CN111039686A - Preparation method of continuous fiber reinforced ceramic matrix composite material containing in-situ pores - Google Patents
Preparation method of continuous fiber reinforced ceramic matrix composite material containing in-situ pores Download PDFInfo
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Abstract
The invention relates to a preparation method of a continuous fiber reinforced ceramic matrix composite material containing in-situ pores, which realizes the maintenance of the structural integrity of the continuous fiber reinforced ceramic matrix composite material while obtaining a pore structure by controlling the processes of preparation of a continuous fiber preform containing in-situ pore structures, fixation of in-situ pore structures, filling of ceramic matrixes and the like, and compared with the existing post-processing pore-making method, the preparation method of the continuous fiber reinforced ceramic matrix composite material containing in-situ pores has the advantages of no damage to continuous fibers and matrixes, high efficiency and low cost, and can improve the mechanical property of the continuous fiber reinforced ceramic matrix composite material containing the pore structures by 10-60%.
Description
Technical Field
The invention discloses a preparation method of a continuous fiber reinforced ceramic matrix composite material containing in-situ pores, belonging to the technical field of preparation of ceramic matrix composite materials.
Background
The continuous fiber reinforced ceramic matrix composite has the advantages of high temperature resistance, oxidation resistance, wear resistance, corrosion resistance and the like of ceramic materials, and has excellent external impact load resistance due to the reinforcing and toughening effects of the continuous fibers. The continuous fiber reinforced ceramic matrix composite is more and more widely applied in the fields of advanced aircraft engine hot end parts, advanced aircraft thermal protection systems and the like by virtue of good high-temperature stability and high-temperature mechanical properties.
Continuous fiber reinforced ceramic matrix composites typically contain pore structures for joining, assembly, as cooling channels, and the like in practical applications. At present, the commonly used hole making mode is to make holes on the complete material by adopting a post-processing mode, such as machining, drilling, laser hole making, water cutting hole making, linear cutting hole making and the like, and all the modes can cause that continuous fibers and matrixes in the material are damaged, so that the mechanical property of the material is reduced, and the integral service performance of the component is further influenced. In addition, the ceramic matrix composite material belongs to a typical difficult-to-machine material due to ultrahigh hardness, non-uniformity of the material and large brittleness, and a post-machining mode has high hole making difficulty and high cost. In the field of advanced aero-engines, thousands or even tens of thousands of array air film holes are required to be prepared for part of hot end members at positions such as a combustion chamber, the air film holes are small in aperture and large in number, the processing difficulty is high, the cost is high, and in addition, for the hot end members of the continuous fiber reinforced ceramic matrix composite, a large number of air film holes can cause serious damage to continuous fibers and a matrix, so that the mechanical property of the members is greatly reduced. How to obtain the pore structure and simultaneously keep the structural integrity of the continuous fiber reinforced ceramic matrix composite, how to obtain the pore structure with high efficiency and low cost, and the problem to be solved in the application field of the continuous fiber reinforced ceramic matrix composite are needed.
Disclosure of Invention
The invention provides a preparation method of a continuous fiber reinforced ceramic matrix composite material containing in-situ pores aiming at the prior art situation, and aims to provide an effective solution for the preparation of the continuous fiber reinforced ceramic matrix composite material containing the pore structure.
The technical solution of the invention is as follows:
the preparation method of the continuous fiber reinforced ceramic matrix composite material containing the in-situ pores comprises the following steps:
preparing a continuous fiber preform containing an in-situ pore structure according to the size and position requirements of pores, wherein the in-situ pore is formed by a cavity which is surrounded by continuous fibers and does not contain the continuous fibers;
step two, fixing the in-situ pore structure, wherein the fixing mode adopts one of the following modes according to the characteristics of the continuous fiber preform:
the first mode is as follows: aiming at a continuous fiber preform of a prepreg type, carrying out heat treatment on the preform to cure or carbonize resin and fix an in-situ pore structure;
the second mode is as follows: aiming at a non-prepreg type continuous fiber preform, preparing a fixing layer on the surface of the continuous fiber preform to fix the in-situ pore structure, wherein the fixing layer is made of pyrolytic carbon, boron nitride, silicon carbide and organic polymer;
and step three, filling the ceramic matrix aiming at the pores except the in-situ pore structure in the continuous fiber preform, wherein the in-situ pores are not filled by the ceramic matrix, and other pores are filled by the ceramic matrix, so that the densification of the continuous fiber reinforced ceramic matrix composite material containing the in-situ pores is completed, and the continuous fiber reinforced ceramic matrix composite material containing the in-situ pores is obtained.
In a second mode of carrying out step two, the thickness of the immobilizing layer is from 500nm to 100 μm.
In one implementation, the in situ pore size is not less than 0.1 mm.
In one implementation, the distribution of in-situ pores is an array distribution.
In one implementation, the continuous fibers are carbon fibers, silicon carbide fibers, nitride fibers, oxide fibers.
In one implementation, the preparation method of the continuous fiber preform is silk laying, tape laying, layer laying, weaving and hand knitting, and the structure of the continuous fiber preform is unidirectional tape, 2D layer laying, 2.5D knitting and 3D knitting.
In one implementation, the fixed layer is prepared by chemical vapor infiltration or liquid phase impregnation.
In one implementation, the ceramic matrix is silicon carbide, nitride ceramic, oxide ceramic.
In one implementation, when the ceramic matrix is filled by adopting liquid phase impregnation, particularly for the thin-wall structure continuous fiber reinforced ceramic matrix composite, the surface of the continuous fiber preform is in contact with a liquid phase impregnant and is not immersed by the liquid phase impregnant, the control of the critical pore size is realized by adjusting the viscosity of the liquid phase impregnant according to the capillary action principle, so that the critical pore size corresponding to the impregnant is larger than the pore size except the in-situ pore structure in the continuous fiber preform, the liquid phase impregnant can fully fill the pores except the in-situ pore structure through the capillary action, the size of the in-situ pore is larger than the critical pore size and cannot be filled, the in-situ pore in the continuous fiber reinforced ceramic matrix composite is finally reserved and formed, the sizes of other pores are smaller than the critical pore size and are filled by the impregnant, and the ceramic matrix is finally filled for densification, the critical pore size is 0.05 mm-5 mm in diameter, and the impregnant is organic resin, inorganic solution or liquid metal. For the continuous fiber reinforced ceramic matrix composite with thicker wall thickness, the continuous fiber preform needs to be partially or completely immersed in the liquid phase impregnant to fully fill the pores, then the continuous fiber preform leaves the liquid phase impregnant, the impregnant in the in-situ pores is discharged under the action of gravity due to lack of capillary action, impregnants in other pores can keep a filling state due to capillary action, if the liquid phase impregnant still remains in the in-situ pores, the remaining liquid phase impregnant can be further removed through physical and chemical modes to realize the retention of the in-situ pore structure, and the removal mode is vacuum suction, high-speed air flow blowing, dissolution removal and reaction removal.
In one implementation, when the ceramic matrix is filled with the gas-phase precursor, the gas flow field is controlled in the chemical gas-phase permeation process without deposition in the in-situ hole, so that the in-situ hole is not filled and is reserved and forms the in-situ hole in the continuous fiber reinforced ceramic matrix composite, deposition occurs in other pores and is filled, and finally the ceramic matrix is filled to densify, and the gas flow field control mode is to set a flow guide device and control the components and concentration of process gas.
The invention has the advantages and beneficial effects that: the preparation method of the in-situ pore-containing continuous fiber reinforced ceramic matrix composite realizes the pore structure and simultaneously keeps the structural integrity of the continuous fiber reinforced ceramic matrix composite through the process control of the preparation of the continuous fiber preform containing the in-situ pore structure, the fixation of the in-situ pore structure, the filling of the ceramic matrix and the like, compared with the existing post-processing pore-making method, the method has the advantages of no damage to continuous fibers and a matrix, high efficiency and low cost, and can improve the mechanical property of the continuous fiber reinforced ceramic matrix composite containing the pore structure by 10-60 percent.
Description of the drawings:
FIG. 1 is a schematic representation of a continuous fiber preform containing an in situ pore structure according to the examples;
FIG. 2 is a schematic view of a continuous fiber and a fixing layer in an embodiment;
FIG. 3 is a schematic illustration of the ceramic matrix filling in the examples.
The specific implementation mode is as follows:
the invention is described in further detail below with reference to the following embodiments and with reference to the following figures:
referring to attached drawings 1-3, the preparation method of the continuous silicon carbide fiber reinforced silicon carbide ceramic matrix composite aeroengine hot end component with the array air film hole structure comprises the following steps of:
step one, preparing a continuous fiber preform containing an in-situ pore structure according to the size and position requirements of pores: preparing a continuous fiber preform 1 with an in-situ hole 2 structure according to the size and position requirements of the in-situ hole 2, weaving the 2.5D structure preform by adopting continuous silicon carbide fibers, and arranging the spatial positions of warp yarns and weft yarns by a weaving machine to obtain the continuous silicon carbide fiber preform 1 with the in-situ hole 2 and other pores 3, wherein the radial size of the in-situ hole 2 is 0.9mm, the sizes of the other pores 3 are less than 0.1mm, the in-situ holes 2 are distributed in a matrix manner, the distance between adjacent columns is 3mm, and the distance between adjacent rows is 2 mm;
step two, fixing the in-situ pore structure: preparing a fixed layer 5 on the surface of the continuous silicon carbide fiber 4 by adopting a chemical vapor infiltration process to fix the in-situ hole 2 structure, wherein the fixed layer 5 is made of pyrolytic carbon, and the thickness of the fixed layer 5 is 50 microns;
step three, filling the ceramic matrix 6 into the pores 3 except the in-situ pore 2 structure in the continuous fiber preform 1: and filling the ceramic matrix by adopting a polycarbosilane impregnation cracking process, wherein the critical pore size corresponding to the polycarbosilane liquid impregnant is 0.1mm in diameter, so that the surface of the continuous fiber preform 1 is in contact with the liquid phase impregnant and is not immersed by the liquid phase impregnant, the liquid phase impregnant fully fills the pores 3 except the structure of the in-situ pores 2 through capillary action, the sizes of the in-situ pores 2 are larger than the critical pore size and cannot be filled, the in-situ pores 2 in the continuous silicon carbide fiber reinforced silicon carbide ceramic matrix composite material 7 are finally reserved and formed, the sizes of the other pores 3 are smaller than the critical pore size and are filled by the impregnant, and the in-situ pores 2 are finally filled and densified by the silicon carbide ceramic matrix 6 through cracking, so that the continuous silicon carbide fiber reinforced silicon carbide ceramic matrix composite material 7 containing the in-situ pores 2 is.
Claims (9)
1. A preparation method of a continuous fiber reinforced ceramic matrix composite material containing in-situ pores is characterized by comprising the following steps: the method comprises the following steps:
preparing a continuous fiber preform containing an in-situ pore structure according to the size and position requirements of pores, wherein the in-situ pore is formed by a cavity which is surrounded by continuous fibers and does not contain the continuous fibers;
step two, fixing the in-situ pore structure, wherein the fixing mode adopts one of the following modes according to the characteristics of the continuous fiber preform:
the first mode is as follows: aiming at a continuous fiber preform of a prepreg type, carrying out heat treatment on the preform to cure or carbonize resin and fix an in-situ pore structure;
the second mode is as follows: aiming at a non-prepreg type continuous fiber preform, preparing a fixing layer on the surface of the continuous fiber preform to fix the in-situ pore structure, wherein the fixing layer is made of pyrolytic carbon, boron nitride, silicon carbide and organic polymer;
and step three, filling the ceramic matrix aiming at the pores except the in-situ pore structure in the continuous fiber preform, wherein the in-situ pores are not filled by the ceramic matrix, and other pores are filled by the ceramic matrix, so that the densification of the continuous fiber reinforced ceramic matrix composite material containing the in-situ pores is completed, and the continuous fiber reinforced ceramic matrix composite material containing the in-situ pores is obtained.
2. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: in a second mode of the second step, the thickness of the anchor layer is 500nm to 100. mu.m.
3. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: the aperture of the in-situ hole is not less than 0.1 mm.
4. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: the distribution of the in-situ holes is array distribution.
5. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: the continuous fiber is carbon fiber, silicon carbide fiber, nitride fiber or oxide fiber.
6. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: the preparation method of the continuous fiber preform comprises the steps of silk laying, belt laying, layer laying, weaving and hand knitting, and the structure of the continuous fiber preform comprises a unidirectional belt, a 2D layer laying, a 2.5D knitting and a 3D knitting.
7. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: the preparation method of the fixed layer is chemical vapor infiltration and liquid phase impregnation.
8. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: the ceramic matrix is silicon carbide, nitride ceramic or oxide ceramic.
9. The method of preparing an in-situ pore containing continuous fiber reinforced ceramic matrix composite as claimed in claim 1, wherein: when the ceramic matrix is filled by liquid phase impregnation, the critical pore size of the impregnant should be larger than the pore size of the continuous fiber preform except for the in-situ pore structure.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112251906A (en) * | 2020-10-12 | 2021-01-22 | 南京航空航天大学 | Air film cooling hole braided structure suitable for ceramic matrix composite material member and manufacturing method thereof |
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| CN101405238A (en) * | 2006-02-01 | 2009-04-08 | 圣戈班欧洲设计研究中心 | Impregnated ceramic foam made of recrystallized silicon carbide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112251906A (en) * | 2020-10-12 | 2021-01-22 | 南京航空航天大学 | Air film cooling hole braided structure suitable for ceramic matrix composite material member and manufacturing method thereof |
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