CN115557800A - Method for preparing silicon carbide-based composite material by uniformly ceramizing porous carbon - Google Patents
Method for preparing silicon carbide-based composite material by uniformly ceramizing porous carbon Download PDFInfo
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Abstract
The invention relates to a method for preparing a silicon carbide-based composite material by uniformly ceramizing porous carbon, and belongs to the technical field of thermal protection materials for aircrafts. According to the method, phenolic resin, ethylene glycol and a curing agent are uniformly mixed to prepare a precursor solution, the precursor solution is soaked into a carbon or ceramic fiber preform, a high-pressure auxiliary phase separation and high-temperature curing method is adopted, boiling of the ethylene glycol and volatilization of free phenol and other substances are inhibited, more active sites of the phenolic resin are promoted to participate in polymerization reaction, and then the porous carbon-based infiltration preform with a uniform nano-pore structure and proper porosity is obtained after curing and carbonization. And (3) siliconizing at 1450-1550 ℃ to completely convert the porous carbon into a silicon carbide matrix, wherein the volume expansion generated in the process can completely fill the original pore channel. The obtained silicon carbide matrix has compact structure, no carbon residue and silicon residue and fine crystal grains; meanwhile, the introduced liquid silicon is completely consumed in the reaction process, and the fibers are not etched.
Description
Technical Field
The invention relates to the technical field of thermal protection materials for aircrafts, in particular to a method for preparing a silicon carbide-based composite material by uniformly ceramizing porous carbon.
Background
The aircraft faces a severe thermal oxygen environment examination in the process of flying at a high speed in an adjacent space or entering the atmosphere again, and the thermal protection system material of the aircraft has the excellent characteristics of high strength and toughness, thermal shock resistance, ultrahigh temperature oxidation resistance-ablation resistance and the like. Carbon or silicon carbide fiber reinforced silicon carbide composite materials (C/SiC, siC/SiC) have a series of advantages of low density, high temperature resistance, high strength, oxidation ablation resistance and the like, and therefore, become important candidate materials in an aircraft thermal protection system. However, the high manufacturing costs and long preparation cycles limit the use of silicon carbide-based composites in aircraft. The main preparation technology of the fiber reinforced SiC ceramic matrix composite material comprises the following steps: chemical Vapor Infiltration (CVI), precursor dip cracking (PIP), reaction Melt Infiltration (RMI), and Slurry Infiltration (SI), among others. The RMI has the advantages of low preparation cost, short period, realization of near-net-shape forming and the like, and is considered as a preparation technology of the SiC ceramic matrix composite material with an industrial prospect. However, in the traditional RMI process, the carbon matrix generally adopts resin carbon, pyrolytic carbon and a mixed matrix thereof, and the carbon wall thickness of the matrix skeleton has a large amount of large holes of hundreds of microns, so that the carbon matrix has incomplete reaction, excessive silicon residues and fiber etching, and the prepared C/SiC composite material has poor high-temperature mechanical, oxidation resistance and ablation resistance. The articles "Journal of the European Ceramic Society, 2012, 32 (16): 4497-4505" and "Ceramics International, 2017, 43 (7): 5832-5836" indicate that the amount of carbon residue in the composite material produced can be effectively reduced by replacing the dense carbon matrix in the conventional preform with a porous carbon matrix. However, because a large amount of macropores with the size of several micrometers to tens of micrometers still remain in the preform, more silicon-rich regions still exist in the prepared composite material, and obvious fiber and interface etching appears. The article "Materials Science and Engineering, 1991, 144: 63-74" proposes that the reaction process of carbon and silicon proceeds by a dissolution-precipitation mechanism in the early stage, and when a micron-sized dense SiC layer is formed on the surface of the carbon particles, the reaction can proceed only by the diffusion of carbon in the SiC layer, the reaction mechanism is converted into a diffusion mechanism, and the reaction speed in the process is very slow, so that the carbon matrix cannot be completely cerammed. Therefore, a carbon matrix having a nano-sized skeleton is expected to achieve a rapid complete ceramic transformation. Aiming at the problems that the aperture and the framework size of porous carbon are large (micron-sized or nearly micron-sized) and the distribution is uneven and the like in the traditional porous carbon prepared from a mixed solution of resin, a pore-forming agent and a curing agent, the porous carbon substrate with nanoscale uniform pores (40 nm) is prepared by a pressure-assisted phase separation-high-temperature curing combined technology, ideal uniform ceramic formation of the carbon substrate is realized by adjusting the porosity of the substrate and optimizing a reaction process, and finally, the fiber-reinforced silicon carbide composite material with no fiber etching, compact substrate, no carbon residue and silicon residue and small grain size (50 to 100 nm) is obtained.
Disclosure of Invention
Aiming at the problems that when the existing RMI process is used for preparing the carbon or ceramic fiber reinforced SiC ceramic matrix composite, the carbon matrix cannot be completely ceramized, a large amount of silicon remains in the obtained SiC matrix, fiber etching and the like, the invention provides the method for preparing the silicon carbide matrix composite by uniformly ceramizing the porous carbon.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a silicon carbide-based composite material by uniformly ceramizing porous carbon comprises the steps of firstly preparing a porous carbon matrix with the porosity of 45-58%, and then carrying out siliconizing treatment to obtain the silicon carbide-based composite material; the method specifically comprises the following steps:
(1) Dipping treatment: soaking the carbon fiber or ceramic fiber preform in a precursor solution for a period of time and then taking out the carbon fiber or ceramic fiber preform;
(2) High-pressure assisted phase separation and curing treatment: pressurizing the carbon or ceramic fiber preform soaked with the precursor solution to 1 to 10 MPa, rapidly heating to a curing temperature, and forming a nano porous organic matrix with a uniform pore structure in the fiber preform under the conditions of external pressure and high curing temperature to obtain the fiber-reinforced nano porous resin matrix composite material; in the process, the boiling of glycol and the volatilization of free phenol and other substances in the precursor solution can be inhibited by the applied pressure, so that the uniform gel forms a porous organic matrix with a uniform pore structure. Meanwhile, the reaction activity of hydroxyl at the molecular chain end of the phenolic resin can be obviously improved by high curing temperature, so that more active sites participate in polymerization reaction in the phase separation process, the number of nucleation sites in the reaction precursor solution is greatly increased, and a three-dimensional network skeleton with the structural characteristic of small aperture (less than 100 nm) is formed.
(3) Carbonizing treatment: carrying out high-temperature carbonization treatment on the fiber-reinforced nano porous resin matrix composite material obtained in the step (2) to obtain a low-density porous carbon-based infiltration preform;
(4) Repeating the processes of soaking, curing and carbonizing in the steps (1) to (3) for multiple times until a porous carbon-based infiltration preform with a required density is obtained;
(5) Siliconizing treatment: and (4) carrying out low-temperature melting siliconizing treatment on the porous carbon-based infiltration preform obtained in the step (4) to obtain the fiber-reinforced silicon carbide composite material.
In the step (1), the precursor solution is prepared by mixing and uniformly stirring phenolic resin, ethylene glycol and a curing agent according to the weight ratio of (10) - (15) to (11) - (16) to (1) - (2); in the precursor solution, the phenolic resin can be common commercial-grade resin or modified boron phenolic, barium phenolic and the like, and 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.
In the step (1), the carbon fiber and ceramic fiber preform may have an interface layer, and the interface layer may be one or more of a pyrolytic carbon interface, a silicon carbide interface, or a boron nitride interface.
In the dipping treatment of the step (1): the pressure range is 0.1 to 9 MPa, the dipping time is 1 to 4 hours, and the dipping treatment is finished when no air bubbles are obvious.
In the step (2), the curing temperature is 120 to 250 ℃, and the heating rate is more than 10 ℃/min; the porous organic matrix on the surface of the fiber has a three-dimensional network framework structure with the characteristic of small pore diameter (less than 100 nm).
In the step (3), the carbonization process includes: and (3) placing the fiber reinforced nano porous resin matrix composite material obtained after curing treatment in a vacuum carbonization furnace, heating the vacuum carbonization furnace to 1200-1800 ℃ at the heating rate of 5-10 ℃/min, and preparing a carbon matrix with uniformly distributed nano pores on the surface of the fiber by cracking the organic matrix and combining micropores under the high-temperature condition, thus obtaining the porous carbon/carbon composite material (the porous carbon-based infiltration preform).
In the step (4), the pore size distribution range of the carbon matrix in the porous carbon-based infiltration preform is 10-80 nm, and the pore size of the mesopore is 40-45 nm.
In the step (5), in the siliconizing treatment process, the siliconizing temperature is 1450 to 1550 ℃, the heat preservation time is 1 to 2 hours, the particle size of the used silicon powder is 10 mu m to 2 mm, and the pressure in the infiltration process is less than 20 Pa. The siliconizing treatment adopts lower reaction temperature, which can avoid the rapid generation of silicon carbide and the blockage of pore channels in the infiltration process, thereby influencing the subsequent silicon melt infiltration. And, the lower reaction temperature can inhibit further growth of the produced silicon carbide grains.
In the step (4), the porosity of the porous carbon substrate obtained after carbonization is calculated according to the matching relationship between the porosity P of the porous carbon substrate and the volume expansion rate under the ideal condition that dense silicon carbide is generated after the porous carbon reacts: p =1-V m C/V m SiC of, wherein V m C is the molar volume of the porous carbon matrix, V m SiC is the molar volume of the compact silicon carbide matrix.
The silicon carbide substrate obtained in the step (5) is compact and has no carbon residue or silicon residue, and the grain size of the silicon carbide is 50-100 nm; and the fibers in the composite material are not etched after the reaction.
The invention has the following beneficial effects:
1. the porous carbon matrix with a uniform nanopore structure (with a median pore of 40-45 nm) is obtained through high-pressure auxiliary phase separation, high-temperature curing and carbonization. Compared with other reaction infiltration methods for preparing C/SiC and the porous carbon substrate selected by SiC/SiC, the substrate has the smallest skeleton size and pore diameter. The small size of the carbon skeleton and pore size facilitates the complete ceramization of the carbon matrix and the complete consumption of liquid silicon.
2. The invention provides and verifies the design criteria of the carbon matrix structure and the reaction infiltration process, and obtains a novel preparation method of the high-performance fiber-reinforced silicon carbide-based composite material. The invention determines the proper porosity range of the ideal porous carbon matrix through theoretical calculation of silicon-carbon reaction, and obtains the corresponding porous carbon matrix through combined regulation and control of precursor raw materials and curing and carbonization processes. The nearly ideal silicon-carbon reaction is achieved by low temperature siliconizing: when the reaction is completed, the porous carbon matrix is completely converted into the silicon carbide matrix, and the original pore channel is completely filled by volume expansion caused in the process; meanwhile, the introduced liquid silicon is completely consumed in the reaction process, and the fibers are not etched.
3. The high-performance silicon carbide-based composite material prepared by the invention is expected to be used as a novel high-temperature oxidation-ablation-resistant material to be applied to the fields of aviation and aerospace thermal protection and the like. The C/SiC material prepared by the invention has excellent mechanical property because the matrix strength is high and the carbon fiber is not damaged. The strength of the C/SiC composite material prepared by taking the T700K needling carbon fiber preform as a reinforcement can reach 270 MPa, which is far higher than that of a composite material with the same preform structure prepared by a traditional reaction infiltration method. Meanwhile, the generated silicon carbide matrix is compact and has no residual silicon and carbon phases, so that the prepared C/SiC has excellent high-temperature ablation resistance, and the linear ablation rate is less than 0.02 mu m/s after the C/SiC is ablated for 500 s in an oxyacetylene environment with the surface temperature of 2200 ℃ for a long time.
Drawings
FIG. 1 is a carbon matrix morphology for the carbon/carbon composite made in example 1.
Fig. 2 is a graph showing the pore size distribution of the carbon/carbon composite material prepared in example 1.
FIG. 3 is a diagram showing the morphology of the silicon carbide substrate in example 1.
FIG. 4 is a graph of the carbon fiber reinforced silicon carbide composite of example 1.
Fig. 5 is a pore size distribution of the carbon/carbon composite prepared in example 2.
FIG. 6 is a graph of the carbon fiber reinforced silicon carbide composite of example 2; wherein (a) and (b) are material morphologies at different magnifications.
FIG. 7 is the composition of the carbon fiber reinforced silicon carbide composite in example 2.
Fig. 8 is a stress-displacement curve of the carbon fiber reinforced silicon carbide composite in example 2.
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.
According to the invention, phenolic resin is used as a carbon source, ethylene glycol and a curing agent are added in a proper proportion, a precursor solution consisting of the phenolic resin, the ethylene glycol and the curing agent is impregnated into a carbon and ceramic fiber preform by an impregnation method, an infiltration preform is obtained after curing and carbonization, and a high-density and high-strength fiber reinforced SiC ceramic matrix composite material can be prepared after siliconizing.
The method specifically comprises the steps of soaking a precursor solution consisting of phenolic resin, ethylene glycol and a curing agent in a specific ratio into a fiber preform, and carrying out high-pressure auxiliary phase separation, high-temperature curing and carbonization to obtain the porous carbon-based infiltration preform with a uniform nanopore structure (-40 nm) and appropriate porosity (45-58%). And (3) siliconizing at 1450 to 1550 ℃ and preserving heat for 1 to 2 hours to realize the silicon-carbon reaction under an almost ideal state: when the reaction is finished, the porous carbon matrix is completely converted into a silicon carbide matrix, and the original pore channel is completely filled by volume expansion caused in the process, so that the generated silicon carbide matrix is compact, has no carbon residue and silicon residue, and is fine (50 to 100 nm) in crystal grain due to the appearance heredity; meanwhile, the introduced liquid silicon is completely consumed in the reaction process, and the fibers are not etched. Because the matrix strength is high (the strength of the ceramic is inversely proportional to the 1/2 power of the crystal grain size), and the fiber is not damaged, the prepared silicon carbide-based composite material has excellent mechanical properties. The bending strength of the C/SiC composite material prepared by taking the T700K needling carbon fiber preform as a reinforcement can reach 270 MPa, and is far higher than that of a composite material prepared by a traditional reaction infiltration method and having the same carbon fiber preform structure. Meanwhile, the generated silicon carbide matrix is compact and has no carbon residue and silicon residue, so that the prepared C/SiC has excellent high-temperature ablation resistance. After the composite material is ablated for 500 s in an oxyacetylene environment with the surface temperature of 2200 ℃ for a long time, the line ablation rate is less than 0.02 mu m/s.
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 0.52 g/cm 3 。
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 60 hours, and the density of the carbon felt reaches 0.7 g/cm 3 。
3) Preparing phenolic resin, ethylene glycol and hexamethylenetetramine into a precursor solution according to the mass ratio of 11.
4) And (3) placing the felt body in a curing furnace for curing, and keeping the temperature of the felt body within the temperature range of 180 to 250 ℃ for 40 hours under the pressure of 4 MPa.
5) The felt body is put in a vacuum carbonization furnace for carbonization, and the process is as follows: raising the temperature from 20 ℃ to 220 ℃ and preserving heat for 0.5 h, raising the temperature from 220 ℃ to 550 ℃ and preserving heat for 3 h, raising the temperature from 550 ℃ to 750 ℃ and preserving heat for 4 h, raising the temperature from 750 ℃ to 1000 ℃ and preserving heat for 2 h, and raising the temperature from 1000 ℃ to 1200 ℃ and preserving heat for 2 h.
6) Repeating the steps (3) to (5) for multiple times until the density of the carbon/carbon composite material reaches 1.3 g/cm 3 And obtaining the porous carbon matrix with uniform pore structure.
7) And (3) putting the carbon/carbon composite material into a siliconizing furnace, heating to 1500 ℃ in a pressure environment of less than 20 Pa, preserving the temperature for 1 h, and allowing liquid silicon to permeate into pores of the prefabricated body and react with carbon to form a silicon carbide substrate.
The morphology of the carbon matrix of the carbon/carbon composite obtained in step (6) of this example is shown in fig. 1. It can be seen that the prepared carbon matrix is in a three-dimensional network communication structure, and the pore diameter and the size of the carbon skeleton are both in nanoscale distribution. Prepared porous carbonThe pore size distribution of the/carbon composite is shown in fig. 2. Wherein the nano-scale peaks correspond to the mesopores of the carbon matrix, the mesopores are mainly distributed between 10 nm and 80 nm, and the median pore diameter is 43.3 nm. Whereas large-sized pores of about 10 μm are residual pores in a small portion of the unfilled preform. The density of the C/SiC composite material prepared in the example is 2.15 g/cm 3 The shape of the silicon carbide substrate is shown in fig. 3, and it can be seen that the sizes of crystal grains in the formed silicon carbide substrate are all tens of nanometers. FIG. 4 is the morphology of the carbon fiber reinforced silicon carbide composite in example 1. It can be seen that the porous carbon matrix is fully converted to a dense silicon carbide matrix and that the pyrolytic carbon layer remains intact with the carbon fibers after reaction and is not etched. Therefore, the three-point bending strength of the material is as high as 271.1 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 0.52 g/cm 3 。
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 h, and the density of the carbon felt reaches 0.65 g/cm 3 。
3) Preparing phenolic resin, ethylene glycol and benzene sulfonyl chloride into a precursor solution according to the mass ratio of 11.
4) And (3) placing the felt body in a curing furnace for curing, and keeping the temperature within the temperature range of 180 to 250 ℃ for 40 hours under the pressure of 4 MPa.
5) The felt body is put in a vacuum carbonization furnace for carbonization, and the process is as follows: heating from 20 ℃ to 220 ℃ and preserving heat for 0.5 h, heating from 220 ℃ to 550 ℃ and preserving heat for 3 h, heating from 550 ℃ to 750 ℃ and preserving heat for 4 h, heating from 750 ℃ to 1000 ℃ and preserving heat for 2 h, and heating from 1000 ℃ to 1200 ℃ and preserving heat for 2 h.
6) Repeating the steps (3) to (5) until the density of the porous carbon/carbon composite material reaches 1.3 g/cm 3 。
7) And (3) putting the carbon/carbon composite material into a siliconizing furnace, heating to 1500 ℃ in a pressure environment of less than 20 Pa, preserving the temperature for 1 h, and allowing liquid silicon to permeate into pores of the prefabricated body and react with carbon to form a silicon carbide substrate.
8) The density of the sample was 2.10 g/cm 3 The three-point bending strength was 234.9 MPa.
The pore size distribution of the carbon/carbon composite material prepared in this example is shown in fig. 5. Wherein the nano-scale peaks correspond to the mesopores of the carbon matrix, the mesopores are mainly distributed between 10 nm and 80 nm, and the median pore diameter is 44.7 nm. The density of the C/SiC composite material prepared in the example is 2.10 g/cm 3 The morphology of the material under different magnifications is shown in fig. 6, and it can be seen that the porous carbon matrix is completely converted into a dense silicon carbide matrix, and the pyrolytic carbon layer and the carbon fibers are still completely preserved and are not etched after the reaction. FIG. 7 is a composition of a carbon fiber reinforced silicon carbide composite material in example 2. The prepared C/SiC composite material comprises a carbon peak and a silicon carbide peak without a silicon peak, which indicates that a porous carbon matrix is converted into a silicon carbide matrix in the reaction process, and the infiltrated liquid silicon is completely consumed in the reaction process. The stress-displacement curve of the prepared C/SiC is shown in FIG. 8, the three-point bending strength of the material is 234.9 MPa, and the bending stress of the material is slowly reduced along with the increase of the displacement in the fracture process, which indicates that the material is in pseudo-plastic fracture rather than brittle fracture. The pseudo-plastic fracture behavior also indicates that the carbon fibers in the composite are not etched.
Claims (10)
1. A method for preparing a silicon carbide-based composite material by uniformly ceramizing porous carbon is characterized by comprising the following steps: firstly, preparing a porous carbon matrix with the porosity of 45-58%, and then carrying out siliconizing treatment to obtain the silicon carbide-based composite material; the method specifically comprises the following steps:
(1) Dipping treatment: soaking the carbon fiber or ceramic fiber preform in a precursor solution for a period of time and then taking out the carbon fiber or ceramic fiber preform;
(2) High-pressure assisted phase separation and curing treatment: pressurizing the carbon or ceramic fiber preform soaked with the precursor solution to 1 to 10 MPa, rapidly heating to a curing temperature, and forming a porous organic matrix with a uniform pore structure in the fiber preform under the conditions of external pressure and high curing temperature to obtain the fiber-reinforced nano porous resin matrix composite material;
(3) Carbonizing treatment: carrying out high-temperature carbonization treatment on the fiber-reinforced nano porous resin matrix composite material obtained in the step (2) to obtain a low-density porous carbon-based infiltration preform;
(4) Repeating the processes of soaking, curing and carbonizing in the steps (1) - (3) for multiple times until a porous carbon-based infiltration preform with the required density is obtained;
(5) Siliconizing treatment: and (4) carrying out low-temperature melting siliconizing treatment on the porous carbon-based infiltration preform obtained in the step (4) to obtain the fiber-reinforced silicon carbide composite material.
2. The method for preparing the silicon carbide-based composite material through the uniform ceramization of porous carbon according to claim 1, wherein: the precursor solution is prepared by mixing and uniformly stirring phenolic resin, ethylene glycol and a curing agent according to the weight ratio of (10) - (15) to (11) - (16) to (1) - (2); in the precursor solution, the phenolic resin can be common commercial-grade resin or modified boron phenolic aldehyde, barium phenolic aldehyde and the like, and 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 the silicon carbide-based composite material through the uniform ceramization of porous carbon according to claim 1, wherein: in the step (1), the carbon fiber and ceramic fiber preform may have an interface layer, and the interface layer may be one or more of a pyrolytic carbon interface, a silicon carbide interface, or a boron nitride interface.
4. The method for preparing the silicon carbide-based composite material through the uniform ceramization of porous carbon according to claim 1, wherein: in the dipping treatment of the step (1): the pressure range is 0.1 to 9 MPa, the dipping time is 1 to 4 hours, and the dipping treatment is finished when no air bubbles are obvious.
5. The method for preparing the silicon carbide-based composite material through the porous carbon uniform ceramic-coating according to claim 1, wherein the method comprises the following steps: in the step (2), the curing temperature is 120 to 250 ℃, and the heating rate is more than 10 ℃/min; the porous organic matrix formed in the fiber preform has a three-dimensional network skeleton structure with the characteristic of small pore diameter (less than 100 nm).
6. The method for preparing the silicon carbide-based composite material through the uniform ceramization of porous carbon according to claim 1, wherein: in the step (3), the carbonization treatment process is as follows: and (3) placing the fiber reinforced nano porous resin matrix composite material obtained after curing treatment in a vacuum carbonization furnace, heating the vacuum carbonization furnace to 1200-1800 ℃ at the heating rate of 5-10 ℃/min, and preparing a carbon matrix with uniformly distributed nano pores on the surface of the fiber by cracking the organic matrix and combining micropores under a high-temperature condition, so as to obtain the porous carbon/carbon composite material (the porous carbon-based infiltration preform).
7. The method for preparing the silicon carbide-based composite material through the uniform ceramization of porous carbon according to claim 1, wherein: in the step (4), in the obtained porous carbon-based infiltration preform, the pore size distribution range of the carbon-based body is 10-80 nm, and the pore size of the mesopore is 40-45 nm.
8. The method for preparing the silicon carbide-based composite material through the uniform ceramization of porous carbon according to claim 1, wherein: in the step (5), in the siliconizing treatment process, the siliconizing temperature is 1450 to 1550 ℃, the heat preservation time is 1 to 2 hours, the particle size of the used silicon powder is 10 mu m-2 mm, and the pressure in the siliconizing process is less than 20 Pa.
9. The method for preparing the silicon carbide-based composite material through the uniform ceramization of porous carbon according to claim 1, wherein: in the step (4), the porosity of the porous carbon substrate obtained after carbonization is calculated according to the matching relationship between the porosity P of the porous carbon substrate and the volume expansion rate under the ideal condition that dense silicon carbide is generated after the porous carbon reacts: p =1-V m C/V m SiC, wherein: v m C is the molar volume of the porous carbon matrix, V m SiC is the molar volume of the compact silicon carbide matrix.
10. The method for preparing the silicon carbide-based composite material through the porous carbon uniform ceramic-coating according to claim 1, wherein the method comprises the following steps: the silicon carbide substrate obtained in the step (5) is compact and has no carbon residue or silicon residue, and the grain size of the silicon carbide is 50-100 nm; and the fiber in the composite material is not etched after the reaction.
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