix are both composed of carbon elements. The C/Si-B-C-Zr composite material is mostly prepared by adopting a slurry impregnation cracking process at present, the preparation process is short in preparation period and low in cost, but uniform dispersion distribution among the slurry is difficult to guarantee, so that the consistency of the matrix structure and the components of the composite material is influenced, the resistance of the slurry in the impregnation process is large, the problem of permeation bottleneck exists, the preparation of the homogeneous and compact composite material is not facilitated, meanwhile, the oxidation resistance of carbon fibers adopted in the process is poor, the oxidative decomposition reaction is easy to occur in an oxidizing atmosphere, and the high-temperature stability of the material is seriously influenced.
Disclosure of Invention
The invention aims to provide a preparation method of a SiC/Si-B-C-Zr ceramic matrix composite material aiming at the defects in the prior art.
The technical solution of the invention is as follows:
1. preparing a silicon carbide fiber preform: preparing a silicon carbide fiber preform by taking continuous silicon carbide fibers as a raw material through weaving, and drying in an oven at 100-120 ℃ for not less than 1 hour;
2. preparing an interface layer: depositing a pyrolytic carbon interface layer on the dried silicon carbide fiber preform, wherein a pyrolytic carbon source is propane, the deposition temperature is 950-1050 ℃, the deposition pressure is 1-3 KPa, the propane flow is 1-3L/min, and the interface layer thickness is 0.2-0.6 mu m;
3. preparation of polymer precursor impregnation solution: preparing a polymer precursor dipping solution I by taking polycarbosilane and a zirconium boride precursor as solutes and xylene as a solvent, wherein the solutes account for 40-60 wt% of the precursor dipping solution, and the zirconium boride precursor accounts for 10-50 wt% of the solutes;
4. shaping of the silicon carbide fiber preform: placing the silicon carbide fiber preform into a graphite mold for fixing;
5. vacuum impregnation: placing the silicon carbide fiber preform with the graphite mold in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing the polymer precursor impregnation solution I into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging the graphite mold in the polymer precursor impregnation solution I, and maintaining the pressure for more than 10 hours;
6. hot die pressing: placing the silicon carbide fiber preform of the impregnated graphite mold in a vacuum hot press, wherein the heating rate is 5-10 ℃/min, the mold pressing temperature is 200-220 ℃, the mold pressing pressure is 1-4 MPa, and the pressure maintaining time is not less than 30 min;
7. high-temperature cracking: placing the silicon carbide fiber preform of the graphite mold subjected to hot die pressing into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1000-1300 ℃ from room temperature at the heating rate of 120-300 ℃/h, and keeping the temperature for 0.5-1 hour;
8. densification: after repeating the steps 5 and 7 for 3-4 cycles, demolding the fiber preform from the graphite mold;
9. preparation of polymer precursor impregnation solution: taking polycarbosilane and zirconium boride precursors as solutes, and xylene as a solvent, wherein the solutes account for 40-60 wt% of the precursor impregnation solution, and the zirconium boride precursors account for 20-60 wt% of the solutes, so as to prepare a polymer precursor impregnation solution II;
10. impregnation and cracking: placing the fiber preform in the step 8 in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing a polymer precursor impregnation solution II into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging a graphite mould in the polymer precursor impregnation solution II, and maintaining the pressure for more than 10 hours; then cracking, putting the silicon carbide fiber preform dipped by the polymer precursor dipping solution II into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1000-1300 ℃ from room temperature at the heating rate of 120-300 ℃/h, and keeping the temperature for 0.5-1 hour;
11. and (5) repeating the process of the step (10) until the weight gain of the fiber preform is less than 1%, and obtaining the SiC/Si-B-C-Zr ceramic matrix composite material.
The invention has the advantages and beneficial effects that:
firstly, the method comprises the following steps: the dipping solution adopted by the invention is polycarbosilane, a zirconium boride precursor and xylene, the solubility of the polycarbosilane, the zirconium boride precursor and the xylene is high, and the polymer precursor can be uniformly dispersed in the solution.
Secondly, the method comprises the following steps: the invention adopts polymer precursor dipping solutions with different zirconium boride precursor weight percentages to carry out vacuum dipping and high-temperature cracking successively, which is beneficial to preparing ceramic substrates with controllable element composition gradient distribution.
Thirdly, the method comprises the following steps: according to the invention, B, Zr element is introduced into the original matrix, so that the synergistic oxidation resistance of boron trioxide, borosilicate, zirconium dioxide and the like which are the oxidation reaction products of the Si-B-C-Zr matrix component in different temperature ranges is fully exerted, and the high-temperature oxidation resistance and ablation resistance of the material are improved by utilizing the characteristics of high melting point and excellent ablation resistance of the Si-B-C-Zr matrix component.
Detailed Description
The following embodiments further illustrate the present invention in detail. The method comprises the following operation steps:
1. preparing a silicon carbide fiber preform: preparing a silicon carbide fiber preform by taking continuous silicon carbide fibers as a raw material through weaving, and drying in an oven at 100-120 ℃ for not less than 1 hour;
2. preparing an interface layer: depositing a pyrolytic carbon interface layer on the dried silicon carbide fiber preform, wherein a pyrolytic carbon source is propane, the deposition temperature is 950-1050 ℃, the deposition pressure is 1-3 KPa, the propane flow is 1-3L/min, and the interface layer thickness is 0.2-0.6 mu m;
3. preparation of polymer precursor impregnation solution: preparing a polymer precursor dipping solution I by taking polycarbosilane and a zirconium boride precursor as solutes and xylene as a solvent, wherein the solutes account for 40-60 wt% of the precursor dipping solution, and the zirconium boride precursor accounts for 10-50 wt% of the solutes;
4. shaping of the silicon carbide fiber preform: placing the silicon carbide fiber preform into a graphite mold for fixing;
5. vacuum impregnation: placing the silicon carbide fiber preform with the graphite mold in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing the polymer precursor impregnation solution I into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging the graphite mold in the polymer precursor impregnation solution I, and maintaining the pressure for more than 10 hours;
6. hot die pressing: placing the silicon carbide fiber preform of the impregnated graphite mold in a vacuum hot press, wherein the heating rate is 5-10 ℃/min, the mold pressing temperature is 200-220 ℃, the mold pressing pressure is 1-4 MPa, and the pressure maintaining time is not less than 30 min;
7. high-temperature cracking: placing the silicon carbide fiber preform of the graphite mold subjected to hot die pressing into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1000-1300 ℃ from room temperature at the heating rate of 120-300 ℃/h, and keeping the temperature for 0.5-1 hour;
8. densification: after repeating the steps 5 and 7 for 3-4 cycles, demolding the fiber preform from the graphite mold;
9. preparation of polymer precursor impregnation solution: taking polycarbosilane and zirconium boride precursors as solutes, and xylene as a solvent, wherein the solutes account for 40-60 wt% of the precursor impregnation solution, and the zirconium boride precursors account for 20-60 wt% of the solutes, so as to prepare a polymer precursor impregnation solution II;
10. impregnation and cracking: placing the fiber preform in the step 8 in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing a polymer precursor impregnation solution II into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging a graphite mould in the polymer precursor impregnation solution II, and maintaining the pressure for more than 10 hours; then cracking, putting the silicon carbide fiber preform dipped by the polymer precursor dipping solution II into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1000-1300 ℃ from room temperature at the heating rate of 120-300 ℃/h, and keeping the temperature for 0.5-1 hour;
11. and (5) repeating the process of the step (10) until the weight gain of the fiber preform is less than 1%, and obtaining the SiC/Si-B-C-Zr ceramic matrix composite material.
Example one
1. Preparing a silicon carbide fiber preform: preparing a silicon carbide fiber preform with the fiber volume fraction of 40% by taking continuous silicon carbide fiber as a raw material through weaving, and drying for 2 hours at 110 ℃ in an oven;
2. preparing an interface layer: depositing a pyrolytic carbon interface layer on the dried silicon carbide fiber preform, wherein a pyrolytic carbon source is propane, the deposition temperature is 1050 ℃, the deposition pressure is 2KPa, the propane flow is 1.5L/min, and the thickness of the interface layer is 0.3 mu m;
3. preparation of polymer precursor impregnation solution: preparing a polymer precursor dipping solution I by taking polycarbosilane and a zirconium boride precursor as solutes and xylene as a solvent, wherein the solutes account for 50 wt% of the precursor dipping solution, and the zirconium boride precursor accounts for 20 wt% of the solutes;
4. shaping of the silicon carbide fiber preform: placing the silicon carbide fiber preform into a graphite mold for fixing;
5. vacuum impregnation: placing the silicon carbide fiber preform with the graphite mold in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing the polymer precursor impregnation solution I into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging the graphite mold in the polymer precursor impregnation solution I, and maintaining the pressure for 20 hours;
6. hot die pressing: placing the impregnated silicon carbide fiber preform of the graphite mold in a vacuum hot press, wherein the heating rate is 5 ℃/min, the molding temperature is 220 ℃, the molding pressure is 2MPa, and the pressure maintaining time is 60 min;
7. high-temperature cracking: placing the silicon carbide fiber preform of the graphite mold subjected to hot die pressing into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1200 ℃ from room temperature at the heating rate of 120 ℃/h, and preserving heat for 1 hour;
8. densification: after repeating the steps 5 and 7 for 3-4 cycles, demolding the fiber preform from the graphite mold;
9. preparation of polymer precursor impregnation solution: taking polycarbosilane and zirconium boride precursors as solutes, and xylene as a solvent, wherein the solutes account for 50 wt% of the precursor impregnation solution, and the zirconium boride precursors account for 50 wt% of the solutes, so as to prepare a polymer precursor impregnation solution II;
10. impregnation and cracking: placing the fiber preform in the step 8 in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing a polymer precursor impregnation solution II into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging a graphite mould in the polymer precursor impregnation solution II, and maintaining the pressure for 20 hours; then cracking, putting the silicon carbide fiber preform soaked by the polymer precursor soaking solution II into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1200 ℃ from room temperature at the heating rate of 120 ℃/h, and keeping the temperature for 1 hour;
11. and (5) repeating the process of the step (10) until the weight gain of the fiber preform is less than 1%, and obtaining the SiC/Si-B-C-Zr ceramic matrix composite material.
Example 2
1. Preparing a silicon carbide fiber preform: preparing a silicon carbide fiber preform with the fiber volume fraction of 45% by taking continuous silicon carbide fibers as raw materials through weaving, and drying for 2 hours at 110 ℃ in an oven;
2. preparing an interface layer: depositing a pyrolytic carbon interface layer on the dried silicon carbide fiber preform, wherein a pyrolytic carbon source is propane, the deposition temperature is 1000 ℃, the deposition pressure is 2KPa, the propane flow is 2.5L/min, and the thickness of the interface layer is 0.3 mu m;
3. preparation of polymer precursor impregnation solution: preparing a polymer precursor dipping solution I by taking polycarbosilane and a zirconium boride precursor as solutes and xylene as a solvent, wherein the solutes account for 40 wt% of the precursor dipping solution, and the zirconium boride precursor accounts for 10 wt% of the solutes;
4. shaping of the silicon carbide fiber preform: placing the silicon carbide fiber preform into a graphite mold for fixing;
5. vacuum impregnation: placing the silicon carbide fiber preform with the graphite mold in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing the polymer precursor impregnation solution I into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging the graphite mold in the polymer precursor impregnation solution I, and maintaining the pressure for 10 hours;
6. hot die pressing: placing the impregnated silicon carbide fiber preform of the graphite mold in a vacuum hot press, wherein the heating rate is 10 ℃/min, the molding temperature is 220 ℃, the molding pressure is 2MPa, and the pressure maintaining time is 30 min;
7. high-temperature cracking: placing the silicon carbide fiber preform of the graphite mold subjected to hot die pressing into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1150 ℃ from room temperature at the heating rate of 300 ℃/h, and preserving heat for 1 hour;
8. densification: after repeating the steps 5 and 7 for 3-4 cycles, demolding the fiber preform from the graphite mold;
9. preparation of polymer precursor impregnation solution: preparing a polymer precursor dipping solution II by taking polycarbosilane and a zirconium boride precursor as solutes and xylene as a solvent, wherein the solutes account for 40 percent of the weight of the precursor dipping solution, and the zirconium boride precursor accounts for 40 percent of the weight of the solutes;
10. impregnation and cracking: placing the fiber preform in the step 8 in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing a polymer precursor impregnation solution II into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging a graphite mould in the polymer precursor impregnation solution II, and maintaining the pressure for 20 hours; then cracking, putting the silicon carbide fiber preform impregnated by the polymer precursor impregnation solution II into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1150 ℃ from room temperature at the heating rate of 300 ℃/h, and preserving heat for 1 hour;
11. and (5) repeating the process of the step (10) until the weight gain of the fiber preform is less than 1%, and obtaining the SiC/Si-B-C-Zr ceramic matrix composite material.
Example 3
1. Preparing a silicon carbide fiber preform: preparing a silicon carbide fiber preform with the fiber volume fraction of 55% by taking continuous silicon carbide fiber as a raw material through weaving, and drying for 1 hour at 110 ℃ in an oven;
2. preparing an interface layer: depositing a pyrolytic carbon interface layer on the dried silicon carbide fiber preform, wherein a pyrolytic carbon source is propane, the deposition temperature is 1000 ℃, the deposition pressure is 3KPa, the propane flow is 3L/min, and the interface layer thickness is 0.4 mu m;
3. preparation of polymer precursor impregnation solution: preparing a polymer precursor dipping solution I by taking polycarbosilane and a zirconium boride precursor as solutes and xylene as a solvent, wherein the solutes account for 60 percent by weight of the precursor dipping solution, and the zirconium boride precursor accounts for 40 percent by weight of the solutes;
4. shaping of the silicon carbide fiber preform: placing the silicon carbide fiber preform into a graphite mold for fixing;
5. vacuum impregnation: placing the silicon carbide fiber preform with the graphite mold in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing the polymer precursor impregnation solution I into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, and finally, completely submerging the graphite mold in the polymer precursor impregnation solution I and maintaining the pressure for more than 20 hours;
6. hot die pressing: placing the impregnated silicon carbide fiber preform of the graphite mold in a vacuum hot press, wherein the heating rate is 5 ℃/min, the molding temperature is 205 ℃, the molding pressure is 4MPa, and the pressure maintaining time is 60 min;
7. high-temperature cracking: placing the silicon carbide fiber preform of the graphite mold subjected to hot die pressing into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1200 ℃ from room temperature at the heating rate of 300 ℃/h, and preserving heat for 0.5 hour;
8. densification: after repeating the steps 5 and 7 for 3-4 cycles, demolding the fiber preform from the graphite mold;
9. preparation of polymer precursor impregnation solution: taking polycarbosilane and zirconium boride precursors as solutes, and xylene as a solvent, wherein the solutes account for 60 wt% of the precursor impregnation solution, and the zirconium boride precursors account for 60 wt% of the solutes, so as to prepare a polymer precursor impregnation solution II;
10. impregnation and cracking: placing the fiber preform in the step 8 in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing a polymer precursor impregnation solution II into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging a graphite mould in the polymer precursor impregnation solution II, and maintaining the pressure for 15 hours; then cracking, putting the silicon carbide fiber preform soaked by the polymer precursor soaking solution II into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1300 ℃ from room temperature at the heating rate of 300 ℃/h, and preserving heat for 0.5 hour;
11. and (5) repeating the process of the step (10) until the weight gain of the fiber preform is less than 1%, and obtaining the SiC/Si-B-C-Zr ceramic matrix composite material.

Claims (2)

1. A preparation method of a SiC/Si-B-C-Zr ceramic matrix composite material is characterized by comprising the following steps:
(1) preparing a silicon carbide fiber preform: preparing a silicon carbide fiber preform by taking continuous silicon carbide fibers as a raw material through weaving, and drying in an oven at 100-120 ℃ for not less than 1 hour;
(2) preparing an interface layer: depositing a pyrolytic carbon interface layer on the dried silicon carbide fiber preform, wherein a pyrolytic carbon source is propane, the deposition temperature is 950-1050 ℃, the deposition pressure is 1-3 KPa, the propane flow is 1-3L/min, and the interface layer thickness is 0.2-0.6 mu m;
(3) preparation of polymer precursor impregnation solution: preparing a polymer precursor dipping solution I by taking polycarbosilane and a zirconium boride precursor as solutes and xylene as a solvent, wherein the solutes account for 40-60 wt% of the precursor dipping solution, and the zirconium boride precursor accounts for 10-50 wt% of the solutes;
(4) shaping of the silicon carbide fiber preform: placing the silicon carbide fiber preform into a graphite mold for fixing;
(5) vacuum impregnation: placing the silicon carbide fiber preform with the graphite mold in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing the polymer precursor impregnation solution I into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging the graphite mold in the polymer precursor impregnation solution I, and maintaining the pressure for more than 10 hours;
(6) hot die pressing: placing the silicon carbide fiber preform of the impregnated graphite mold in a vacuum hot press, wherein the heating rate is 5-10 ℃/min, the mold pressing temperature is 200-220 ℃, the mold pressing pressure is 1-4 MPa, and the pressure maintaining time is not less than 30 min;
(7) high-temperature cracking: placing the silicon carbide fiber preform of the graphite mold subjected to hot die pressing into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1000-1300 ℃ from room temperature at the heating rate of 120-300 ℃/h, and keeping the temperature for 0.5-1 hour;
(8) densification: after repeating the steps 5 and 7 for 3-4 cycles, demolding the fiber preform from the graphite mold;
(9) preparation of polymer precursor impregnation solution: taking polycarbosilane and zirconium boride precursors as solutes, and xylene as a solvent, wherein the solutes account for 40-60 wt% of the precursor impregnation solution, and the zirconium boride precursors account for 20-60 wt% of the solutes, so as to prepare a polymer precursor impregnation solution II;
(10) impregnation and cracking: placing the fiber preform in the step 8 in vacuum impregnation equipment, vacuumizing the vacuum impregnation equipment by using a vacuum pump, introducing a polymer precursor impregnation solution II into the inner cavity of the vacuum impregnation equipment through a stainless steel pipeline when the pressure of the inner cavity of the vacuum impregnation equipment is lower than 0.01MPa, finally completely submerging a graphite mould in the polymer precursor impregnation solution II, and maintaining the pressure for more than 10 hours; then cracking, putting the silicon carbide fiber preform dipped by the polymer precursor dipping solution II into a high-temperature cracking furnace, vacuumizing to less than 2KPa, heating to 1000-1300 ℃ from room temperature at the heating rate of 120-300 ℃/h, and keeping the temperature for 0.5-1 hour;
(11) repeating the process of the step 10 until the weight gain of the fiber preform is less than 1%, and obtaining the SiC/Si-B-C-Zr ceramic matrix composite;
in the preparation process, the polymer precursor dipping solution I and the polymer precursor dipping solution II with different weight percentages of the zirconium boride precursors are adopted to carry out vacuum dipping and pyrolysis successively, so that the prepared ceramic matrix with controllable element composition gradient distribution is obtained.
2. The method for preparing the SiC/Si-B-C-Zr ceramic matrix composite material according to claim 1, wherein the fiber volume fraction of the silicon carbide fiber preform prepared by weaving is 40-60%.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5246736A (en) * 1990-10-26 1993-09-21 Societe Europeenne De Propulsion Process for the manufacture of a refractory composite material protected against corrosion
CN101863665A (en) * 2009-04-15 2010-10-20 中国科学院上海硅酸盐研究所 Method for preparing self-healing anti-oxidation functional fiber reinforced ceramic matrix composite material
CN102910927A (en) * 2012-11-16 2013-02-06 中国航空工业集团公司北京航空制造工程研究所 Method for preparing self-healing silicon carbide ceramic-based composite material
CN103332944A (en) * 2013-06-08 2013-10-02 山东工业陶瓷研究设计院有限公司 Preparation method of Cf-ZrB2/ZrC/SiC composite material
CN106565261A (en) * 2016-11-01 2017-04-19 中国航空工业集团公司基础技术研究院 Method for manufacturing SiC/SiC composite material pin with precursor infiltration and pyrolysis method
CN106567246A (en) * 2016-10-31 2017-04-19 航天材料及工艺研究所 Method used for preparing SiC reinforced low-density porous carbon fiber thermal insulation composite material via chemical vapor infiltration
CN106747477A (en) * 2015-11-25 2017-05-31 中国科学院上海硅酸盐研究所 A kind of Cf/SiC-ZrC-ZrB2The preparation method of ultra-temperature ceramic-based composite material
CN106747487A (en) * 2016-06-12 2017-05-31 北京航空航天大学 1800 DEG C of preparation methods of thermostructural composite of heatproof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE602005001247T2 (en) * 2004-09-28 2008-01-24 General Electric Co. Cost effective manufacturing process for high performance ceramic matrix composites

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5246736A (en) * 1990-10-26 1993-09-21 Societe Europeenne De Propulsion Process for the manufacture of a refractory composite material protected against corrosion
CN101863665A (en) * 2009-04-15 2010-10-20 中国科学院上海硅酸盐研究所 Method for preparing self-healing anti-oxidation functional fiber reinforced ceramic matrix composite material
CN102910927A (en) * 2012-11-16 2013-02-06 中国航空工业集团公司北京航空制造工程研究所 Method for preparing self-healing silicon carbide ceramic-based composite material
CN103332944A (en) * 2013-06-08 2013-10-02 山东工业陶瓷研究设计院有限公司 Preparation method of Cf-ZrB2/ZrC/SiC composite material
CN106747477A (en) * 2015-11-25 2017-05-31 中国科学院上海硅酸盐研究所 A kind of Cf/SiC-ZrC-ZrB2The preparation method of ultra-temperature ceramic-based composite material
CN106747487A (en) * 2016-06-12 2017-05-31 北京航空航天大学 1800 DEG C of preparation methods of thermostructural composite of heatproof
CN106567246A (en) * 2016-10-31 2017-04-19 航天材料及工艺研究所 Method used for preparing SiC reinforced low-density porous carbon fiber thermal insulation composite material via chemical vapor infiltration
CN106565261A (en) * 2016-11-01 2017-04-19 中国航空工业集团公司基础技术研究院 Method for manufacturing SiC/SiC composite material pin with precursor infiltration and pyrolysis method

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