CN115819099A - High-performance SiC f Preparation method of/SiC composite material - Google Patents
High-performance SiC f Preparation method of/SiC composite material Download PDFInfo
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Abstract
Provides a high-performance SiC f The preparation method of the/SiC composite material comprises the following steps of taking SiC fibers as a reinforcement and silicon carbide as a matrix, wherein the volume fraction of the SiC fibers is 35-45%; the preparation method comprises the following steps: s1, sequentially carrying out high-temperature heat treatment, chemical vapor deposition of a cracked carbon interface layer and chemical vapor deposition of a SiC matrix on the SiC fiber prefabricated part to obtain a first density intermediate; s2, preparing SiC precursor solution from solid polycarbosilane and xylene; s3, vacuum-dipping the first density intermediate into the SiC precursor solution prepared in the S2, sequentially carrying out crosslinking curing and cracking to obtain a precursor impregnated cracked SiC matrix; s4, repeating the S3 cycle for 5-7 times, obtaining a second density intermediate; s5, dipping the second density intermediate into a polycarbosilane solution, and then carrying out in-situ crosslinking curing and cracking; s6, repeating S5 weeksThe period is 2-4 times.
Description
Technical Field
The invention generally relates to the technical field of composite materials, in particular to high-performance SiC f SiC composite material the preparation method of (1).
Background
In order to improve the thermal efficiency of an aircraft engine, which is a constant goal of the aviation industry, there is a great driving force to improve the working temperature of the engine. The upper limit of the temperature of the traditional nickel-based high-temperature alloy is about 1100 ℃, and the requirement that the service temperature of a novel aero-engine is continuously increased cannot be met, so that the development of a novel structural material with low density and capability of bearing higher temperature becomes the key and the foundation for developing a high-performance engine, and the novel structural material is used for replacing the high-temperature alloy and refractory metal materials.
SiC f the/SiC composite material is ideal as a substitute for high temperature alloys and has found application in hot end components such as combustors, turbine blades, vane blades, turbine disks, and the like. SiC f the/SiC composite material has low density, high specific strength and specific modulus, excellent high-temperature mechanical property, oxidation resistance and thermal shock resistance, high reliability and damage tolerance, can effectively improve the air inlet temperature of the aero-engine, and can reduce the weight of a component by more than 50%, which has great significance for improving the thrust-weight ratio of the aero-engine and promoting the independent research and development of a new-generation aero-engine.
At present, siC f The common preparation process of the/SiC composite material comprises the following steps: precursor Impregnation and Pyrolysis (PIP), chemical Vapor Infiltration (CVI), and Reactive Infiltration (RMI).
The precursor impregnation cracking method is that the air in the fiber prefabricated member is removed by a vacuumizing method, then the precursor is filled into the prefabricated member by an impregnation method, and high-temperature cracking is carried out after crosslinking and curing. And the densification of the material is realized after multiple times of dipping and cracking.
The chemical vapor infiltration method comprises the steps of placing the fiber preform in a deposition furnace, conveying pyrolysis gas to the preform through a pressure difference method, and depositing generated solid products (crystallization particles) on the inner pore walls of the preform, wherein the solid products are diffused into a lattice through the surfaces of the solid products, so that the thickness of the surfaces of the pore walls is gradually increased to achieve densification.
The reactive infiltration method realizes the reaction of Si and C to generate SiC by utilizing the capillary action principle in vacuum so as to realize densification.
The PIP process can prepare a component with a complex shape, and the preparation temperature is low, so that the damage to fibers is small; but the cracked product is amorphous SiC, small molecules escape in the process, and the porosity is high. The CVI process can prepare complex components, and the product is SiC with high purity and high crystallinity; but is not suitable for preparing thick-wall components, has complex equipment, long preparation period and high cost, and can not fill macropores among fiber bundles. The RMI process is quick and simple, the cost is low, and the porosity is low; but the existence of residual Si damages the high-temperature performance, and in addition, the preparation temperature is high, and the fiber is greatly damaged.
SiC f The performance of the/SiC composite material is closely related to the preparation process thereof, and the SiC composite material is used for the hot end part of a novel aircraft engine f The composite material has high stability and reliability, excellent high temperature resistance, low preparation cost and short preparation period.
SiC prepared by adopting traditional process at present f the/SiC composite material has high porosity, uneven porosity distribution and uneven microstructure, so that the performance stability is poor, the discreteness is high, the preparation period is long, and the cost is high. Therefore, the development of a SiC with high density, high stability, uniform tissue structure, excellent mechanical properties and short preparation period is urgently needed f A preparation method of a/SiC composite material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides high-performance SiC f A preparation method of a/SiC composite material. The product has high density, high stability, uniform tissue structure and excellent mechanical property, meets the application requirements of the product on hot end parts of the aeroengine, and has short preparation period and simple and convenient process.
The technical scheme of the invention is that the high performance isEnergy SiC f Method for producing a SiC composite material, siC f The SiC composite material takes SiC fiber as a reinforcement and takes silicon carbide as a matrix, the volume fraction of the SiC fibers is 35-45%; the porosity of the composite material is within the range of 10.0-14.0%, and the density is within the range of 2.36-2.40g/cm 3 In the range of 430-500MPa in mechanical property; the dispersion is in the range of 5%, the method comprising the steps of:
s1, carrying out high-temperature heat treatment on the SiC fiber prefabricated part under a vacuum condition to obtain a prefabricated part after glue removal;
s2, placing the prefabricated member obtained in the S1 in a chemical vapor deposition furnace, and depositing a cracking carbon interface layer on the surface of the SiC fiber by taking propylene as a source gas and hydrogen as a carrier gas;
s3, placing the prefabricated part processed in the step S2 in a silicon carbide chemical vapor deposition furnace, and carrying out chemical vapor deposition on a SiC matrix by using methyltrichlorosilane as a precursor, hydrogen as a carrier gas and argon as a diluent gas to obtain a first density intermediate;
s4, preparing SiC precursor solution from solid polycarbosilane and xylene;
s5, vacuum dipping the first density intermediate into the SiC precursor solution prepared in the S4, taking out, airing, performing crosslinking solidification, then cracking under the condition of argon or nitrogen atmosphere, and then cooling along with a furnace to obtain a precursor dipping cracking SiC matrix;
s6, repeating the S5 cycle for 5-7 times to obtain a second density intermediate;
s7, impregnating the second density intermediate in a polycarbosilane solution through mechanical auxiliary pressurization, taking out the impregnated second density intermediate together with a container containing a precursor solution, carrying out in-situ crosslinking and solidification, then carrying out cracking under the condition of argon or nitrogen atmosphere, and then cooling along with a furnace; the mechanical auxiliary pressure is 50-250MPa, the pressure maintaining time is 10-30min, and the impregnation time is 5-8h;
s8, repeating the S7 cycle for 2-4 times to obtain the high-performance SiC f a/SiC composite material.
Further, in the step S1, the high temperature heat treatment conditions are as follows: the temperature is 500-800 ℃, and the heat preservation time is 30-90 min.
Further, in the step S2, the flow rate of propylene is 140-160ml/min, the flow rate of hydrogen is 140-160ml/min, the deposition temperature is 900-1050 ℃, the deposition pressure is 1.5-2kPa, and the deposition time is 10-15h; the final thickness of the obtained cracking carbon interface layer is 200-400nm.
Further, in the step S3, the hydrogen flow is 280-320ml/min, the argon flow is 180-220ml/min, and the CVI SiC matrix is deposited at 1050-1100 ℃ under the pressure condition of 1.3-1.5 kPa for 100-160h; the density of the first intermediate is 1.8-1.9g/cm 3 。
Further, in the above step S4, the SiC precursor solution is prepared from the solid polycarbosilane and xylene in a mass ratio of (1.
Further, in the step S6, the density of the second intermediate is 2.20 to 2.25g/cm 3 。
Further, in the above-mentioned case, in the step S5: the dipping time is 5-8h; the temperature of the step S5 and the step S7 for in-situ crosslinking and curing is 140-160 ℃, and the heat preservation time is as follows: 3-5h; the cracking temperature is 1000-1200 ℃, and the heat preservation time is 1-2h.
Compared with the prior art, the invention has the advantages that:
1. compared with the prior art, the composite material prepared by the invention has higher density, lower porosity, good uniformity and low discreteness, and greatly improves the bending strength. The porosity can be reduced from more than 15% in the prior art to less than 14%, the bending strength can be improved by about 30% compared with the prior art, and the dispersion performance is controlled to be less than 5%.
2. The invention aims at the SiC prepared by the traditional process f The porosity of the/SiC composite material is generally higher than 15%, the porosity distribution is uneven, the microstructure is uneven, the defects of poor mechanical property stability, dispersion larger than 10% and the like are caused, and on the basis of a CVI + PIP combined process, a mechanical auxiliary pressurizing and dipping method is further adopted to prepare SiC with high density, uniform tissue structure and low performance stability and dispersion f A/SiC composite material.
3. In the preparation method, the SiC matrix is firstly deposited by adopting a CVI (chemical vapor infiltration) process, and the deposition rate is controlled to ensure thatThe small holes in the fiber bundle can be effectively filled when the density of the intermediate body reaches 1.8-1.9g/cm 3 And then filling the macropores among the fiber bundles by the SiC matrix cracked by the PIP process. The porosity can be effectively reduced by the combination of CVI + PIP process.
4. Aiming at the technical problems that a PIP cracked SiC matrix is amorphous, a channel of a precursor entering a prefabricated member is easily blocked in the PIP process, a certain closed hole is inevitably formed in the prefabricated member, the performance of a composite material is influenced and the like, the method utilizes a mechanical auxiliary pressurizing and dipping mode to open the blocked closed hole after a CVI + PIP process, so that the precursor can enter the closed hole, the density can be improved, the closed hole rate is reduced, the uniformity of a fiber tissue structure is improved, the mechanical property can be improved, and the stability can be improved.
5. The method adopts a mechanical auxiliary pressurizing and dipping mode, greatly improves the density, reduces the closed pore rate and improves the uniformity and the stability of the tissue structure.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings of which:
FIG. 1 high Performance SiC obtained in example 1 of the invention f Electron microscope pictures of the sections of the/SiC composite materials;
FIG. 2 is a graph comparing the weight gain of the PIP process at step S6 in example 1 of the present invention and comparative example 1;
FIG. 3 SiC produced in example 1 of the present invention, comparative example 1 and comparative example 2 f Comparative plot of density and flexural strength of the/SiC composite.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following detailed description of the invention is provided in conjunction with the accompanying drawings and the detailed description of the invention.
Example 1:
high-performance SiC f The preparation method of the/SiC composite material comprises the following steps:
s1, preserving the heat of a SiC fiber prefabricated part (the volume fraction of the fiber is 45%) in a 2.5D weaving mode for 1h at 600 ℃ under a vacuum condition, and performing high-temperature degumming treatment;
s2, placing the prefabricated member obtained in the S1 into a chemical vapor deposition furnace, and using propylene (C) 3 H 6 ) As source gas, hydrogen (H) 2 ) The carrier gas is propylene flow of 150ml/min, hydrogen flow of 150ml/min, deposition temperature of 900-1050 ℃, deposition pressure of 1.5-2kPa, and deposition of a cracked carbon (PyC) interface layer on the surface of the SiC fiber, wherein the thickness of the interface layer is about 200nm;
s3, placing the prefabricated part obtained in the S2 into a CVI SiC deposition furnace, taking Methyl Trichlorosilane (MTS) as a precursor, carrying the MTS into the furnace chamber in a bubbling mode, and adding hydrogen (H) 2 ) Using argon (Ar) as a carrier gas, using the hydrogen flow of 300ml/min and the argon flow of 200ml/min as a diluent gas, depositing a CVI SiC matrix under the process conditions of the temperature of 1075 ℃ and the pressure of 1.4 kPa for 135-145h, and obtaining an intermediate with the density of 1.85g/cm 3 ；
S4, preparing a SiC precursor from the solid polycarbosilane and the dimethylbenzene according to the mass ratio of 1;
s5, vacuum dipping the intermediate prepared in the S3 into the SiC precursor solution prepared in the S4, dipping for 8h, taking out and airing, then preserving heat for 4h at 150 ℃ for crosslinking and curing, then preserving heat for 1h at 1200 ℃ under the argon atmosphere condition for cracking, then cooling along with a furnace to obtain a PIP SiC matrix, and repeating the PIP cycle for 5 times;
s6, impregnating the intermediate obtained in the step S5 in polycarbosilane solution under mechanical assistance and pressurization, keeping the pressure at 200MPa for 10min, taking out the sample and SiC precursor solution together, preserving the heat at 150 ℃ for 4h for in-situ crosslinking and curing, preserving the heat at 1200 ℃ for 1h for cracking under the argon atmosphere condition, cooling along with a furnace, and repeating PIP4 cycles to obtain high-density SiC f a/SiC composite material.
Comparative example 1 (without mechanical assistance pressure impregnation)
Comparative example 1 differs from example 1 in that: step in S6, instead of using mechanically assisted pressure impregnation, 4 PIP densifications were performed in the same manner as in step S5, with the remainder of the procedure as in example 1.
Comparative example 2
Comparative example 2 differs from example 1 in that: the operation in step S6 is not performed, and the rest of the steps are the same as in example 1.
FIG. 1 shows high-density SiC obtained in example 1 f Electron microscope pictures of the sections of the/SiC composite materials;
fig. 2 is a graph comparing the PIP process weight gain curves at step S6 in example 1 and comparative example 1;
FIG. 3 shows SiC prepared in example 1, comparative example 1 and comparative example 2 f Comparison graph of density and bending strength of the/SiC composite material.
As can be seen from fig. 2, the weight gain efficiency in the PIP process in example 1 is higher, that is, the densification effect is better obtained after the mechanical assisted pressure impregnation, which indicates that the mechanical assisted pressure impregnation and the in-situ curing can better promote the composite material densification process.
From FIG. 3, it can be seen that SiC produced in example 1, comparative example 1 and comparative example 2 f The density of the/SiC composite material is 2.37g/cm respectively 3 ，2.33g/cm 3 And 2.25g/cm 3 The flexural strengths were 472.8. + -. 10.1MPa, 351.4. + -. 18.4MPa and 232.4. + -. 25.9MPa, respectively, and the open cell contents measured by the drainage method were 13.6%,15.9% and 22.7%, respectively. The comparison shows that the prepared composite material has higher density, lower porosity, greatly improved bending strength, good uniformity and low discreteness by mechanically assisting pressurization. It can also be seen from the SEM picture of fig. 1 that the composite material has a uniform and dense microstructure.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (7)
1. High-performance SiC f A preparation method of a/SiC composite material,characterized in that the SiC f the/SiC composite material takes SiC fibers as a reinforcement and takes silicon carbide as a matrix, and the volume fraction of the SiC fibers is 35-45%; the porosity of the composite material is within the range of 10.0-14.0%, and the density is within the range of 2.36-2.40g/cm 3 Within the range, the mechanical property is within the range of 430-500MPa, and the discreteness is within the range of 5%; the method comprises the following steps:
s1, carrying out high-temperature heat treatment on the SiC fiber prefabricated part under a vacuum condition to obtain a prefabricated part after glue removal;
s2, placing the prefabricated member obtained in the S1 in a chemical vapor deposition furnace, and depositing a cracking carbon interface layer on the surface of the SiC fiber by taking propylene as a source gas and hydrogen as a carrier gas;
s3, placing the prefabricated part processed in the step S2 in a silicon carbide chemical vapor deposition furnace, and carrying out chemical vapor deposition on a SiC matrix by using methyltrichlorosilane as a precursor, hydrogen as a carrier gas and argon as a diluent gas to obtain a first density intermediate;
s4, preparing SiC precursor solution from solid polycarbosilane and xylene;
s5, vacuum dipping the first density intermediate into the SiC precursor solution prepared in the S4, taking out, airing, performing crosslinking solidification, then cracking under the condition of argon or nitrogen atmosphere, and then cooling along with a furnace to obtain a precursor dipping cracking SiC matrix;
s6, repeating the S5 cycle for 5-7 times to obtain a second density intermediate;
s7, impregnating the second density intermediate in a polycarbosilane solution through mechanical auxiliary pressurization, taking out the impregnated second density intermediate together with a container containing a precursor solution, carrying out in-situ crosslinking and solidification, then carrying out cracking under the condition of argon or nitrogen atmosphere, and then cooling along with a furnace; the mechanical auxiliary pressure is 50-250MPa, the pressure maintaining time is 10-30min, and the impregnation time is 5-8h;
s8, repeating the S7 cycle for 2-4 times to obtain the high-performance SiC f a/SiC composite material.
2. High performance SiC according to claim 1 f Method for producing a/SiC composite materialCharacterized in that, in step S1, the high-temperature heat treatment conditions are as follows: the temperature is 500-800 ℃, and the heat preservation time is 30-90 min.
3. High performance SiC according to claim 1 f The preparation method of the/SiC composite material is characterized in that in the step S2, the flow rate of propylene is 140-160ml/min, the flow rate of hydrogen is 140-160ml/min, the deposition temperature is 900-1050 ℃, the deposition pressure is 1.5-2kPa, and the deposition time is 10-15h; the final thickness of the obtained cracking carbon interface layer is 200-400nm.
4. High performance SiC according to claim 1 f The preparation method of the/SiC composite material is characterized in that in the step S3, hydrogen flow is 280-320ml/min, argon flow is 180-220ml/min, a CVI SiC matrix is deposited under the conditions of 1050-1100 ℃ temperature and 1.3-1.5 kPa pressure, and the deposition time is 100-160h; the density of the first intermediate is 1.8-1.9g/cm 3 。
5. High performance SiC according to claim 1 f The preparation method of the SiC composite material is characterized in that in the step S4, the SiC precursor solution is prepared by mixing the solid polycarbosilane and the dimethylbenzene according to the mass ratio of (1.
6. High performance SiC according to claim 1 f The preparation method of the/SiC composite material is characterized in that in the step S6, the density of the second intermediate is 2.20-2.25g/cm 3 。
7. High performance SiC according to claim 1 f The preparation method of the/SiC composite material is characterized in that in the step S5: the dipping time is 5-8h; in the step S5 and the step S7, the temperature of in-situ crosslinking and curing is 140-160 ℃, and the heat preservation time is as follows: 3-5h; the cracking temperature is 1000-1200 ℃, and the heat preservation time is 1-2h.
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