CN117447218A - Ceramic matrix composite based on ceramic prepreg and rapid preparation method thereof - Google Patents

Ceramic matrix composite based on ceramic prepreg and rapid preparation method thereof Download PDF

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CN117447218A
CN117447218A CN202311383978.6A CN202311383978A CN117447218A CN 117447218 A CN117447218 A CN 117447218A CN 202311383978 A CN202311383978 A CN 202311383978A CN 117447218 A CN117447218 A CN 117447218A
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ceramic
prepreg
matrix composite
ceramic matrix
preparing
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马登浩
张国兵
孙新
张大海
李军平
焦星剑
戴志锋
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Aerospace Research Institute of Materials and Processing Technology
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Aerospace Research Institute of Materials and Processing Technology
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Abstract

The invention provides a ceramic matrix composite based on a ceramic prepreg and a rapid preparation method thereof, wherein the ceramic matrix composite is prepared by combining prepreg layering forming with a precursor dipping and cracking process or a fused siliconizing process as a technical main line, a dry process is adopted to prepare a glue film for the prepreg from mixed slurry of a liquid ceramic precursor and ceramic powder, and the glue film is attached to fiber cloth containing a pyrolytic carbon interface layer to prepare the ceramic prepreg; preparing a ceramic matrix composite blank by adopting a layering mode of the prepreg, and then re-compacting the blank by utilizing a ceramic precursor circulating dipping-solidifying-cracking or melting siliconizing process for at most three times to finally prepare the ceramic matrix composite meeting the design requirement; the preparation process has the remarkable advantages of short period and low cost.

Description

Ceramic matrix composite based on ceramic prepreg and rapid preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic matrix composite materials, and particularly relates to a ceramic matrix composite material based on a ceramic prepreg and a rapid preparation method thereof.
Background
The traditional prepreg is a composition prepared by impregnating continuous fibers or fabrics with one or more resin substrates, is an important intermediate material for transition from raw materials to products, and is mainly divided into unidirectional fiber prepreg, fabric fiber prepreg, mixed fiber prepreg and the like. The prepreg has the advantages of controllable fiber component proportion, various and mature preparation process types, convenient use and the like, can be used for preparing a plurality of composite materials with different performances and functions by combining different molding processes, and has wide application in the high-tech fields of aerospace, aviation, navigation, traffic and the like at home and abroad.
The existing ceramic matrix composite materials adopt a continuous fiber braiding structure and a precursor dipping and cracking composite process, and have the problems of expensive raw materials, multiple preparation procedures, long manufacturing period, large fiber braiding and multi-round composite damage, low composite efficiency, high manufacturing cost and the like, so that the requirements of the aerospace field on low-cost and short-period development of the ceramic matrix composite materials are difficult to meet, and the ceramic matrix composite materials become bottlenecks for restricting the wide application of the ceramic matrix composite materials. Therefore, the novel rapid and low-cost process is developed to prepare the ceramic prepreg and the ceramic matrix composite material thereof, so that the rapid and efficient preparation and large-scale application of the ceramic matrix composite material are expected to meet the current development demands.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: the ceramic matrix composite based on the ceramic prepreg and the rapid preparation method thereof are provided, and the problems of large fiber damage, long period, high cost and the like in the traditional preparation process are solved.
The invention takes a ceramic matrix composite prepared by combining prepreg ply forming and precursor dipping and cracking process or melting and siliconizing process as a technical main line, adopts a dry process to prepare a glue film for the prepreg from the mixed slurry of liquid ceramic precursor and ceramic powder, and is attached to fiber cloth containing a pyrolytic carbon interface layer to prepare the ceramic prepreg; preparing a ceramic matrix composite blank by adopting a layering mode of the prepreg, and then re-compacting the blank by utilizing a ceramic precursor circulating dipping-solidifying-cracking or melting siliconizing process for at most three times to finally prepare the ceramic matrix composite meeting the design requirement; the preparation process has the remarkable advantages of short period and low cost.
The technical scheme provided by the invention is as follows:
in a first aspect, a method for the rapid preparation of a ceramic matrix composite based on a ceramifiable prepreg, comprising:
preparing a glue film for prepreg by using mixed slurry of a liquid ceramic precursor and ceramic powder through a compression roller;
laminating the adhesive film with the upper surface and the lower surface of continuous fiber cloth containing a pyrolytic carbon interface layer through a compression roller to prepare a ceramic prepreg;
preparing a two-dimensional structure ceramic matrix composite blank by the prepreg through a layering process, and performing primary densification by vacuum auxiliary curing and high-temperature pyrolysis in the forming process;
and re-densification is carried out on the ceramic matrix composite blank through at most three rounds of PIP process, RMI process or PIP-RMI combined process, so as to obtain the densified composite.
In a second aspect, a ceramic matrix composite based on a ceramifiable prepreg is produced by the rapid manufacturing method based on a ceramifiable prepreg ceramic matrix composite according to the first aspect.
According to the ceramic matrix composite based on the ceramic prepreg and the rapid preparation method thereof, the ceramic matrix composite based on the ceramic prepreg has the following beneficial effects:
(1) Compared with the traditional PIP process, the preparation period of the ceramic-based composite material based on the ceramic prepreg and the rapid preparation method thereof provided by the invention can be greatly reduced, and the impregnation cracking is reduced from 10-15 rounds to 2-4 rounds.
(2) Compared with the traditional RMI technology, the ceramic matrix based ceramic matrix composite material based on the ceramic prepreg and the rapid preparation method thereof provided by the invention can obviously reduce the residual silicon content in the ceramic matrix, and are beneficial to improving the comprehensive performance of the composite material.
(3) The ceramic matrix composite based on the ceramifiable prepreg and the rapid preparation method thereof provided by the invention have obvious application prospects for preparing the ceramic matrix composite in a short period at low cost.
Drawings
FIG. 1 is a block diagram of a C/SiC composite material prepared based on a ceramifiable prepreg;
FIG. 2 is an XRD pattern of a ceramic matrix in a C/SiC composite material prepared by a conventional RMI process and the process of the invention;
FIG. 3 is an XRD pattern of a ceramic matrix in a C/SiC composite material prepared by a conventional RMI process and the process of the invention.
Detailed Description
The features and advantages of the present invention will become more apparent and clear from the following detailed description of the invention.
The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
The invention provides a ceramic matrix composite based on a ceramic prepreg, which comprises the following steps:
and (1) preparing the glue film for the prepreg by using the mixed slurry of the liquid ceramic precursor and the ceramic powder through a compression roller.
In the step, mixed slurries with different viscosities are prepared by changing the introduction amount of ceramic powder in a liquid ceramic precursor, and then a glue film for the ceramic prepreg is prepared by a compression roller, wherein the viscosity range is preferably controlled between 15000cp and 30000cp (70 ℃).
In the step, the liquid ceramic precursor is at least one of polycarbosilane, polysilazane or polysilabozane; the ceramic powder is at least one of nano-scale or micro-scale silicon carbide, zirconium boride or hafnium carbide.
In the step, the thickness of the adhesive film is 0.1 mm-0.2 mm.
And (2) bonding the adhesive film obtained in the step (1) with the upper surface and the lower surface of continuous fiber cloth containing a pyrolytic carbon interface layer through a compression roller to prepare the ceramic prepreg with set adhesive content and thickness.
In this step, the fiber cloth is a carbon fiber cloth or a silicon carbide (SiC) fiber cloth.
Step (3), preparing a two-dimensional structure ceramic matrix composite blank by adopting a layering process for the prepreg obtained in the step (2), and performing primary densification by adopting vacuum auxiliary curing and high-temperature cracking in the forming process; and cleaning residues on the surface of the blank body after the pyrolysis is finished.
The method comprises the steps of repeatedly cleaning the surface of a layering die by using a solvent, coating a release agent, paving a high-temperature-resistant anti-adhesion film (such as a polytetrafluoroethylene film), then adopting an automatic blanking machine to perform blanking on prepreg according to the pre-designed blanking size and quantity, paving the prepreg layer by layer on the molded surface of the layering die, scraping the prepreg layer by using a plastic scraper, paving 5-10 layers in each paving process, wrapping a vacuum bag for vacuum compaction, paving high-temperature release cloth (such as polytetrafluoroethylene coated glass fiber cloth), a porous isolating film and a high-temperature airfelt on the surface of a blank after all layering is completed, and adopting the vacuum bag for packaging treatment; and finally, solidifying and high-temperature cracking are carried out. Wherein, the curing system is: the curing temperature is 150-250 ℃ and the curing time is 1-3 h. The cracking system is as follows: the cracking temperature is 800-1400 ℃ and the cracking time is 1-4 h.
Step (4), re-densification is carried out on the ceramic matrix composite blank obtained in the step (3) through at most three rounds of precursor dipping-solidifying-cracking process (PIP) or melt siliconizing process (RMI) or PIP-RMI combined process, so that the volume density of the composite material after cleaning is 1.9-2.5g/cm 3
In the step, if the PIP process or the PIP-RMI combined process is adopted for re-densification, the impregnant adopted in the impregnation step is consistent with the liquid ceramic precursor for the adhesive film. The curing system is as follows: the curing temperature is 150-250 ℃ and the curing time is 1-3 h; the cracking system is as follows: the cracking temperature is 800-1400 ℃ and the cracking time is 1-4 h.
In this step, if the re-densification is performed by a fused siliconizing process (RMI) or a PIP-RMI combined process, the RMI process parameters include: the infiltration reaction temperature is 1450-1600 ℃, the reaction time is 0.5-2 h, and the grain diameter of the silicon powder is 1-5 mm.
In the step, if a fused siliconizing process (RMI) or a PIP-RMI combined process is adopted for re-densification, phenolic resin can be added into the adhesive film to prepare mixed phase prepreg, the introduction of the phenolic resin can controllably increase the carbon content in the ceramic matrix composite blank after the first densification, and the densification degree of the composite can be improved by converting residual carbon into silicon carbide SiC after the RMI process. Preferably, the mass of the phenolic resin is 5% -10% of that of the liquid ceramic precursor.
Examples
Example 1
(1) The liquid polycarbosilane precursor and SiC ceramic powder are mixed according to the weight ratio of 100:50 to prepare ceramic slurry, the viscosity is 28000cp (70 ℃), and then a glue film for prepreg is prepared through a pressing roller, wherein the thickness is about 0.1mm.
(2) And (3) bonding the adhesive film obtained in the step (1) with the upper surface and the lower surface of continuous carbon fiber cloth containing a pyrolytic carbon interface layer through a compression roller to prepare the ceramic prepreg, wherein the thickness of the ceramic prepreg is about 0.4mm.
(3) Preparing a two-dimensional structure ceramic matrix composite blank from the prepreg obtained in the step (2) by adopting a layering process, repeatedly cleaning the surface of a layering die by using a solvent, coating a release agent, paving a polytetrafluoroethylene film, then blanking the prepreg according to a pre-designed blanking size and number by adopting an automatic blanking machine, paving the prepreg layer by layer on the surface of the layering die, scraping the prepreg by using a plastic scraper, paving 5-10 layers in each paving process, wrapping a vacuum bag for vacuum compaction, paving high-temperature release cloth, a porous isolation film and a high-temperature airfelt on the surface of the blank after all layering is completed, and adopting a vacuum bag for packaging treatment; finally, carrying out vacuum assisted curing at 200 ℃ and high-temperature pyrolysis at 1000 ℃, and cleaning residues on the surface of the blank body after pyrolysis is finished.
(4) Performing twice densification on the ceramic matrix composite blank obtained in the step (3) through a precursor dipping-curing-cracking process until the volume density of the composite material reaches 1.95g/cm after cleaning 3 The SEM electron microscope image is shown in fig. 1. Wherein the curing temperature is 200 ℃, the curing time is 2 hours, the cracking temperature is 1000 ℃, and the cracking time is 2 hours.
Compared with the traditional PIP process, the densification cycle is reduced from 10 cycles to 3 cycles.
Example 2
(1) The liquid polycarbosilane precursor and SiC ceramic powder are mixed according to the weight ratio of 100:40 to prepare ceramic slurry, the viscosity is 19000cp (70 ℃), and then a glue film for prepreg is prepared through a pressing roller, wherein the thickness is about 0.1mm.
(2) And (3) bonding the adhesive film obtained in the step (1) with the upper surface and the lower surface of the continuous carbon fiber cloth containing the pyrolytic carbon interface layer through a compression roller to prepare the ceramic prepreg with the set adhesive content and thickness, wherein the thickness is about 0.4mm.
(3) Preparing a two-dimensional structure ceramic matrix composite blank from the prepreg obtained in the step (2) by adopting a layering process, repeatedly cleaning the surface of a layering die by using a solvent, coating a release agent, paving a polytetrafluoroethylene film, then blanking the prepreg according to a pre-designed blanking size and number by adopting an automatic blanking machine, paving the prepreg layer by layer on the surface of the layering die, scraping the prepreg by using a plastic scraper, paving 5-10 layers in each paving process, wrapping a vacuum bag for vacuum compaction, paving high-temperature release cloth, a porous isolation film and a high-temperature airfelt on the surface of the blank after all layering is completed, and adopting a vacuum bag for packaging treatment; finally, carrying out vacuum assisted curing at 200 ℃ and high-temperature pyrolysis at 900 ℃, and cleaning residues on the surface of the blank body after pyrolysis is finished.
(4) Densification treatment is carried out on the ceramic matrix composite blank obtained in the step (3) through a fused siliconizing process, and the volume density of the composite material after cleaning is 2.10g/cm 3 . Wherein, the grain diameter of the silicon powder is 3mm, and the infiltration reaction temperature is highThe degree was 1500 ℃. Compared with the traditional PIP process, the densification cycle is reduced from 10 cycles to 2 cycles. Meanwhile, the content of residual silicon in the ceramic matrix of the C/SiC composite material prepared by the process is lower than that of the composite material prepared by the conventional RMI process, as shown in figure 2.
Example 3
(1) Mixing the liquid polycarbosilane precursor, siC ceramic powder and phenolic resin according to the weight ratio of 100:40:10 to prepare ceramic slurry, wherein the viscosity is 18000cp (70 ℃), and then preparing the adhesive film for prepreg through a compression roller, wherein the thickness is about 0.1mm.
(2) And (3) bonding the adhesive film obtained in the step (1) with the upper surface and the lower surface of the continuous carbon fiber cloth containing the pyrolytic carbon interface layer through a compression roller to prepare the ceramic prepreg with the set adhesive content and thickness, wherein the thickness is about 0.4mm.
(3) Preparing a two-dimensional structure ceramic matrix composite blank from the prepreg obtained in the step (2) by adopting a layering process, repeatedly cleaning the surface of a layering die by using a solvent, coating a release agent, paving a polytetrafluoroethylene film, then blanking the prepreg according to a pre-designed blanking size and number by adopting an automatic blanking machine, paving the prepreg layer by layer on the surface of the layering die, scraping the prepreg by using a plastic scraper, paving 5-10 layers in each paving process, wrapping a vacuum bag for vacuum compaction, paving high-temperature release cloth, a porous isolation film and a high-temperature airfelt on the surface of the blank after all layering is completed, and adopting a vacuum bag for packaging treatment; finally, carrying out vacuum assisted curing at 200 ℃ and high-temperature pyrolysis at 900 ℃, and cleaning residues on the surface of the blank body after pyrolysis is finished.
(4) Densification treatment is carried out on the ceramic matrix composite blank obtained in the step (3) through a fused siliconizing process, and the volume density of the composite material after cleaning is 2.05g/cm 3 . Wherein, the grain diameter of the silicon powder is 3mm, and the infiltration reaction temperature is 1500 ℃. Compared with the traditional PIP process, the densification cycle is reduced from 10 cycles to 2 cycles. Meanwhile, the content of residual silicon in the ceramic matrix of the C/SiC composite material prepared by the process is obviously lower than that of the composite material prepared by the conventional RMI process, as shown in figure 3.
The invention has been described in detail in connection with the specific embodiments and exemplary examples thereof, but such description is not to be construed as limiting the invention. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, and these fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
What is not described in detail in the present specification is a well known technology to those skilled in the art.

Claims (10)

1. A rapid preparation method based on a ceramic-based composite material of a ceramic prepreg, which is characterized by comprising the following steps:
preparing a glue film for prepreg by using mixed slurry of a liquid ceramic precursor and ceramic powder through a compression roller;
laminating the adhesive film with the upper surface and the lower surface of continuous fiber cloth containing a pyrolytic carbon interface layer through a compression roller to prepare a ceramic prepreg;
preparing a two-dimensional structure ceramic matrix composite blank by the prepreg through a layering process, and performing primary densification by vacuum auxiliary curing and cracking in the forming process;
and re-densification is carried out on the ceramic matrix composite blank through at most three rounds of PIP process, RMI process or PIP-RMI combined process, so as to obtain the densified composite.
2. The method for rapidly preparing a ceramic matrix composite based on a ceramic prepreg according to claim 1, wherein in the step of preparing a glue film for a prepreg by mixing a liquid ceramic precursor and ceramic powder with a pressing roller, the glue film has a viscosity of 15000cp to 30000cp at 70 ℃.
3. The method for preparing a ceramic matrix composite based on a ceramic prepreg according to claim 1, wherein in the step of preparing a glue film for a prepreg by mixing a liquid ceramic precursor and ceramic powder through a press roll, the liquid ceramic precursor is at least one of polycarbosilane, polysilazane or polysilazane.
4. The method for rapidly preparing a ceramic matrix composite based on a ceramic prepreg according to claim 1, wherein in the step of preparing a glue film for a prepreg by passing a mixed slurry of a liquid ceramic precursor and a ceramic powder through a press roll, the ceramic powder is at least one of silicon carbide, zirconium boride or hafnium carbide.
5. The method for rapidly preparing a ceramic matrix composite based on a ceramic prepreg according to claim 1, wherein in the step of preparing a glue film for a prepreg by mixing a liquid ceramic precursor and ceramic powder with a pressing roller, the thickness of the glue film is 0.1mm to 0.2mm.
6. The method for preparing the ceramic matrix composite based on the ceramic prepreg according to claim 1, wherein in the step of attaching the adhesive film to the upper surface and the lower surface of the continuous fiber cloth containing the pyrolytic carbon interface layer through a pressing roller to prepare the ceramic prepreg, the fiber cloth is carbon fiber cloth or silicon carbide fiber cloth, and the thickness of the pyrolytic carbon interface layer is preferably 100-500 nm.
7. The rapid preparation method of ceramic matrix composite based on ceramic prepreg according to claim 1, wherein the prepreg adopts a layering process to prepare a two-dimensional structure ceramic matrix composite blank, in the step of performing primary densification by vacuum assisted curing and cracking in the forming process, 5-10 layers are paved in each layering process, a vacuum bag is wrapped for vacuum compaction, after layering is completed, release cloth, a porous isolating film and a high-temperature airfelt are paved on the surface of the blank, packaging treatment is performed by adopting the vacuum bag, and curing and high-temperature cracking are performed.
8. The method of claim 1, wherein the step of re-densifying the ceramic matrix composite by at most three PIP processes, RMI processes or PIP-RMI combined processes to obtain a densified composite comprises the following parameters: the impregnation pressure is 0.5-4 MPa, the curing temperature is 150-250 ℃, and the cracking temperature is 800-1400 ℃;
the parameters of the melt siliconizing process include: the grain diameter of the silicon powder is 1-5 mm, and the infiltration reaction temperature is 1450-1600 ℃.
9. The method for rapid preparation of ceramic matrix composites based on ceramifiable prepregs according to claim 1, wherein the ceramic matrix composite blank is re-densified by at most three rounds of PIP process, RMI process or PIP-RMI combined process to give a densified composite having a density of 1.9 to 2.5g/cm 3
10. Ceramic matrix composite based on a ceramifiable prepreg according to claim 1, which is produced by the rapid preparation method based on a ceramifiable prepreg according to claim 1.
CN202311383978.6A 2023-10-24 2023-10-24 Ceramic matrix composite based on ceramic prepreg and rapid preparation method thereof Pending CN117447218A (en)

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