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 PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- fiber preform
- silicon carbide
- polymer precursor
- temperature
- vacuum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C04B35/806—
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/5805—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides
- C04B35/58064—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides
- C04B35/58078—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on borides based on refractory borides based on zirconium or hafnium borides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
- C04B2235/486—Boron containing organic compounds, e.g. borazine, borane or boranyl
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5224—Alumina or aluminates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
- C04B2235/5256—Two-dimensional, e.g. woven structures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
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
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%.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710500824.9A CN107226707B (en) | 2017-06-27 | 2017-06-27 | Preparation method of SiC/Si-B-C-Zr ceramic matrix composite material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710500824.9A CN107226707B (en) | 2017-06-27 | 2017-06-27 | Preparation method of SiC/Si-B-C-Zr ceramic matrix composite material |
Publications (2)
Publication Number | Publication Date |
---|---|
CN107226707A CN107226707A (en) | 2017-10-03 |
CN107226707B true CN107226707B (en) | 2021-02-09 |
Family
ID=59936545
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710500824.9A Active CN107226707B (en) | 2017-06-27 | 2017-06-27 | Preparation method of SiC/Si-B-C-Zr ceramic matrix composite material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107226707B (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108218453B (en) * | 2017-12-01 | 2021-03-26 | 中国航空工业集团公司基础技术研究院 | Forming method of thin-wall conical cylindrical ceramic matrix composite component |
CN108441791A (en) * | 2018-03-21 | 2018-08-24 | 苏州宏久航空防热材料科技有限公司 | A kind of metal ceramic-based composite material of fibre reinforced |
CN110981516B (en) * | 2019-12-13 | 2022-04-15 | 苏州纳迪微电子有限公司 | Composite bulletproof plate and preparation method thereof |
CN113896558B (en) * | 2021-11-10 | 2023-03-21 | 航天特种材料及工艺技术研究所 | High-performance heat-conducting composite material and preparation method thereof |
CN114163252A (en) * | 2021-12-22 | 2022-03-11 | 成都成维精密机械制造有限公司 | Preparation method of ultrahigh-temperature silicon carbide ceramic-based composite material and ultrahigh-temperature silicon carbide ceramic-based composite material |
CN114195525A (en) * | 2022-01-11 | 2022-03-18 | 成都成维精密机械制造有限公司 | Preparation method of low-oxygen-content ceramic matrix composite |
Citations (8)
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)
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 |
-
2017
- 2017-06-27 CN CN201710500824.9A patent/CN107226707B/en active Active
Patent Citations (8)
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 |
Also Published As
Publication number | Publication date |
---|---|
CN107226707A (en) | 2017-10-03 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN107226707B (en) | Preparation method of SiC/Si-B-C-Zr ceramic matrix composite material | |
CN107353025B (en) | Preparation method of 1200-DEG C-resistant and oxidation-resistant ceramic matrix composite | |
CN109354823B (en) | Preparation method of heat-insulation ceramizable phenolic resin-based gradient composite material | |
CN110372390B (en) | Preparation method of continuous fiber reinforced SiC part based on additive manufacturing and product | |
CN108395266A (en) | A kind of preparation method of fiber reinforcement multiphase ceramic matrix composite | |
CN102910927B (en) | Method for preparing self-healing silicon carbide ceramic-based composite material | |
CN110028330B (en) | Ceramic matrix composite and preparation method thereof | |
CN102173815B (en) | Method for preparing ceramic material by process steps of powder green body dipping and precursor cracking | |
CN112341235B (en) | Multiphase coupling rapid densification method for ultrahigh-temperature self-healing ceramic matrix composite | |
CN107311682B (en) | SiC nanowire reinforced Cf/SiC ceramic matrix composite and preparation method thereof | |
CN109265188A (en) | A kind of fibre reinforced hafnium boride-tantalum boride-carbon ceramics based composites and preparation method thereof | |
CN100532329C (en) | Preparation method of carbon-silicon carbide base composite material toughened by carbon fiber | |
CN103332944A (en) | Preparation method of Cf-ZrB2/ZrC/SiC composite material | |
CN112010653B (en) | Fiber-reinforced silicon-boron-nitrogen composite material and preparation method thereof | |
CN110563479A (en) | Ultrahigh-temperature ceramic matrix composite and preparation method thereof | |
CN108101566A (en) | The method that RTM technique auxiliary prepares carbon/silicon carbide ceramic matrix composite component | |
CN105110807B (en) | C/C SiC ceramic matrix composite materials prepared with siliceous aryne resin and preparation method thereof | |
CN108947588B (en) | C/SiC composite material, antioxidant coating used for same and preparation method thereof | |
CN112142486A (en) | Preparation method of ablation-resistant silicon carbide fiber reinforced ceramic matrix composite | |
CN108892524B (en) | Preparation method of C/SiC composite material | |
CN112500180B (en) | Nitride fiber reinforced ceramic-based wave-transparent composite material and precision forming method thereof | |
CN112645725B (en) | Ceramic matrix composite material component with step structure and preparation method thereof | |
CN112010654B (en) | Fiber-reinforced silicon nitride composite material and preparation method thereof | |
CN103332943A (en) | Microstructure design and performance control method for preparing carbon-ceramic-based composite materials based on liquid silicon melt infiltration method | |
CN110776339B (en) | Antioxidant coating for C/ZrC-SiC composite material and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |