CN116063091A - Three-dimensional continuous porous carbon-based preform and application thereof in preparation of SiC-based composite material - Google Patents
Three-dimensional continuous porous carbon-based preform and application thereof in preparation of SiC-based composite material Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic nonmetallic hybrid metal matrix composite material preparation, in particular to a three-dimensional continuous porous carbon-based preform and application thereof in preparing a SiC-based composite material, and aims at solving the problems that when the SiC-based composite material is prepared by using porous carbon as a single carbon matrix and Si-Al as a main penetrating agent and performing reaction infiltration at the temperature below 1400 ℃, the reinforcing phase has high-temperature reaction damage or insufficient effective infiltration depth, a porous carbon skeleton-three-dimensional continuous porous carbon-based preform is provided, and the porous carbon skeleton-three-dimensional continuous porous carbon-based preform is applied to the preparation of the SiC-based composite material, so that the problems of the high-temperature reaction damage of the reinforcing phase, the serious reduction of the reaction infiltration rate due to insufficient dynamic activity of carbon and the inhibition of the reaction infiltration due to the wet-heat reaction are solved.
Description
Technical Field
The invention belongs to the technical field of inorganic nonmetallic hybrid metal matrix composite material preparation, and particularly relates to a three-dimensional continuous porous carbon-based preform and application thereof in preparation of SiC-based composite materials.
Background
The SiC-based composite material has excellent properties of low density, heat resistance, wear resistance, ablation resistance and the like, and the self-lubricating, strength, heat conduction, impact resistance and erosion resistance of the SiC-based composite material can be effectively improved by introducing carbon and a communicated metal phase into the SiC-based composite material, and the SiC-based composite material can be widely used as a lightweight thermal structure material for manufacturing cores and key parts of advanced equipment, such as the fields of hot ends of aircrafts, brake parts, armors, combustion chambers of internal combustion engines, bearing bushes, rapid-fire weapon barrels, thermal management and the like.
When the one-dimensional reinforcing phases such as fibers, whiskers, nanowires and the like of carbon and silicon carbide, particularly high-dimensional fabrics thereof are used as the reinforcing phases, the SiC-based composite material is mainly prepared by introducing a chemical vapor infiltration method, a precursor impregnation cracking method, a slurry infiltration method, a vapor phase siliconizing method, a reaction melt infiltration method and the like of a SiC matrix into a porous preform, wherein the reaction infiltration method has a short preparation period, low cost and can be molded in a near-net size relative to the preparation method, but is limited by the melting point (1410 ℃) of Si, and the preparation temperature of the material is usually higher than 1450 ℃. The specific adverse effects of this preparation condition are represented by: on one hand, the silicon carbide rod or the resistance wire cannot be prepared in a heat treatment furnace taking a conventional silicon carbide rod or resistance wire as a heating body, has high equipment requirements and high energy consumption, and is not beneficial to large-area industrial production; on the other hand, the types of the reinforcing phases caused by high temperature are mainly limited to carbon and silicon carbide fibers, so that other one-dimensional reinforcing phases are rarely applied to SiC-based composite materials. Obviously, the preparation temperature is reduced to 1400 ℃, especially below 1200 ℃, which is beneficial to reducing high energy consumption and high equipment requirements, and can greatly widen the optional range of the reinforcing phase and facilitate the design of the composite material.
The inventor researches the microstructure, phase composition, density, strength, erosion, ablation and other performance characteristics of a C/C-SiC-AlSi composite material prepared by low-temperature reaction infiltration at 1100-1200 ℃ when Si-Al powder is taken as a penetrating agent and pyrolytic carbon is taken as a porous C/C carbon matrix in the documents of Ceram.Int.46 (2020) 8469-8472, J.Cent.southwiv.27 (2020) 2557-2566 and DOI:10.1016/j.Ceramint.2022.10.280, and discovers that different degrees of reaction damage exist in fibers when textured carbon in vapor deposition is taken as a porous C/C carbon matrix. In the further research process, the Si-Al powder below 1400 ℃ is used as a main penetrating agent, carbon with low technical requirements such as resin carbon is used as a porous carbon matrix, and although texture carbon in thermodynamics and vapor deposition presents similar reaction characteristics, the dynamic characteristic difference of reaction infiltration is huge, the effective penetration depth is less than 1mm, and simultaneously the penetration effect and the material performance are obviously influenced by the porous carbon, the Si-Al powder, the humidity of a heat treatment furnace and the like.
Disclosure of Invention
Aiming at the problems that the reinforcing phase is damaged by high-temperature reaction or the effective penetration depth is insufficient when the porous carbon is taken as a single carbon matrix and the Si-Al is taken as a main penetrating agent to prepare the SiC-based composite material by reaction infiltration at the temperature below 1400 ℃, the invention provides a porous carbon skeleton-three-dimensional continuous porous carbon-based preform and is applied to the preparation of the SiC-based composite material, and aims to solve the problems that the reinforcing phase is damaged by high-temperature reaction, the dynamic activity of carbon is insufficient to seriously reduce the reaction infiltration rate and the damp-heat reaction inhibits the reaction infiltration.
In order to solve the technical problems, the invention adopts the following technical scheme:
a three-dimensional continuous porous carbon-based preform, the microstructure unit of which is composed of a reinforcing phase, a first layer of carbon coating the reinforcing phase and a second layer of carbon as a permeable pore wall which are sequentially arranged from inside to outside; the reinforcing phase is at least one of fiber, whisker and nanowire, and the components of the reinforcing phase are selected from carbon, silicon carbide, basalt or mullite;
the first layer of carbon of the coating reinforcing phase is selected from resin carbon, pitch carbon or vapor deposition isotropic carbon, and the second layer of carbon used as a penetrating pore wall is selected from vapor deposition medium texture carbon, high texture carbon or pyrolytic graphite.
Preferably, in the three-dimensional continuous porous carbon-based preform, the volume percentage of the reinforcing phase is 10-30vol.%, the volume percentage of the first layer of carbon coating the reinforcing phase is 5-30vol.%, the volume percentage of the second layer of carbon serving as a permeable pore wall is 5-50vol.%, and the balance is pores.
The invention also protects the application of the three-dimensional continuous porous carbon-based preform in preparing the SiC-based composite material, wherein the three-dimensional continuous porous carbon-based preform is used for preparing the SiC-based composite material by infiltration at the reaction temperature of 900-1400 ℃ when Si-Al is used as a main infiltration agent.
Preferably, the application method comprises the following steps:
(1) Machining, polishing and cleaning the three-dimensional continuous porous carbon-based preform, drying to constant weight to obtain a dried porous carbon test piece to be infiltrated, and sealing and preserving;
(2) Uniformly mixing the main penetrating agent, drying to constant weight to obtain dry mixed powder to be penetrated, and sealing and preserving;
(3) Placing the porous carbon test piece to be infiltrated in the step (1) into the mixed powder to be infiltrated in the step (2), preserving heat for 30-180min in a dry heat treatment furnace at 900-1400 ℃ and under the vacuum condition less than 1kPa, and then cooling to room temperature through stress relief annealing or directly cooling to room temperature to remove surface residual powder, thereby obtaining the SiC-based composite material.
Preferably, the main penetrating agent in the step (2) is composed of the following raw materials in parts by weight: 5-9 parts of Si powder, 1-5 parts of Al powder and less than 2 parts of X powder;
wherein the X powder is selected from Mg, cu, fe, ni, W, cr, mn, mo, ag, ti, zr, hf, B, or Mg, cu, fe, ni, W, cr, mn, mo, ag, ti, zr, hf, B alloy, carbide, boride, oxide, or Al 2 O 3 At least one of the powders.
Preferably, the drying conditions in the step (1) are as follows: drying in a forced air drying oven at 80-300 deg.C for 24-48 hr; the drying conditions in the step (2) are as follows: drying in a forced air drying oven at 80-300 deg.C for 12-24 hr.
Preferably, the destressing annealing operation in the step (3) is carried out by cooling to 450-570 ℃ along with the furnace, preserving heat for 30-180min, and then cooling to room temperature along with the furnace; or cooling to 450 ℃ at a speed of less than or equal to 3 ℃/min, and then cooling to room temperature along with the furnace.
Preferably, the drying method of the heat treatment furnace in (3) comprises the following steps: heating the sealed heat treatment furnace to 200-500 ℃, preserving heat for 0.5-6h, vacuumizing to <1kPa in the whole process, and then cooling to room temperature.
Compared with the prior art, the invention has the beneficial effects that:
1. the whole preparation process of the SiC-based composite material is lower than 1400 ℃, namely the SiC-based composite material can be implemented in a heat treatment furnace taking a silicon carbide rod, a resistance wire and the like as heating elements, the preparation temperature is reduced, so that an optional reinforcing phase is expanded to basalt, mullite and the like from carbon and silicon carbide, and compared with the conventional preparation of the SiC-based composite material by reaction infiltration, the SiC-based composite material has low energy consumption, is convenient for industrialized mass production and has strong material designability;
2. the porous carbon matrix is of a double-carbon layer structure and is formed by sequentially coating two reinforcing phases by carbon, the reaction kinetic activity of the first layer of carbon and Si-Al is very weak, and the phenomenon that the reinforcing phases are damaged by chemical reaction generated by excessive reaction of Si-Al melt and the reinforcing phases when the Si-Al melt reacts and infiltrates the carbon matrix can be avoided; the second layer of carbon is used for reacting with Si-Al to realize infiltration, so that the reinforced phase can be effectively protected from reaction damage compared with the single vapor deposition of the textured carbon and other substrates, and infiltration can be effectively promoted compared with the single resin carbon and other substrates; aiming at the defect that the pore structure of the porous carbon is poor due to the double-layer carbon structure, and the inhibition of the reaction infiltration of the Si-Al infiltration agent by the alumina formed by the wet-heat reaction is effectively relieved by combining the porous carbon, infiltration powder and the humidity control of a heat treatment furnace; thereby realizing the preparation of the SiC-based composite material with single-side penetration depth reaching more than 5 mm.
3. Porous carbon and powder are easy to absorb moisture, and excessive water vapor can cause excessive Al at high temperature 2 O 3 Ceramic phase formation, thereby impeding the reaction of the si—al melt with carbon; in addition, al melt is easy to dissolve and adsorb H-containing gas in a high-humidity environment such as a rainy day, and casting defects such as pinholes are formed by precipitation during cooling and solidification; the drying treatment in the preparation of the material is to reduce the vapor in the porous carbon, the powder and the heat treatment furnace, thereby avoiding the excessive vapor absorption of Al; in addition, the water vapor content is reducedThe humidity can avoid the defects of pinholes and the like formed during the solidification of Al, so that the performance of the composite material is reduced; the porous carbon drying and sealing preservation, powder drying and sealing preservation and drying treatment before the use of the heat treatment furnace are all used for reducing the negative influence of vapor in air on infiltration and realizing the regulation and control of humidity.
Drawings
FIG. 1 is a schematic diagram of a two-carbon layer structure of a three-dimensional continuous porous carbon-based preform according to embodiments 1-3 of the present invention, wherein the left view is a macroscopic morphology diagram of the three-dimensional continuous porous carbon-based preform, and the right view is a schematic diagram of the microstructure of the three-dimensional continuous porous carbon-based preform;
FIG. 2 is a macroscopic view of the SiC-based composite material obtained after infiltration of Si-Al-Cu by low temperature reaction of the three-dimensional continuous porous carbon-based preform of example 1 of the present invention;
FIG. 3 is a micro-domain SEM contrast graph of the SiC-based composite material obtained by infiltration of Si-Al-Cu by a low temperature reaction of the single carbon layer of comparative example 1 and the dual carbon layer of the three-dimensional continuous porous carbon-based preform of example 1, respectively, wherein the left graph is the SiC-based composite material obtained by infiltration of Si-Al-Cu by a low temperature reaction of the single carbon layer of comparative example 1, and the right graph is the SiC-based composite material obtained by infiltration of Si-Al-Cu by a low temperature reaction of the three-dimensional continuous porous carbon-based preform of example 1;
FIG. 4 shows a low temperature reaction infiltration Si-Al-ZrB of a three-dimensional continuous porous carbon-based preform according to example 2 of the present invention 2 XRD patterns of the obtained composite material, wherein small patterns in the XRD patterns are low-temperature reaction infiltration Si-Al-ZrB 2 Macroscopic view of the resulting composite.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The experimental methods described in the examples of the present invention are conventional methods unless otherwise specified.
The preparation of the three-dimensional continuous porous carbon-based preform can be realized by performing resin/pitch impregnation-carbonization, chemical vapor deposition and other well-known methods on reinforced phase fabrics; the three-dimensional continuous porous carbon-based preform can also be prepared by mixing the reinforcing phase with an alcoholic solution of a resin to prepare slurry, and performing suction filtration molding, drying, curing and carbonization, and also belongs to a well-known method in the field.
Example 1
The method for preparing the SiC-based composite material by adopting the three-dimensional continuous porous carbon-based preform comprises the following steps:
preparing a three-dimensional continuous porous carbon-based preform with a double-carbon layer structure by selecting 2.5D needled carbon fiber felt (reinforcing phase), vapor deposition isotropic carbon coated on carbon fiber (first carbon layer coated with reinforcing phase), and texture carbon in vapor deposition (second carbon layer used as permeation hole wall), and preparing a C/C-SiC composite material by reaction infiltration of Si-Al-Cu serving as a penetrant at 1200 ℃ and a vacuum degree lower than 10Pa, wherein the 2.5D needled carbon fiber felt accounts for 25vol.%, the vapor deposition isotropic carbon coated on carbon fiber accounts for 5vol.%, the texture carbon accounts for 30vol.% in vapor deposition of the second carbon layer used as permeation hole wall, and the balance is pore space; the preparation method of the SiC-based composite material comprises the following specific steps:
(1) Preparation of a three-dimensional continuous porous carbon-based preform:
the preparation method of the carbon matrix by adopting the thermal gradient chemical vapor deposition method comprises the following steps: natural gas is used as carbon source gas, a 2.5D needled carbon fiber felt is clamped between two electrodes of a thermal gradient vapor deposition furnace, the deposition temperature is controlled to 1000 ℃, and the gas flow rate is controlled to 0.4m 3 Depositing for 0.5h to finish the preparation of the first layer of carbon, namely vapor deposition isotropic carbon; then heating to 1100 ℃ and setting the gas flow rate to 1.0m 3 Depositing for 4 hours to finish the preparation of the second layer of carbon, namely texture carbon in vapor deposition, so as to prepare the three-dimensional continuous porous carbon-based preform;
(2) Preparing a SiC-based composite material by adopting a three-dimensional continuous porous carbon-based preform:
s1, sawing the porous carbon into square block samples, ultrasonically cleaning the square block samples in distilled water for 30min, repeatedly cleaning the square block samples for three times, drying the square block samples for more than 24 hours at 150 ℃ in a blast drying box with humidity less than or equal to 30%, drying the square block samples to constant weight to obtain porous carbon square block samples to be infiltrated, and placing the porous carbon square block samples in a wide-mouth bottle with a drying agent and a bottle stopper;
s2, weighing 7 parts of silicon powder, 3 parts of aluminum powder and 0.5 part of Cu powder, manually stirring for more than 4 hours by using a mortar and a grinding rod until the mixture is uniformly mixed, then drying the mixture in a blast drying box with humidity less than or equal to 30% at 100 ℃ for more than 12 hours, drying the mixture to constant weight to obtain mixed powder to be infiltrated, and sealing and storing the mixed powder in a vacuum drying box;
s3, heating the closed heat treatment furnace to 200 ℃, preserving heat for 60min, continuously vacuumizing by a whole-course rotary-vane mechanical vacuum pump, and then cooling to room temperature to obtain a dry heat treatment furnace;
s4, placing the dried porous carbon sample obtained in the first step into the dried mixed powder obtained in the second step, placing the dried porous carbon sample into a dried heat treatment furnace obtained in the third step within 60min, heating to 1200 ℃, preserving heat for 120min under the vacuum condition of less than 10Pa, and then directly cooling to room temperature along with furnace cooling after power failure to obtain the C/C-SiC-SiAlCu-based composite material.
Example 2
The method for preparing the SiC-based composite material by adopting the three-dimensional continuous porous carbon-based preform comprises the following steps:
preparing a three-dimensional continuous porous carbon-based preform with a double-carbon layer structure by adopting a chopped carbon fiber needled felt (reinforcing phase), resin carbon (first layer carbon coating the reinforcing phase) and vapor deposition high-texture carbon (second layer carbon as penetrating pore walls), wherein the three-dimensional continuous porous carbon-based preform is Si-Al-ZrB 2 Preparing a C/C-SiC composite material by reaction infiltration of a penetrant at 1400 ℃ and under vacuum of less than 1000Pa, wherein a chopped carbon fiber needled felt accounts for 10vol.%, a resin carbon coated on carbon fibers accounts for 30vol.%, a vapor deposition high-texture carbon serving as a second layer carbon of a infiltration hole wall accounts for 5vol.%, and the balance is pores; the preparation method of the SiC-based composite material comprises the following specific steps:
(1) Preparation of a three-dimensional continuous porous carbon-based preform:
preparation of a first layer of resin carbon: placing a chopped carbon fiber needled felt in a vacuum tank by taking phenolic resin as a carbon source, vacuumizing to below 5kPa for 40min, then introducing 30wt.% of absolute ethyl alcohol solution of the phenolic resin into the vacuum tank until the carbon felt is completely covered, taking out the carbon felt, drying at 80 ℃ for 24h, placing the carbon felt in a heat treatment furnace, heating to 220 ℃ for 2h, continuously heating to 900 ℃ for 2h, and cooling to room temperature to finish the preparation of a resin carbon layer;
preparation of a second layer of high-texture carbon: adopting isothermal chemical vapor deposition method, taking natural gas as carbon source gas, placing porous C/C prepared with resin carbon in vapor deposition furnace, clamping graphite tool, controlling deposition temperature at 1000-1200deg.C, and gas flow rate at 0.6m 3 And (3) depositing for 2 hours to finish the preparation of the high-texture carbon layer; thereby preparing a three-dimensional continuous porous carbon-based preform;
(2) Preparing a SiC-based composite material by adopting a three-dimensional continuous porous carbon-based preform:
s1, cutting the porous carbon wire into a cake sample, ultrasonically cleaning the cake sample in absolute ethyl alcohol for 60min, repeatedly cleaning the cake sample for three times, drying the cake sample in a blast drying box with humidity less than or equal to 40% at 300 ℃ for more than 24h, drying the cake sample to constant weight to obtain a porous carbon square sample to be infiltrated, and placing the porous carbon square sample in a vacuum drying box;
s2, weighing 9 parts of silicon powder, 1 part of aluminum powder and 1 part of ZrB 2 Mixing the powder uniformly by using a planetary ball mill in a polytetrafluoroethylene ball milling tank and using agate balls, then drying the powder for more than 12 hours at 300 ℃ in a blast drying box with humidity less than or equal to 40%, drying the powder to constant weight to obtain mixed powder to be infiltrated, and sealing and storing the mixed powder in a vacuum drying box;
s3, heating the closed heat treatment furnace to 1000 ℃, preserving heat for 30min, continuously pumping coarse vacuum through a whole-course rotary-vane mechanical vacuum pump, and then cooling to room temperature to obtain a dry heat treatment furnace;
s4, placing the dried porous carbon sample obtained in the first step into the dried mixed powder obtained in the second step, placing the dried porous carbon sample into a dried heat treatment furnace obtained in the third step within 30min, heating to 1400 ℃ and preserving heat for 30min under the vacuum condition of lower than 1000Pa, cooling to 500 ℃ along with the furnace, preserving heat for 120min, and then cooling to room temperature along with the furnace after power failure to obtain the C/C-SiC-SiAl-ZrB 2 A base composite material.
Example 3
The method for preparing the SiC-based composite material by adopting the three-dimensional continuous porous carbon-based preform comprises the following steps:
this embodiment is a mullite fiber reinforced SiC-based composite,preparing a three-dimensional continuous porous carbon-based preform with a double-carbon layer structure by using chopped mullite fiber (reinforcing phase), resin carbon (first carbon layer coating the reinforcing phase) and textured carbon (second carbon layer as penetrating pore wall) in vapor deposition 2 O 3 Preparing a C/C-SiC composite material by performing reaction infiltration at the temperature of 1000 ℃ under vacuum of less than 500Pa as a penetrating agent, wherein the mullite fiber accounts for 30vol.%, the resin carbon coated on the mullite fiber accounts for 10vol.%, the texture carbon accounts for 20vol.% in vapor deposition of the second layer of carbon as a penetrating hole wall, and the balance is pores; the preparation method of the SiC-based composite material comprises the following specific steps:
(1) Preparation of a three-dimensional continuous porous carbon-based preform:
mechanically mixing mullite fiber with the length of 3-5mm with 20wt.% furan resin alcohol solution to prepare slurry, carrying out negative pressure suction filtration and molding, then placing the molded embryo body in a corundum crucible and placing in a heat treatment furnace, and carrying out heat treatment for 2 hours at 850 ℃ under the conditions of nitrogen atmosphere and atmospheric pressure to prepare porous carbon of resin carbon coated chopped mullite fiber;
adopting a thermal gradient chemical vapor deposition method, taking natural gas as carbon source gas, and clamping the porous carbon of the resin carbon coated chopped mullite fiber between two electrodes of a thermal gradient vapor deposition furnace; controlling the deposition temperature at 1050-1150 ℃ and setting the gas flow rate at 1.0m 3 And/h, depositing for 3h, and completing the preparation of the second layer of carbon, namely texture carbon in vapor deposition, so as to prepare a three-dimensional continuous porous carbon-based preform;
(2) Preparing a SiC-based composite material by adopting a three-dimensional continuous porous carbon-based preform:
s1, turning the porous carbon into a cylindrical sample, ultrasonically cleaning the cylindrical sample in tap water for 40min, repeatedly cleaning the cylindrical sample for three times, drying the cylindrical sample for more than 24 hours at 80 ℃ in a blast drying box with humidity less than or equal to 40%, drying the cylindrical sample to constant weight to obtain a porous carbon square sample to be infiltrated, and placing the porous carbon square sample in a vacuum drying box;
s2, weighing 5 parts of silicon powder, 5 parts of aluminum powder and 2 parts of Al 2 O 3 Mixing the powder with corundum balls in a polytetrafluoroethylene ball milling tank by using a roller ball mill, drying the powder for more than 12 hours at 80 ℃ in a blast drying box with humidity less than or equal to 40%, and drying the powder to constant weightObtaining mixed powder to be infiltrated, and sealing and storing in a vacuum drying oven;
s3, heating the closed heat treatment furnace to 500 ℃, preserving heat for 30min, continuously pumping coarse vacuum through a whole-course rotary-vane mechanical vacuum pump, and then cooling to room temperature to obtain a dry heat treatment furnace;
s4, placing the dried porous carbon sample obtained in the first step into the dried mixed powder obtained in the second step, placing the dried porous carbon sample into a dried heat treatment furnace obtained in the third step within 120min, heating to 1000 ℃, preserving heat for 180min under the vacuum condition of less than 500Pa, then cooling to 450 ℃ at the speed of not more than 3 ℃/min, and then cooling to room temperature along with the furnace after power failure, thus obtaining the mullite fiber reinforced hybrid SiC-based composite material.
Example 4
The procedure was identical to that of example 1, except that:
s3, heating the closed heat treatment furnace to 200 ℃, preserving heat for 6 hours, continuously vacuumizing by a whole-course rotary-vane mechanical vacuum pump, and then cooling to room temperature to obtain a dry heat treatment furnace;
s4, placing the dried porous carbon sample obtained in the first step into the dried mixed powder obtained in the second step, placing the dried porous carbon sample into a dried heat treatment furnace obtained in the third step within 60min, heating to 900 ℃, preserving heat for 180min under the vacuum condition of less than 10Pa, and then directly cooling to room temperature along with furnace cooling after power failure to obtain the C/C-SiC-SiAlCu-based composite material.
Comparative example 1
The same procedure as in example 1 was followed except that this comparative example used a single layer of carbon to prepare the SiC-based composite material, i.e., the three-dimensional continuous porous carbon-based preform of example 1 was replaced with a single layer of carbon, which was prepared as follows: adopting a thermal gradient chemical vapor deposition method, taking natural gas as carbon source gas, clamping a 2.5D needled carbon fiber felt between two electrodes of a thermal gradient vapor deposition furnace, controlling the deposition temperature to 1100 ℃ and controlling the gas flow rate to be 1.0m 3 And (5) depositing for 5 hours to finish the preparation of the texture carbon single-carbon layer structure in the vapor deposition.
The results of fig. 1 show that the three-dimensional continuous porous carbon (three-dimensional continuous porous carbon-based preform) is a bulk porous body composed of two kinds of microstructure units of carbon sequentially coated with a reinforcing phase.
The macroscopic morphology of the C/C-SiC-SiAlCu-based composite material of the example 1 is shown in figure 2; the vapor deposition isotropic carbon coated with carbon fiber in the process of forming the composite material by reaction infiltration prevents random unoriented reaction of Si activated by Al, so that the fiber is well protected, and meanwhile, the unilateral infiltration depth of the reaction infiltration is about 10mm, and compared with the effective infiltration depth of the porous carbon of single isotropic carbon, the method is remarkably improved; in addition, the compression strength reaches 220MPa, and the strength of the C/C-SiC-SiAl obtained by the same process is improved by about 10 percent compared with the Si/Al ratio and the C/C-SiC-SiAl obtained by the same process disclosed in 'microstructural and magnetic property of C/C-SiCcompositesprepared byreactivemeltinfiltrationatlowtemperatureinvacuum'.
The microstructure comparison chart of the composite material prepared by the porous carbon with the single carbon layer is shown in the figure 3, and the result of the figure 3 shows that the fiber reaction is damaged when the porous carbon is a single carbon layer matrix, and the fiber is protected by the first layer of low-reaction active carbon and is not damaged when the porous carbon is a double carbon layer matrix.
The XRD pattern of the C/C-SiC-SiAl-ZrB 2-based composite material of example 2 is shown in figure 4, and the density of the prepared composite material is more than 2.0g/cm 3 The density is measured according to the mass and the volume, and the unilateral penetration depth reaches more than 5 mm.
EXAMPLE 3 mullite fiber reinforced hybrid SiC-based composite having a density greater than 2.2g/cm 3 The unilateral penetration depth reaches more than 5mm, the forefront of the infiltration reaction stops at the interface of the two carbon layers, and the fiber is not damaged by reaction.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof. The above-described embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of protection is not limited thereto. Equivalent substitutions and modifications are intended to be within the scope of the present invention, as will be apparent to those skilled in the art based upon the present disclosure.
Claims (8)
1. The three-dimensional continuous porous carbon-based preform is characterized in that microstructure units of the three-dimensional continuous porous carbon-based preform consist of a reinforcing phase, a first layer of carbon coating the reinforcing phase and a second layer of carbon serving as a permeable pore wall, which are sequentially arranged from inside to outside; the reinforcing phase is at least one of fiber, whisker and nanowire, and the components of the reinforcing phase are selected from carbon, silicon carbide, basalt or mullite;
the first layer of carbon of the coating reinforcing phase is selected from resin carbon, pitch carbon or vapor deposition isotropic carbon, and the second layer of carbon used as a penetrating pore wall is selected from vapor deposition medium texture carbon, high texture carbon or pyrolytic graphite.
2. The three-dimensional continuous porous carbon-based preform according to claim 1, wherein the volume percentage of the reinforcing phase in the three-dimensional continuous porous carbon-based preform is 10 to 30vol.%, the volume percentage of the first layer of carbon coating the reinforcing phase is 5 to 30vol.%, the volume percentage of the second layer of carbon as the walls of the infiltration pores is 5 to 50vol.%, and the balance is pores.
3. Use of a three-dimensional continuous porous carbon-based preform according to claim 1 for preparing a SiC-based composite material by infiltration at a reaction temperature of 900-1400 ℃ when Si-Al is the main infiltrant.
4. The use according to claim 3, characterized in that the application method is:
(1) Machining, polishing and cleaning the three-dimensional continuous porous carbon-based preform, drying to constant weight to obtain a dried porous carbon test piece to be infiltrated, and sealing and preserving;
(2) Uniformly mixing the main penetrating agent, drying to constant weight to obtain dry mixed powder to be penetrated, and sealing and preserving;
(3) Placing the porous carbon test piece to be infiltrated in the step (1) into the mixed powder to be infiltrated in the step (2), preserving heat for 30-180min in a dry heat treatment furnace at 900-1400 ℃ and under the vacuum condition less than 1kPa, and then cooling to room temperature through stress relief annealing or directly cooling to room temperature to remove surface residual powder, thereby obtaining the SiC-based composite material.
5. The use according to claim 4, wherein the main penetrant of step (2) is composed of the following raw materials in parts by weight: 5-9 parts of Si powder, 1-5 parts of Al powder and less than 2 parts of X powder;
wherein the X powder is selected from Mg, cu, fe, ni, W, cr, mn, mo, ag, ti, zr, hf, B, or Mg, cu, fe, ni, W, cr, mn, mo, ag, ti, zr, hf, B alloy, carbide, boride, oxide, or Al 2 O 3 At least one of the powders.
6. The use according to claim 4, wherein the drying conditions of step (1) are: drying in a forced air drying oven at 80-300 deg.C for 24-48 hr; the drying conditions in the step (2) are as follows: drying in a forced air drying oven at 80-300 deg.C for 12-24 hr.
7. The use according to claim 4, wherein the heat treatment furnace in (3) is dried by: heating the sealed heat treatment furnace to 200-500 ℃, preserving heat for 0.5-6h, vacuumizing to <1kPa in the whole process, and then cooling to room temperature.
8. The use according to claim 4, wherein the destressing annealing operation in step (3) is furnace cooled to 450-570 ℃ and kept for 30-180min, and then furnace cooled to room temperature; or cooling to 450 ℃ at a speed of less than or equal to 3 ℃/min, and then cooling to room temperature along with the furnace.
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