CN110668839A - Low-cost high-strength carbon fiber reinforced silicon carbide composite material and preparation method thereof - Google Patents
Low-cost high-strength carbon fiber reinforced silicon carbide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-cost high-strength carbon fiber reinforced ceramic matrix composite and a preparation method thereof. The technical scheme is as follows: mixing phenolic resin, ethylene glycol and a curing agent according to the mass ratio of (10-15) to (11-16) to (1-2), and uniformly stirring to obtain a precursor solution. And (3) dipping the precursor solution into the carbon fiber preform with the interface layer, curing at the temperature range of 120-250 ℃, then heating to 1000 ℃ at the rate of 5-10 ℃ per minute, and carrying out multi-section heat preservation to obtain the low-density porous carbon/carbon composite material. Siliconizing at 1450-1650 ℃, and preserving the heat for 1-4 hours to obtain the carbon fiber reinforced silicon carbide composite material. According to the invention, the carbon/carbon preform with the matrix carbon in the bead chain net-shaped porous structure is prepared by adding the ethylene glycol and the curing agent, and the structure is favorable for permeation and dispersion of liquid silicon and is not easy to cause infiltration channel blockage. The prepared carbon fiber reinforced silicon carbide composite material has the advantages of low cost, high temperature resistance, high strength and the like.
Description
Technical Field
The invention relates to the technical field of C/C-SiC composite material preparation, in particular to a low-cost high-strength carbon fiber reinforced silicon carbide composite material and a preparation method thereof.
Background
The aircraft is in a very severe thermal environment during long-time high-speed flight and reentry in the adjacent space, and the surface temperature of the aircraft is very high under the action of aerodynamic heating, so that a severe challenge is provided for the thermal protection structure and materials of the aircraft. The carbon fiber reinforced silicon carbide composite material has a series of advantages of high temperature resistance, high strength, scouring resistance and the like, thereby becoming one of the most main heat-proof materials in an aircraft heat protection system. Meanwhile, the use and replacement of the carbon fiber reinforced silicon carbide composite material on an aircraft are restricted by high cost and long preparation period. The main preparation technology of the carbon fiber reinforced silicon carbide composite material comprises the following steps: chemical vapor deposition (CVI), precursor dip cracking (PIP), Reaction Melt Infiltration (RMI), Slurry Infiltration (SI), and the like. The Reaction Melt Infiltration (RMI) process has the advantages of low cost, short preparation period, near net shape forming and the like, but the high-temperature mechanical property, the oxidation resistance and the ablation resistance of the prepared ceramic matrix composite material are poor because the etching of fibers, incomplete reaction of matrix carbon and the residue of infiltration metal are caused in the reaction process of the traditional RMI process. The document "Kumar S, Kumar A, SampathK, et al.preparation and interaction students of C-SiC composite Jet valves in solvent motor exhaust [ J]Journal of the European Ceramic Society,2011,31(13): 2425-; literature reference
Magnant,Laurence Maillé,René Pailler,etal.Carbon fiber/reaction-bonded carbide matrix for composite materials–Manufacture and characterization[J]Journal of the European Ceramic Society,2012,32(16): 4497-; document "Zhong Q, Zhang X, Dong S, et al.reactive melt encapsulated Cf/SiCcompounds with a robust matrix derived from novel engineered cementitious carbon structures [ J]Ceramics International,2017,43(7): 5832-. However, it is difficult to obtain a dense silicon carbide matrix by siliconizing directly a carbon fiber reinforced porous carbon preform to obtain a high density carbon fiber reinforced silicon carbide composite.
Disclosure of Invention
The invention provides a low-cost high-strength carbon fiber reinforced silicon carbide composite material and a preparation method thereof, aiming at the problems that silicon can not completely react with matrix carbon in the RMI process of the carbon fiber reinforced ceramic matrix composite material and a porous carbon matrix can not be converted into a compact silicon carbide matrix. The method comprises the steps of soaking a precursor solution consisting of phenolic resin, ethylene glycol and a curing agent into a carbon fiber preform, and curing and carbonizing to obtain the low-density porous carbon/carbon composite material. And carrying out siliconizing reaction on the carbon/carbon prefabricated part under a proper temperature condition to obtain the high-density carbon fiber reinforced silicon carbide composite material. According to the invention, a three-dimensional grid structure is formed by phase separation of the phenolic resin and an organic solvent in the curing polymerization reaction process, a porous carbon matrix formed after carbonization has proper pore size and porosity, and the high-density high-strength carbon fiber reinforced ceramic matrix composite material can be prepared after siliconizing.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a low-cost high-strength carbon fiber reinforced silicon carbide composite material comprises the following steps:
(1) soaking treatment: soaking the carbon fiber preform in a precursor solution consisting of phenolic resin, ethylene glycol and a curing agent for a period of time, and taking out the carbon fiber preform;
(2) curing treatment: curing the carbon fiber preform soaked with the precursor solution to obtain a carbon fiber reinforced porous resin matrix composite material;
(3) carbonizing treatment: carbonizing the carbon fiber reinforced porous resin matrix composite material obtained in the step (2) to obtain a porous carbon/carbon composite material;
(4) repeating the processes of soaking, curing and carbonizing in the steps (1) to (3) for multiple times until a porous carbon/carbon composite material with the required density is obtained;
(5) siliconizing treatment: and (4) carrying out melt siliconizing treatment on the carbon/carbon composite material obtained in the step (4) to obtain the carbon fiber reinforced silicon carbide composite material with low cost and high strength.
In the step (1), the curing agent in the precursor solution is at least one of sodium carbonate, propylene carbonate, p-toluenesulfonic acid, phosphoric acid, benzenesulfonic acid, benzenesulfonyl chloride, hexamethylenetetramine and hydroxymethyl urea.
In the precursor solution, the weight ratio of the phenolic resin, the ethylene glycol and the curing agent is (10-20): (5-20): 1-2).
The carbon fiber preform may have an interface layer, which is a pyrolytic carbon interface, a silicon carbide interface, or a boron nitride interface.
Before the soaking treatment, one or more of dense resin carbon, mesoporous resin carbon and microporous resin carbon can be filled in the carbon fiber preform or the carbon fiber preform with the interface layer.
In the step (1), the soaking process includes: the pressure range is 0.1-9MPa, the soaking time is 1-4 hours, and the soaking is finished when no obvious bubbles exist.
In the step (2), in the curing process: the curing temperature is 120-.
In the step (3), the carbonization process includes: and (2) placing the carbon fiber reinforced porous resin matrix composite material obtained after the curing treatment in a vacuum carbonization furnace, sequentially heating the vacuum carbonization furnace to 20-220 ℃, 220-550 ℃, 550-750 ℃, 700-1000 ℃ and 1000 ℃ at a heating rate of 5-10 ℃/min, and preserving the heat of each temperature section for 0.5-2h, 3-4h, 4-5h, 2-3h and 1-3h in sequence, and cracking and carbonizing the resin matrix after the carbonization treatment to form a porous carbon matrix, thereby obtaining the porous carbon/carbon composite material.
In the step (5), in the siliconizing treatment process, the siliconizing temperature is 1450-1650 ℃, the heat preservation time is 0.5-3 hours, the grain diameter of the used silicon powder is 10 μm-2mm, and the pressure in the infiltration process is less than 20 Pa.
The density of the prepared carbon fiber reinforced silicon carbide composite material is 2.0-2.5g/cm3The three-point bending strength is 80-270 MPa.
The invention has the following beneficial effects:
the structural form of carbon formed by cracking resin in the fiber preform is changed by adding the pore-forming agent, a porous carbon matrix with proper pore size and porosity is obtained, and the high-density high-strength carbon fiber reinforced ceramic matrix composite material can be prepared after siliconizing.
Drawings
FIG. 1 is a graph showing a carbon fiber-reinforced silicon carbide composite material (density: 2.14 g/cm) in example 13) Stress-displacement curve of (a).
FIG. 2 is a graph showing a carbon fiber-reinforced silicon carbide composite material (density: 2.15 g/cm) in example 23) Stress-displacement curve of (a).
FIG. 3 is a graph of the carbon fiber reinforced silicon carbide composite material (density 2.10 g/cm) in example 33) Stress-displacement curve of (a).
FIG. 4 is a graph of the carbon fiber-reinforced silicon carbide composite material (density 2.14 g/cm) in example 13) SEM microstructure morphology of (a).
FIG. 5 shows a carbon fiber-reinforced silicon carbide composite material (density: 2.15 g/cm) in example 23) SEM microstructure morphology of (a).
Detailed Description
For further understanding of the present invention, the present invention will be described with reference to the following examples, which are provided for the purpose of further illustrating the features and advantages of the present invention and are not intended to limit the scope of the present invention as claimed. The invention takes phenolic resin as a carbon source, adds glycol and a curing agent in proper proportion, impregnates a precursor solution consisting of the phenolic resin, the glycol and the curing agent into a carbon fiber preform by an impregnation method, obtains a carbon/carbon preform after curing and carbonization, and can prepare the high-density high-strength carbon fiber reinforced ceramic matrix composite after siliconizing.
Example 1
In this embodiment, a PAN-based T700 carbon felt prepared by a needling process technology is used as a fiber preform, and the specific process steps are as follows:
1) preparing PAN-based T700 carbon felt with the density of 0.52g/cm3。
2) Putting the felt body into a chemical vapor deposition furnace to deposit a pyrolytic carbon matrix, wherein the carbon source is propane, the deposition temperature is 900 ℃, the deposition time is 50 hours, and the density of the carbon felt reaches 0.6g/cm3。
3) Putting the felt body into an impregnation furnace, impregnating furfuryl alcohol resin into the felt body under the vacuum condition of-0.1 MPa, introducing nitrogen into the impregnation furnace to maintain the pressure in the furnace to be 2.0MPa, heating to 180 ℃ at the heating rate of 5 ℃/min, curing for 10 hours, heating to 1000 ℃ at the heating rate of 5 ℃/min under the vacuum condition of-0.1 MPa, preserving heat for one hour at 1000 ℃, and ensuring that the density of the carbon felt reaches 1.0g/cm3。
4) Preparing phenolic resin, ethylene glycol and benzene sulfonyl chloride into a precursor solution according to the mass ratio of 11:10:2, soaking a felt body into the precursor solution, and keeping the felt body for 2 hours under the pressure of 8 MPa.
5) The felt body is placed in an oven for curing, and the temperature is maintained at 150 ℃ for 40h at 120-.
6) The felt body is put in a vacuum carbonization furnace for carbonization, the temperature rise curve is kept for 0.5h at 20-220 ℃, the temperature is kept for 3h at 550 ℃ for 220-plus-materials, the temperature is kept for 4h at 750-plus-materials, the temperature is kept for 2h at 1000 ℃ for 750-plus-materials, and the temperature is kept for 1h at 1000 ℃.
7) Repeating the steps (4), (5) and (6) until the density of the carbon/carbon composite material reaches 1.3g/cm3。
8) And putting the carbon/carbon composite material into a siliconizing furnace, burying silicon powder with the particle size of 10 mu m-2mm, heating to 1500 ℃ in a pressure environment of less than 20Pa, preserving heat for 1h, and allowing liquid silicon to penetrate into pores of the preform and react with carbon to form a silicon carbide substrate.
This implementationThe microstructure of the prepared C/C-SiC composite material is shown in FIG. 4, and the density of the sample is 2.14g/cm3The three-point bending strength was 218.9 MPa.
Example 2
In this embodiment, a PAN-based T700 carbon felt prepared by a needling process technology is used as a fiber preform, and the specific process steps are as follows:
1) preparing PAN-based T700 carbon felt with the density of 0.52g/cm3。
2) Putting the felt body into a chemical vapor deposition furnace to deposit a pyrolytic carbon matrix, wherein the carbon source is propane and trichloromethylsilane, the deposition temperature is 900 ℃, the deposition time is 50 hours, and the density of the carbon felt reaches 0.6g/cm3。
3) Phenolic resin, ethylene glycol and hexamethylenetetramine are prepared into a precursor solution according to the mass ratio of 11:14:1, and a felt body is soaked in the precursor solution and kept for 2 hours.
4) The felt body is placed in an oven for curing and is kept at the temperature of 150 ℃ for 40h under the pressure of 4 MPa.
5) The felt body is put in a vacuum carbonization furnace for carbonization, the temperature rise curve is kept for 0.5h at 20-220 ℃, the temperature is kept for 3h at 550 ℃ for 220-plus-materials, the temperature is kept for 4h at 750-plus-materials, the temperature is kept for 2h at 1000 ℃ for 750-plus-materials, and the temperature is kept for 1h at 1000 ℃. .
6) Repeating the steps (3), (4) and (5) until the density of the carbon/carbon composite material reaches 1.3g/cm3。
7) And (3) putting the carbon/carbon composite material into a siliconizing furnace, heating to 1500 ℃ in a pressure environment of less than 20Pa, preserving the temperature for 1h, and allowing liquid silicon to penetrate into pores of the prefabricated body and react with carbon to form a silicon carbide substrate.
The microstructure of the C/C-SiC composite material prepared in this example is shown in FIG. 5, and the density of the sample is 2.15g/cm3The three-point bending strength was 271.1 MPa.
Example 3
In this embodiment, a PAN-based T700 carbon felt prepared by a needling process technology is used as a fiber preform, and the specific process steps are as follows:
1) preparing PAN-based T700 carbon felt with the density of 0.52g/cm3。
2) Putting felt body into chemical vapor deposition furnace to deposit pyrolytic carbon baseThe carbon source is propane, the deposition temperature is 900 ℃, the deposition time is 50 hours, and the density of the carbon felt reaches 0.6g/cm3。
3) Preparing phenolic resin, ethylene glycol and benzene sulfonyl chloride into a precursor solution according to the mass ratio of 11:10:2, and soaking the felt body into the precursor solution for 2 hours.
4) The felt body is placed in an oven for curing, and the temperature is maintained at 150 ℃ for 40h at 120-.
5) The felt body is put in a vacuum carbonization furnace for carbonization, the temperature rise curve is 20-220 ℃ for 0.5h, the temperature rise curve is 220-220 ℃ for 3h, the temperature rise curve is 550-750 ℃ for 4h, the temperature rise curve is 750-750 ℃ for 2h, and the temperature rise curve is 1000 ℃ for 1 h.
6) Repeating the steps (3), (4) and (5) until the density of the carbon/carbon composite material reaches 1.3g/cm3。
7) And (3) putting the carbon/carbon composite material into a siliconizing furnace, heating to 1500 ℃ in a pressure environment of less than 20Pa, preserving the temperature for 1h, and allowing liquid silicon to penetrate into pores of the prefabricated body and react with carbon to form a silicon carbide substrate.
8) The density of the sample was 2.10g/cm3The three-point bending strength was 234.9 MPa.
Claims (10)
1. A preparation method of a low-cost high-strength carbon fiber reinforced silicon carbide composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) soaking treatment: soaking the carbon fiber preform in a precursor solution consisting of phenolic resin, ethylene glycol and a curing agent for a period of time, and taking out the carbon fiber preform;
(2) curing treatment: curing the carbon fiber preform soaked with the precursor solution to obtain a carbon fiber reinforced porous resin matrix composite material;
(3) carbonizing treatment: carbonizing the carbon fiber reinforced porous resin matrix composite material obtained in the step (2) to obtain a porous carbon/carbon composite material;
(4) repeating the processes of soaking, curing and carbonizing in the steps (1) to (3) for multiple times until a porous carbon/carbon composite material with the required density is obtained;
(5) siliconizing treatment: and (4) carrying out melt siliconizing treatment on the carbon/carbon composite material obtained in the step (4) to obtain the carbon fiber reinforced silicon carbide composite material with low cost and high strength.
2. The method for preparing a high specific strength porous carbon/carbon composite material according to claim 1, characterized in that: in the step (1), in the precursor solution, the curing agent is at least one of sodium carbonate, propylene carbonate, p-toluenesulfonic acid, phosphoric acid, benzenesulfonic acid, benzenesulfonyl chloride, hexamethylenetetramine and hydroxymethyl urea.
3. The method for preparing a high specific strength porous carbon/carbon composite material according to claim 1, characterized in that: in the step (1), the weight ratio of the phenolic resin, the glycol and the curing agent in the precursor solution is (10-20): (5-20): 1-2.
4. The method for preparing a high specific strength porous carbon/carbon composite material according to claim 1, characterized in that: the carbon fiber preform is provided with an interface layer, and the interface layer is a pyrolytic carbon interface, a silicon carbide interface or a boron nitride interface.
5. The method for preparing a high specific strength porous carbon/carbon composite material according to claim 1, characterized in that: and before the soaking treatment, filling one or more of compact resin carbon, mesoporous resin carbon and microporous resin carbon into the carbon fiber preform or the carbon fiber preform with the interface layer.
6. The method for preparing a high specific strength porous carbon/carbon composite material according to claim 1, characterized in that: in the step (1), the soaking treatment comprises the following steps: the pressure range is 0.1-9MPa, the soaking time is 1-4 hours, and the soaking is finished when no obvious bubbles exist.
7. The method for preparing a high specific strength porous carbon/carbon composite material according to claim 1, characterized in that: in the step (2), in the curing process: the curing temperature is 120-.
8. The method for preparing a high specific strength porous carbon/carbon composite material according to claim 1, characterized in that: in the step (3), the carbonization treatment process is as follows: and (2) placing the carbon fiber reinforced porous resin matrix composite material obtained after the curing treatment in a vacuum carbonization furnace, sequentially heating the vacuum carbonization furnace to 20-220 ℃, 220-550 ℃, 550-750 ℃, 700-1000 ℃ and 1000 ℃ at a heating rate of 5-10 ℃/min, and preserving the heat of each temperature section for 0.5-2h, 3-4h, 4-5h, 2-3h and 1-3h in sequence, and cracking and carbonizing the resin matrix after the carbonization treatment to form a porous carbon matrix, thereby obtaining the porous carbon/carbon composite material.
9. The method for producing a carbon fiber-reinforced silicon carbide composite material according to claim 1, characterized in that: in the step (5), in the siliconizing treatment process, the siliconizing temperature is 1450-.
10. A carbon fiber reinforced silicon carbide composite material prepared by the method of any one of claims 1 to 9, wherein: the density of the carbon fiber reinforced silicon carbide composite material is 2.0-2.5g/cm3The three-point bending strength is 80-270 MPa.
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| CN112266262A (en) * | 2020-11-04 | 2021-01-26 | 兰州理工大学 | Novel C/C-SiC composite material and preparation method thereof |
| CN112374901A (en) * | 2020-11-19 | 2021-02-19 | 航天特种材料及工艺技术研究所 | Ablation-resistant modified C/SiC composite material and preparation method thereof |
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