CN113929480A - C/SiC ceramic matrix composite material and preparation method thereof - Google Patents

C/SiC ceramic matrix composite material and preparation method thereof Download PDF

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CN113929480A
CN113929480A CN202111341985.0A CN202111341985A CN113929480A CN 113929480 A CN113929480 A CN 113929480A CN 202111341985 A CN202111341985 A CN 202111341985A CN 113929480 A CN113929480 A CN 113929480A
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composite material
carbon fiber
powder
reaction
silicon
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CN113929480B (en
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杨小健
刘俊鹏
于艺
于新民
刘伟
郑旭
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Aerospace Research Institute of Materials and Processing Technology
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    • C04B35/573—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 by reaction sintering or recrystallisation
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632—Organic additives
    • C04B35/634—Polymers
    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • 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
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Abstract

The invention provides a preparation method of a C/SiC ceramic matrix composite, which comprises the following steps: (1) placing the short carbon fiber prepreg strips in a die cavity, and sequentially carrying out die pressing treatment and cracking reaction to obtain a carbon fiber framework; (2) mixing the carbon fiber skeleton and solid powder, and sequentially carrying out mould pressing treatment and cracking reaction to obtain a composite material green body; (3) adopting a chemical vapor deposition method to perform densification treatment on the composite material green body to obtain a densified composite material green body; (4) and mixing the densified composite material green blank with silicon powder and then carrying out a silicon infiltration reaction to obtain the C/SiC ceramic matrix composite material. The preparation method is simple and low in cost, and the prepared ceramic matrix composite material is uniform in mechanical property, excellent in high temperature resistance and friction performance and wide in application prospect in automobile brake disc materials.

Description

C/SiC ceramic matrix composite material and preparation method thereof
Technical Field
The invention relates to the technical field of composite materials, in particular to a C/SiC ceramic matrix composite material and a preparation method thereof, which can be applied to the preparation of an automobile brake disc.
Background
The conventional preparation method of the carbon fiber reinforced ceramic matrix composite material comprises the processes of CVI (chemical vapor infiltration) + PIP (precursor impregnation cracking), CVI (chemical vapor infiltration) + RMI (silicon infiltration) and the like; the processes mainly rely on a prefabricated body woven by long carbon fibers as a matrix skeleton and toughening components, and then ceramic-based materials are gradually filled around the prefabricated body, so that the strong heat-resistant composite material with a compact and hard structure and certain toughness is finally formed. In the preparation process, the fiber preform can be made into the required fiber orientation through different weaving processes, so that the requirements of the composite material on the shape and the performance are met. However, in the cost accounting of material preparation, the long carbon fiber woven fabric occupies a high proportion, and the preform requires a certain preparation and turnaround time.
The mould pressing is a common material forming process, and the material is formed and shaped in a fixed space by providing a certain temperature and pressure for substances in a cavity. However, in the prior art, the chopped fibers and the resin powder are directly molded, and the chopped fibers inevitably flow in the melted resin powder matrix in the molding process; under the action of gravity, the chopped carbon fibers are finally distributed in a high X-Y plane and low Z direction orientation state, so that the toughening effect is uneven, and the mechanical property anisotropy of the prepared composite material is obvious, thereby seriously stopping the use of the chopped carbon fiber toughened ceramic matrix composite material. Therefore, there is a need to develop a ceramic matrix composite material with uniform mechanical properties, simple method and low cost.
The Chinese patent 201810348023.X discloses a method for preparing an automobile brake disc by die pressing chopped carbon fibers, wherein the chopped carbon fibers and resin powder are used for die pressing to prepare a blank, and the blank is assisted by a CVI + RMI process to prepare the ceramic matrix composite. However, in compression molding, the chopped carbon fibers flow in the resin matrix, eventually making the composite material mechanically anisotropic.
Disclosure of Invention
The invention provides a C/SiC ceramic matrix composite and a preparation method thereof, the preparation method is simple and low in cost, and the prepared ceramic matrix composite has uniform mechanical properties and excellent high temperature resistance and friction performance.
In a first aspect, the invention provides a preparation method of a C/SiC ceramic matrix composite, which comprises the following steps:
(1) placing the short carbon fiber prepreg strips in a die cavity, and sequentially carrying out die pressing treatment and cracking reaction to obtain a carbon fiber framework;
(2) mixing the carbon fiber skeleton and solid powder, and sequentially carrying out mould pressing treatment and cracking reaction to obtain a composite material green body;
(3) adopting a chemical vapor deposition method to perform densification treatment on the composite material green body to obtain a densified composite material green body;
(4) and mixing the densified composite material green blank with silicon powder and then carrying out a silicon infiltration reaction to obtain the C/SiC ceramic matrix composite material.
Preferably, in step (1), the chopped carbon fiber prepreg strips have a fiber volume fraction of 50% to 85%.
Preferably, in the step (1), the length of the chopped carbon fiber prepreg strip is 10-80 mm, the width of the chopped carbon fiber prepreg strip is 2-10 mm, and the height of the chopped carbon fiber prepreg strip is 1-3 mm.
Preferably, in the step (2), the solid powder comprises phenolic resin powder, carbon powder and silicon powder;
the mass ratio of the sum of the mass of the carbon powder and the silicon powder to the mass of the phenolic resin powder is (1-5): 10.
preferably, the powder particle size of the silicon powder is 35-1000 μm.
Preferably, in the step (1) and the step (2), the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h;
the reaction temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-18 h.
Preferably, in the step (3), the deposition temperature of the chemical vapor deposition method is 900 to 1100 ℃, and the deposition time is 100 to 500 hours.
Preferably, in the step (3), the density of the densified composite material green body is 0.85-1.25 g/cm3。
Preferably, in the step (4), the mass ratio of the densified composite raw blank to the silicon powder is 1: (2-5).
Preferably, in the step (4), the reaction temperature of the silicon infiltration reaction is 1460-1600 ℃, and the reaction time is 0.5-3.5 h.
Preferably, the preparation method comprises the following steps: (1) placing the chopped carbon fiber prepreg strips with the fiber volume fraction of 50-85% in a mold cavity, and sequentially carrying out mold pressing treatment and cracking reaction to obtain a carbon fiber framework; wherein the length of the short carbon fiber prepreg strip is 10-80 mm, the width of the short carbon fiber prepreg strip is 2-10 mm, and the height of the short carbon fiber prepreg strip is 1-3 mm; the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h; the temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-8 h;
(2) mixing the carbon fiber skeleton and solid powder, and sequentially carrying out mould pressing treatment and cracking reaction to obtain a composite material green body; wherein the solid powder comprises phenolic resin powder, carbon powder and silicon powder; the mass ratio of the sum of the mass of the carbon powder and the silicon powder to the mass of the phenolic resin powder is (1-5): 10; the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h; the temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-8 h;
(3) adopting a chemical vapor deposition method to carry out densification treatment on the composite material green body to obtain the composite material green body with the density of 0.85-1.25 g/cm3The densified composite green body of (a); wherein, the chemical vapor deposition methodThe deposition temperature is 900-1100 ℃, and the deposition time is 100-500 h;
(4) and (3) mixing the densified composite material green blank and silicon powder according to the proportion of 1: (2-5) mixing the components according to the mass ratio, and then carrying out a silicon infiltration reaction to obtain the C/SiC ceramic matrix composite; wherein the reaction temperature of the silicon infiltration reaction is 1460-1600 ℃, and the reaction time is 0.5-3.5 h.
In a second aspect, the invention provides a C/SiC ceramic matrix composite material prepared by the preparation method of any one of the first aspect.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) the preparation method comprises the steps of firstly carrying out compression molding on the chopped carbon fiber prepreg strips, and then mixing the chopped carbon fiber prepreg strips with solid powder, wherein all components of a matrix in the prepared ceramic matrix composite material are uniformly distributed, and the ceramic matrix composite material has excellent mechanical strength, high temperature resistance and friction performance and has wide application prospect in brake disc materials;
(2) the preparation method is simple, the process is stable, and the preparation method has the advantages of short period and low cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer and more complete, the technical solutions in the embodiments of the present invention will be described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The invention provides a preparation method of a C/SiC ceramic matrix composite, which comprises the following steps:
(1) placing the short carbon fiber prepreg strips in a die cavity, and sequentially carrying out die pressing treatment and cracking reaction to obtain a carbon fiber framework;
(2) mixing the carbon fiber skeleton and solid powder, and sequentially carrying out mould pressing treatment and cracking reaction to obtain a composite material green body;
(3) adopting a chemical vapor deposition method to perform densification treatment on the composite material green body to obtain a densified composite material green body;
(4) and mixing the densified composite material green blank with silicon powder and then carrying out a silicon infiltration reaction to obtain the C/SiC ceramic matrix composite material.
In the prior art, chopped carbon fibers and resin powder are generally mixed and then molded, however, in the process of mold pressing and temperature rising, the chopped carbon fibers inevitably flow in a melted resin powder matrix, so that the chopped carbon fibers are unevenly distributed in each orientation under the action of gravity, and finally, the composite material has obvious anisotropy of mechanical properties. In the invention, in order to uniformly toughen the carbon fiber composite material, the chopped carbon fiber prepreg strips are firstly molded to form a carbon fiber framework, then mixed with solid powder and molded again, so that the condition that the chopped carbon fibers flow in resin under the action of gravity is effectively avoided, and the prepared ceramic matrix composite material has uniform high-temperature resistance and mechanical property and excellent isotropy.
According to some preferred embodiments, in step (1), the chopped carbon fiber prepreg strips have a fiber volume fraction of 50% to 85% (e.g., may be 50%, 55%, 60%, 65%, 70%, 75%, 80%, or 85%).
In the invention, the fiber volume fraction of the chopped carbon fiber prepreg strips is lower than the range, so that the carbon fibers can not achieve the toughening effect in the composite material; if the fiber volume fraction is higher than the above range, a poor gel phenomenon may occur during the preparation process, and a carbon fiber skeleton may not be formed.
According to some preferred embodiments, in step (1), the chopped carbon fiber prepreg strip has a length of 10 to 80mm (for example, 10mm, 20mm, 30mm, 40mm, 50mm, 60mm, 70mm or 80mm may be used), a width of 2 to 10mm (for example, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm or 10mm may be used), and a height of 1 to 3mm (for example, 1mm, 2mm or 3mm may be used).
In the invention, the carbon fiber valuable-free fabric is cut into the chopped carbon fiber prepreg strips in the range, and when the carbon fiber valuable-free fabric is placed in a mold cavity, the chopped carbon fiber prepreg strips can be ensured to extend in multiple directions, and the built carbon fiber framework has uniform orientation, so that the mechanical property of the composite material is excellent; if the length and width of the chopped carbon fiber prepreg strip are lower than or higher than the above range, a fiber skeleton with uniform orientation cannot be built among the fibers, and the performance of the composite material is affected.
According to some preferred embodiments, in the step (2), the solid powder comprises phenolic resin powder, carbon powder and silicon powder;
the mass ratio of the sum of the mass of the carbon powder and the silicon powder to the mass of the phenolic resin powder is (1-5): 10 (e.g., may be 1: 10, 2: 10, 3: 10, 4: 10, or 5: 10).
It should be noted that, in the invention, the phenolic resin in the solid powder can provide a body mother blank for the carbon fiber framework, and the two can be formed by cross-linking in the mould pressing process; the carbon powder can provide a certain protection effect for the carbon fiber framework; and the addition of the silicon powder can prevent the carbon fiber framework from deforming in the subsequent die pressing process.
In the invention, the ratio of the sum of the mass of the carbon powder and the silicon powder in the solid powder to the mass of the phenolic resin powder is lower than the range, so that the overall performance of the final composite material is influenced; meanwhile, under the condition of satisfying the above range, the carbon powder and the silicon powder in the solid powder can be mixed in any proportion, but cannot be single carbon powder or single silicon powder.
According to some preferred embodiments, the powder particle size of the silicon powder is 35 to 1000 μm (for example, 35 μm, 50 μm, 100 μm, 200 μm, 300 μm, 400 μm, 500 μm, 600 μm, 700 μm, 800 μm, 900 μm, or 1000 μm).
It should be noted that, in the present invention, if the powder particle size of the silicon powder is higher than the above range, on one hand, the number of the silicon powder particles is reduced, and the deformation during the high temperature preparation of the composite material green body cannot be effectively prevented; on the other hand, the excessive silicon powder particles increase the difficulty of melting, and the silicon powder has poor fluidity and cannot be uniformly distributed in the fiber framework and the composite material, so that the final composite material has obvious anisotropy of high-temperature resistance.
According to some preferred embodiments, in the step (1) and the step (2), the temperature of the molding treatment is 140 to 280 ℃ (for example, 140 ℃, 160 ℃, 180 ℃, 200 ℃, 220 ℃, 240 ℃, 260 ℃ or 280 ℃), the pressure is 0.5 to 20MPa (for example, 0.5MPa, 1MPa, 2MPa, 5MPa, 8MPa, 10MPa, 13MPa, 15MPa, 18MPa or 20MPa can be used), and the time is 0.5 to 5h (for example, 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h or 5h can be used);
the reaction temperature of the cracking reaction is 800-1100 ℃ (for example, 800 ℃, 850 ℃, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃ or 1100 ℃), and the reaction time is 2-18 h (for example, 2h, 4h, 6h, 8h, 10h, 12h, 14h, 16h or 18 h).
According to some preferred embodiments, in the step (3), the deposition temperature of the chemical vapor deposition method is 900 to 1100 ℃ (for example, 900 ℃, 950 ℃, 1000 ℃, 1050 ℃ or 1100 ℃), and the deposition time is 100 to 500 hours (for example, 100 hours, 150 hours, 200 hours, 250 hours, 300 hours, 350 hours, 400 hours, 450 hours or 500 hours).
It should be noted that, in the present invention, the chemical vapor deposition process is used to perform densification protection on the composite material green body, and the chemical vapor deposition reaction is performed on the composite material green body in several times under the condition that the total deposition time is ensured to be within the above range, so that the occurrence of the situation that the surface of the material is excessively densified due to single deposition and many internal holes are generated can be avoided, and the uniform densification degree between the surface and the inside of the material can be ensured as much as possible.
According to some preferred embodiments, in the step (3), the density of the densified composite green body is 0.85 to 1.25g/cm3(for example, it may be 0.85 g/cm)3、0.86g/cm3、0.87g/cm3、 0.88g/cm3、0.90g/cm3、0.92g/cm3、0.94g/cm3、0.96g/cm3、1.01g/cm3、1.03 g/cm3、1.05g/cm3、1.11g/cm3、1.15g/cm3、1.20g/cm3Or 1.25g/cm3)。
In the present invention, if the density of the densified composite green compact is higher than the above range, the porosity of the composite green compact is too small, and the efficiency of the subsequent silicon infiltration reaction is too low; if the density is lower than the above range, the carbon interface layer is too thin and the carbon fiber is easily damaged; therefore, the overall performance of the ceramic matrix composite is guaranteed to be excellent only if the density of the densified composite green body is within the range of the invention.
According to some preferred embodiments, in step (4), the mass ratio of the densified composite green body to the silica fume is 1: (2-5) (for example, 1:2, 1: 2.5, 1:3, 1: 3.5, 1:4, 1: 4.5 or 1: 5).
In the present invention, the particle diameter of the silicon powder subjected to the silicon infiltration is the same as that of the silicon powder in the solid powder; in the silicon infiltration reaction, if the content of the silicon powder is lower than the range, the high temperature resistance of the composite material is deteriorated, and the mechanical property is low; if the content of the silicon powder is higher than the above range, the composite material is excessively ceramized, and a large amount of silicon metal remains on the surface of the material after infiltration.
According to some preferred embodiments, in the step (4), the reaction temperature of the siliconizing reaction is 1460 to 1600 ℃ (for example, 1460 ℃, 1480 ℃, 1500 ℃, 1520 ℃, 1550 ℃, 1580 ℃ or 1600 ℃) and the reaction time is 0.5 to 3.5h (for example, 0.5h, 1h, 1.5h, 2h, 2.5h, 3h or 3.5 h).
In the present invention, if the reaction temperature of the silicon infiltration is too low or the reaction time is too short, the fluidity of the silicon melt is poor, and the wettability to the densified composite material green compact is low, so that the reaction is insufficient; if the reaction temperature is too high or the reaction time is too long, the carbon fibers may be damaged.
According to some preferred embodiments, the preparation method comprises the steps of: (1) placing the chopped carbon fiber prepreg strips with the fiber volume fraction of 50-85% in a mold cavity, and sequentially carrying out mold pressing treatment and cracking reaction to obtain a carbon fiber framework; wherein the length of the short carbon fiber prepreg strip is 10-80 mm, the width of the short carbon fiber prepreg strip is 2-10 mm, and the height of the short carbon fiber prepreg strip is 1-3 mm; the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h; the temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-8 h;
(2) mixing the carbon fiber skeleton and solid powder, and sequentially carrying out mould pressing treatment and cracking reaction to obtain a composite material green body; wherein the solid powder comprises phenolic resin powder, carbon powder and silicon powder; the mass ratio of the sum of the mass of the carbon powder and the silicon powder to the mass of the phenolic resin powder is (1-5): 10; the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h; the temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-8 h;
(3) adopting a chemical vapor deposition method to carry out densification treatment on the composite material green body to obtain the composite material green body with the density of 0.85-1.25 g/cm3The densified composite green body of (a); wherein the deposition temperature of the chemical vapor deposition method is 900-1100 ℃, and the deposition time is 100-500 h;
(4) and (3) mixing the densified composite material green blank and silicon powder according to the proportion of 1: (2-5) mixing the components according to the mass ratio, and then carrying out a silicon infiltration reaction to obtain the C/SiC ceramic matrix composite; wherein the reaction temperature of the silicon infiltration reaction is 1460-1600 ℃, and the reaction time is 0.5-3.5 h.
The invention also provides a C/SiC ceramic matrix composite material prepared by the preparation method provided by the invention.
In order to more clearly illustrate the technical scheme and advantages of the invention, a C/SiC ceramic matrix composite material and a preparation method thereof are described in detail by several embodiments.
Example 1:
(1) cutting the carbon fiber valuable-free cloth into short carbon fiber prepreg strips (with the length of 30mm, the width of 5mm and the height of 2mm), wherein the fiber volume fraction of the short carbon fiber prepreg strips is 50%, and then uniformly and randomly placing the short carbon fiber prepreg strips into a tool cavity until the carbon fiber valuable-free cloth is full; carrying out mould pressing treatment for 2h at 180 ℃ and 1MPa, demoulding the formed product, and carrying out cracking reaction for 8h at 850 ℃ to obtain a carbon fiber framework;
(2) uniformly mixing phenolic resin, carbon powder and silicon powder (the particle size is 35 mu m) in a mass ratio of 10:2:1 to obtain solid powder, embedding a carbon fiber framework in the solid powder, uniformly mixing, transferring the solid powder into a tool cavity, carrying out mould pressing treatment for 2.5h at 185 ℃ and 1MPa, demoulding after forming, and carrying out cracking reaction for 10h at 800 ℃ to obtain a composite material green body;
(3) carrying out chemical vapor deposition reaction twice on the composite material green blank at 1020 ℃, wherein the deposition time is respectively 80h and 50h (total 130h), and obtaining the densified composite material green blank (the density is 0.93 g/cm)3)；
(4) And mixing the densified composite material green blank and silicon powder according to the mass ratio of 1:2, and carrying out silicon infiltration reaction at 1500 ℃ for 0.5h to obtain the C/SiC ceramic matrix composite.
Example 2
(1) Cutting the carbon fiber valuable-free cloth into short carbon fiber prepreg strips (with the length of 10mm, the width of 2mm and the height of 1mm), wherein the volume part of fibers of the short carbon fiber prepreg strips is 60%, and then uniformly and randomly placing the short carbon fiber prepreg strips into a tool cavity until the carbon fiber valuable-free cloth is full; carrying out mould pressing treatment for 2.5h at 140 ℃ and 3Mpa, demoulding the formed product, and carrying out cracking reaction for 10h at 900 ℃ to obtain a carbon fiber framework;
(2) uniformly mixing phenolic resin, carbon powder and silicon powder (the particle size is 100 mu m) in a mass ratio of 10:2:2 to obtain solid powder, embedding a carbon fiber framework in the solid powder, uniformly mixing, transferring the solid powder into a tool cavity, carrying out 3-hour mould pressing treatment at 150 ℃ and 3Mpa, demoulding after forming, and carrying out cracking reaction at 900 ℃ for 10 hours to obtain a composite material green body;
(3) carrying out three times of chemical vapor deposition reaction on the composite material green blank at 900 ℃, wherein the deposition time is respectively 40h, 50h and 90h (totally 180h), and obtaining the densified composite material green blank (the density is 1.09 g/cm)3)；
(4) And mixing the densified composite material green blank and silicon powder according to the mass ratio of 1:3, and carrying out silicon infiltration reaction for 1h at 1550 ℃ to obtain the C/SiC ceramic matrix composite material.
Example 3
(1) Cutting the carbon fiber Renwei cloth into chopped carbon fiber prepreg strips (with the length of 20mm, the width of 4mm and the height of 2mm), wherein the volume part of fibers of the chopped carbon fiber prepreg strips is 65%, and then uniformly and randomly placing the chopped carbon fiber prepreg strips into a tool cavity until the carbon fiber Renwei cloth is full; performing mould pressing treatment at 200 deg.C and 10Mpa for 3 hr, demolding, and performing cracking reaction at 950 deg.C for 10 hr to obtain carbon fiber skeleton;
(2) uniformly mixing phenolic resin, carbon powder and silicon powder (the particle size is 200 mu m) in a mass ratio of 10:1:1 to obtain solid powder, embedding a carbon fiber framework in the solid powder, uniformly mixing, transferring the solid powder into a tool cavity, carrying out mould pressing treatment for 2 hours at 185 ℃ and 10Mpa, demoulding after forming, and carrying out cracking reaction for 15 hours at 900 ℃ to obtain a composite material green body;
(3) carrying out chemical vapor deposition reaction twice on the composite material green blank at 950 ℃, wherein the deposition time is respectively 80h and 90h (total 170h), and obtaining the densified composite material green blank (the density is 1.01 g/cm)3)；
(4) And mixing the densified composite material green blank and silicon powder according to the mass ratio of 1:4, and carrying out silicon infiltration reaction at 1490 ℃ for 2 hours to obtain the C/SiC ceramic matrix composite material.
Example 4
(1) Cutting the carbon fiber valuable-free cloth into short carbon fiber prepreg strips (with the length of 50mm, the width of 5mm and the height of 3mm), wherein the volume part of fibers of the short carbon fiber prepreg strips is 70%, and then uniformly and randomly placing the short carbon fiber prepreg strips into a tool cavity until the carbon fiber valuable-free cloth is full; performing mould pressing treatment at 210 deg.C and 0.5Mpa for 3 hr, demolding, and performing cracking reaction at 1000 deg.C for 6 hr to obtain carbon fiber skeleton;
(2) uniformly mixing phenolic resin, carbon powder and silicon powder (the particle size is 400 mu m) in a mass ratio of 10:0.5:1 to obtain solid powder, embedding a carbon fiber framework in the solid powder, uniformly mixing, transferring the solid powder into a tool cavity, performing mould pressing treatment at 210 ℃ and 10Mpa for 2.5 hours, demolding after molding, and performing cracking reaction at 1000 ℃ for 10 hours to obtain a composite material green body;
(3) carrying out three times of chemical vapor deposition reaction on the composite material green blank at the temperature of 1000 ℃, wherein the deposition time is respectively 80h, 80h and 90h (total 260h), and obtaining the densified composite material green blank (the density is 1.00 g/cm)3)；
(4) And mixing the densified composite material green blank and silicon powder according to the mass ratio of 1:5, and carrying out silicon infiltration reaction for 1h at 1550 ℃ to obtain the C/SiC ceramic matrix composite material.
Example 5
(1) Cutting the carbon fiber Renwei cloth into chopped carbon fiber prepreg strips (with the length of 60mm, the width of 6mm and the height of 2mm), wherein the fiber volume part of the chopped carbon fiber prepreg strips is 80%, and then uniformly mixing the chopped carbon fiber prepreg strips
Randomly placing the workpiece in a tool cavity until the workpiece is full; performing mould pressing treatment at 230 deg.C and 10Mpa for 4 hr, demoulding, and performing cracking reaction at 1100 deg.C for 2 hr to obtain carbon fiber skeleton;
(2) uniformly mixing phenolic resin, carbon powder and silicon powder (the particle size is 500 mu m) in a mass ratio of 10:3:2 to obtain solid powder, embedding a carbon fiber framework in the solid powder, uniformly mixing, transferring the solid powder into a tool cavity, performing mould pressing treatment at 230 ℃ and 10Mpa for 5 hours, demolding after forming, and performing cracking reaction at 1100 ℃ for 2 hours to obtain a composite material green body;
(3) carrying out three times of chemical vapor deposition reaction on the composite material green blank at the temperature of 1030 ℃, wherein the deposition time is respectively 50h, 150h and 100h (300 h in total), and obtaining the densified composite material green blank (the density is 1.15 g/cm)3)；
(4) And mixing the densified composite material green blank and silicon powder according to the mass ratio of 1:3, and carrying out silicon infiltration reaction at 1600 ℃ for 2 hours to obtain the C/SiC ceramic matrix composite material.
Example 6
(1) Cutting the carbon fiber Renwei cloth into chopped carbon fiber prepreg strips (with the length of 70mm, the width of 8mm and the height of 3mm), wherein the volume part of fibers of the chopped carbon fiber prepreg strips is 85%, and then uniformly and randomly placing the chopped carbon fiber prepreg strips into a tool cavity until the carbon fiber Renwei cloth is full; performing mold pressing treatment at 250 deg.C and 15Mpa for 0.5 hr, demolding, and performing cracking reaction at 900 deg.C for 8 hr to obtain carbon fiber skeleton;
(2) uniformly mixing phenolic resin, carbon powder and silicon powder (the particle size is 800 mu m) in a mass ratio of 10:2.5:2.5 to obtain solid powder, embedding a carbon fiber framework in the solid powder, uniformly mixing, transferring the solid powder into a tool cavity, carrying out mould pressing treatment at 250 ℃ and 15Mpa for 0.55h, demoulding after forming, and carrying out cracking reaction at 900 ℃ for 8h to obtain a composite material green body;
(3) carrying out three times of chemical vapor deposition reaction on the composite material green blank at 1050 ℃, wherein the deposition time is respectively 150h, 150h and 100h (total 400h), and obtaining the densified composite material green blank (the density is 1.20 g/cm)3)；
(4) And mixing the densified composite material green blank and silicon powder according to the mass ratio of 1:3, and carrying out silicon infiltration reaction at 1550 ℃ for 3.5 hours to obtain the C/SiC ceramic matrix composite.
Example 7
(1) Cutting the carbon fiber Renwei cloth into chopped carbon fiber prepreg strips (with the length of 80mm, the width of 10mm and the height of 1mm), wherein the volume part of fibers of the chopped carbon fiber prepreg strips is 78%, and then uniformly and randomly placing the chopped carbon fiber prepreg strips into a tool cavity until the carbon fiber Renwei cloth is full; performing mold pressing treatment at 280 deg.C and 20Mpa for 0.5 hr, demolding, and performing cracking reaction at 900 deg.C for 8 hr to obtain carbon fiber skeleton;
(2) uniformly mixing phenolic resin, carbon powder and silicon powder (the particle size is 1000 microns) in a mass ratio of 10:1.5:2.5 to obtain solid powder, embedding a carbon fiber framework in the solid powder, uniformly mixing, transferring the solid powder into a tool cavity, performing mould pressing treatment at 280 ℃ and 15MPa for 5 hours, demolding after forming, and performing cracking reaction at 900 ℃ for 8 hours to obtain a composite material green body;
(3) carrying out three times of chemical vapor deposition reaction on the composite material green blank at 1100 ℃, wherein the deposition time is respectively 150h, 150h and 200h (total 500h), and obtaining the densified compositeComposite material green body (density 1.25 g/cm)3)；
(4) And mixing the densified composite material green blank and silicon powder according to the mass ratio of 1:3, and carrying out silicon infiltration reaction at 1600 ℃ for 2.5 hours to obtain the C/SiC ceramic matrix composite.
Example 8
Example 8 is essentially the same as example 2, except that: in step (3), the density of the densified composite green body is 0.75g/cm3。
Example 9
Example 9 is essentially the same as example 2, except that: in step (3), the density of the densified composite green body is 1.35g/cm3。
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that: and (3) directly mixing the chopped carbon fiber prepreg strips in the step (1) with the solid powder in the step (2), and then sequentially carrying out mould pressing treatment and cracking reaction.
Comparative example 2
Comparative example 1 is substantially the same as example 1 except that: and (2) directly mixing the chopped carbon fiber prepreg strips in the step (1) with resin, and then sequentially carrying out mould pressing treatment and cracking reaction.
Comparative example 3
Comparative example 3 is substantially the same as example 1 except that: the solid powder in the step (2) only comprises phenolic resin powder.
Comparative example 4
Comparative example 4 is substantially the same as example 1 except that: the solid powder in the step (2) only comprises phenolic resin powder and carbon powder.
Comparative example 5
Comparative example 5 is substantially the same as example 1 except that: the solid powder in the step (2) only comprises phenolic resin powder and silicon powder.
Comparative example 6
Comparative example 6 is substantially the same as example 1 except that: the method does not comprise the step (1) and the step (2), and directly adopts a fiber preform woven by long carbon fibers as a framework to carry out chemical vapor deposition reaction and silicon infiltration reaction in sequence.
The ceramic matrix composite materials prepared in examples 1 to 9 and comparative examples 1 to 6 were respectively subjected to performance tests, and the test results are shown in table 1.
The various performance tests of the invention are obtained by testing the conventional test methods of the technicians in the field. It should be noted that the in-plane compressive strength is measured by compressing the material downward from the upper surface thereof; the Z-direction compressive strength is measured as the compression of the material from its side to its opposite side.
TABLE 1
Figure BDA0003352478660000121
Figure BDA0003352478660000131
As can be seen from Table 1, the ceramic matrix composite materials prepared in the embodiments 1 to 7 of the present invention have uniform mechanical properties, excellent compression resistance and friction resistance, and less abrasion; in examples 8 to 9, when the density of the green compact of the densified composite material obtained is lower than the range of the present invention, the overall properties of the ceramic matrix composite material obtained are deteriorated; in comparative example 1, when the chopped carbon fibers are directly mixed with the solid powder, the chopped carbon fibers flow under the action of gravity, so that the toughening effect is not uniform, the anisotropy of the ceramic matrix composite material is obvious, and the compression resistance and the friction resistance are poor; in comparative example 2, when the chopped carbon fibers were directly mixed with the resin, not only the carbon fibers were unevenly distributed in the resin, but also the material was entirely deformed during the subsequent molding and cracking processes, and finally the properties of the ceramic matrix composite were deteriorated; in comparative examples 3 to 5, when the carbon fiber skeleton was mixed with only the phenol resin, cracking and warp deformation occurred on the surface of the material after pyrolysis; when the carbon fiber framework is only mixed with phenolic resin and carbon powder, the fiber framework is deformed due to the lack of silicon powder; when the carbon fiber framework is only mixed with phenolic resin and silicon powder, the carbon fiber is damaged due to lack of protection of the carbon powder; therefore, in comparative examples 3 to 5, the overall performance of the finally prepared ceramic matrix composite was poor; in comparative example 6, when the fiber preform woven from the fibers was directly used as the skeleton, the overall performance of the composite material was not much different from that in the examples, but the preparation period of the entire composite material was extended and the preparation cost of the entire experiment was significantly increased.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention. The invention has not been described in detail and is in part known to those of skill in the art.

Claims (10)

1. The preparation method of the C/SiC ceramic matrix composite is characterized by comprising the following steps:
(1) placing the short carbon fiber prepreg strips in a die cavity, and sequentially carrying out die pressing treatment and cracking reaction to obtain a carbon fiber framework;
(2) mixing the carbon fiber skeleton and solid powder, and sequentially carrying out mould pressing treatment and cracking reaction to obtain a composite material green body;
(3) adopting a chemical vapor deposition method to perform densification treatment on the composite material green body to obtain a densified composite material green body;
(4) and mixing the densified composite material green blank with silicon powder and then carrying out a silicon infiltration reaction to obtain the C/SiC ceramic matrix composite material.
2. The production method according to claim 1, wherein in step (1):
the chopped carbon fiber prepreg strips have a fiber volume fraction of 50-85%.
3. The production method according to claim 1, wherein in step (1):
the short carbon fiber prepreg strip is 10-80 mm in length, 2-10 mm in width and 1-3 mm in height.
4. The production method according to claim 1, wherein in step (2):
the solid powder comprises phenolic resin powder, carbon powder and silicon powder;
the mass ratio of the sum of the mass of the carbon powder and the silicon powder to the mass of the phenolic resin powder is (1-5): 10.
5. the method of claim 4, wherein: the powder particle size of the silicon powder is 35-1000 mu m.
6. The production method according to claim 1, wherein in step (1) and step (2):
the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h;
the reaction temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-18 h.
7. The production method according to claim 1, wherein in step (3):
the deposition temperature of the chemical vapor deposition method is 900-1100 ℃, and the deposition time is 100-500 h; and/or
The density of the densified composite material green body is 0.85-1.25 g/cm3。
8. The production method according to claim 1, wherein in step (4):
the mass ratio of the densified composite material green blank to the silicon powder is 1: (2-5); and/or
The reaction temperature of the silicon infiltration reaction is 1460-1600 ℃, and the reaction time is 0.5-3.5 h.
9. The method according to any one of claims 1 to 8, characterized by comprising the steps of:
(1) placing the chopped carbon fiber prepreg strips with the fiber volume fraction of 50-85% in a mold cavity, and sequentially carrying out mold pressing treatment and cracking reaction to obtain a carbon fiber framework; wherein the length of the short carbon fiber prepreg strip is 10-80 mm, the width of the short carbon fiber prepreg strip is 2-10 mm, and the height of the short carbon fiber prepreg strip is 1-3 mm; the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h; the temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-8 h;
(2) mixing the carbon fiber skeleton and solid powder, and sequentially carrying out mould pressing treatment and cracking reaction to obtain a composite material green body; wherein the solid powder comprises phenolic resin powder, carbon powder and silicon powder; the mass ratio of the sum of the mass of the carbon powder and the silicon powder to the mass of the phenolic resin powder is (1-5): 10; the temperature of the mould pressing treatment is 140-280 ℃, the pressure is 0.5-20 MPa, and the time is 0.5-5 h; the temperature of the cracking reaction is 800-1100 ℃, and the reaction time is 2-8 h;
(3) adopting a chemical vapor deposition method to carry out densification treatment on the composite material green body to obtain the composite material green body with the density of 0.85-1.25 g/cm3The densified composite green body of (a); wherein the deposition temperature of the chemical vapor deposition method is 900-1100 ℃, and the deposition time is 100-500 h;
(4) and (3) mixing the densified composite material green blank and silicon powder according to the proportion of 1: (2-5) mixing the components according to the mass ratio, and then carrying out a silicon infiltration reaction to obtain the C/SiC ceramic matrix composite; wherein the reaction temperature of the silicon infiltration reaction is 1460-1600 ℃, and the reaction time is 0.5-3.5 h.
10. A C/SiC ceramic matrix composite characterized by being prepared by the preparation method of any one of claims 1 to 9.
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