CN117185827A - Annular thin-wall component made of ceramic matrix composite material and preparation method thereof - Google Patents
Annular thin-wall component made of ceramic matrix composite material and preparation method thereof Download PDFInfo
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- CN117185827A CN117185827A CN202311255014.3A CN202311255014A CN117185827A CN 117185827 A CN117185827 A CN 117185827A CN 202311255014 A CN202311255014 A CN 202311255014A CN 117185827 A CN117185827 A CN 117185827A
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- 239000011153 ceramic matrix composite Substances 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000835 fiber Substances 0.000 claims abstract description 66
- 239000004744 fabric Substances 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 19
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 17
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 17
- 238000000465 moulding Methods 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001257 hydrogen Substances 0.000 claims abstract description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 239000002153 silicon-carbon composite material Substances 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010000 carbonizing Methods 0.000 claims abstract description 8
- 229910000077 silane Inorganic materials 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 7
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 44
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 44
- 238000001764 infiltration Methods 0.000 claims description 36
- 230000008595 infiltration Effects 0.000 claims description 35
- 238000000151 deposition Methods 0.000 claims description 34
- 230000008021 deposition Effects 0.000 claims description 27
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 26
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 23
- 239000004917 carbon fiber Substances 0.000 claims description 23
- 239000000919 ceramic Substances 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 238000003763 carbonization Methods 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 13
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 11
- 239000005011 phenolic resin Substances 0.000 claims description 11
- 229920001568 phenolic resin Polymers 0.000 claims description 11
- 239000011863 silicon-based powder Substances 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 238000011534 incubation Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 19
- 238000002679 ablation Methods 0.000 abstract description 3
- 239000002184 metal Substances 0.000 description 23
- 238000001816 cooling Methods 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 8
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
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- 238000009423 ventilation Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 description 3
- 239000001294 propane Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000012945 sealing adhesive Substances 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000003698 laser cutting Methods 0.000 description 2
- 238000000626 liquid-phase infiltration Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
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- 238000007740 vapor deposition Methods 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 230000037303 wrinkles Effects 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
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- 238000005498 polishing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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Abstract
The invention provides a ceramic matrix composite annular thin-wall member and a preparation method thereof, comprising the following steps: a) Arranging fibers in a chemical vapor deposition furnace, and introducing a carbon source and hydrogen to obtain fiber cloth deposited with pyrolytic carbon; b) Introducing silane gas and hydrogen to obtain fiber cloth deposited with a silicon-carbon composite interface; c) Coating the surface with prepreg slurry to obtain fiber prepreg; d) Molding the fiber prepreg on the surface of a mold to obtain a resin-based annular blank; e) Sequentially carbonizing and infiltrating the resin-based annular blank to obtain a ceramic matrix composite annular blank; f) And (5) carrying out size processing on the upper end face and the lower end face to obtain the annular thin-wall component made of the ceramic matrix composite material. The composite material member prepared by the method has extremely low porosity, so that the member has excellent high-temperature ablation resistance and high-temperature durability in the application field of aerospace thermostructural materials.
Description
Technical Field
The invention belongs to the technical field of ceramic composite materials, and particularly relates to a ceramic matrix composite annular thin-wall member and a preparation method thereof.
Background
Ceramic matrix composite materials are lightweight and high temperature resistant, and have been applied to aerospace thermal structural materials, and annular components are commonly used for hot end components of aircraft engines, such as structures of combustion chambers, turbine outer rings and the like. In recent years, in order to further improve the performance of the aeroengine, the temperature resistance level of the hot end part is also improved, and the ceramic matrix composite material has good temperature resistance, so that the ceramic matrix composite material becomes the most potential hot end part material of a new generation of engines.
In the manufacturing process of ceramic matrix composite components, the molding technique is one of the key techniques. At present, a mature molding technology is that a fiber preform is woven and molded, namely, carbon fibers are woven on the surface of a graphite mold to form a three-dimensional preform, and then densification treatment is carried out on the fiber preform in a state of a mold through manufacturing technologies such as chemical vapor deposition (CVI), precursor impregnation cracking (PIP) or Melt Infiltration (MI), and finally, a ceramic matrix composite component with a complex shape is formed. However, the method is difficult to achieve near-net-size molding of the component, has the limitations of large processing allowance, high cost and the like, and particularly has certain deviation between the actual size and the design size for the thin-wall annular or cylindrical component limited by the braiding technology, so that the component needs to be processed in a large area after molding, and the mechanical property of the component is damaged. In the field of hot end components of aeroengines and hypersonic aircrafts, the thin-wall ring and barrel-shaped components are widely applied, such as components of turbine outer rings, flame barrels and the like of aeroengines, the wall thickness is not more than 5mm, and the cross section characteristics are annular, so that the thin-wall ring-shaped ceramic matrix composite component has important significance in the research on the preparation method of the thin-wall ring-shaped ceramic matrix composite component.
Disclosure of Invention
The invention aims to provide a ceramic matrix composite annular thin-wall member and a preparation method thereof.
The invention provides a preparation method of a ceramic matrix composite annular thin-wall member, which comprises the following steps:
a) Arranging carbon fiber cloth or silicon carbide fiber in a chemical vapor deposition furnace, introducing a carbon source and hydrogen, and depositing to obtain fiber cloth deposited with pyrolytic carbon;
b) Introducing silane gas and hydrogen gas for deposition to obtain fiber cloth deposited with a silicon-carbon composite interface;
c) Coating prepreg slurry on the surface of the fiber cloth deposited with the silicon-carbon composite interface to obtain fiber prepreg;
the prepreg comprises phenolic resin, siC ceramic particles and an organic solvent;
d) Molding the fiber prepreg on the surface of a mold to obtain a resin-based annular blank;
e) Sequentially carbonizing and infiltrating the resin-based annular blank to obtain a ceramic matrix composite annular blank;
f) And performing dimension processing on the upper end face and the lower end face of the annular ceramic matrix composite blank to obtain the annular thin-wall ceramic matrix composite member.
Preferably, the temperature of the deposition in the step A) is 900-1100 ℃, and the deposition time is 10-15 hours.
Preferably, the temperature of the deposition in the step B) is 900-1200 ℃, and the deposition time is 10-15 hours.
Preferably, the mass ratio of phenolic resin to SiC ceramic particles in the prepreg slurry is (0.3-0.6): 1, the mass fraction of the organic solvent in the prepreg slurry is 20-40%.
Preferably, the weight of the fiber cloth deposited with the silicon-carbon composite interface is increased by 80-150% after the fiber prepreg is formed.
Preferably, the carbonization is performed under an argon atmosphere, the carbonization temperature is 800-1000 ℃, and the heat preservation time is 0.5-2 hours.
Preferably, the outer wall of the carbonized annular blank is coated with an infiltration agent for infiltration, wherein the infiltration agent comprises silicon powder and polyvinyl alcohol;
the mass ratio of Si powder in the infiltration agent to the carbonized annular blank is (2.5-3.5): 1.
preferably, the infiltration is performed under vacuum, the temperature of the infiltration is 1450-1550 ℃, and the heat preservation time is 20-40 min.
The invention provides the ceramic matrix composite annular thin-wall member prepared by the preparation method.
Preferably, the porosity of the annular thin-wall component made of the ceramic matrix composite is less than 1%.
The invention provides a preparation method of a ceramic matrix composite annular thin-wall member, which comprises the following steps: a) Arranging carbon fiber cloth or silicon carbide fiber in a chemical vapor deposition furnace, introducing a carbon source and hydrogen, and depositing to obtain fiber cloth deposited with pyrolytic carbon; b) Introducing silane gas and hydrogen gas for deposition to obtain fiber cloth deposited with a silicon-carbon composite interface; c) Coating prepreg slurry on the surface of the fiber cloth deposited with the silicon-carbon composite interface to obtain fiber prepreg; the prepreg comprises phenolic resin, siC ceramic particles and an organic solvent; d) Molding the fiber prepreg on the surface of a mold to obtain a resin-based annular blank; e) Sequentially carbonizing and infiltrating the resin-based annular blank to obtain a ceramic matrix composite annular blank; f) And performing dimension processing on the upper end face and the lower end face of the annular ceramic matrix composite blank to obtain the annular thin-wall ceramic matrix composite member. In the prior art, fibers are woven into a component preform fabric, and then a ceramic matrix composite component is obtained by a densification method of chemical vapor deposition and precursor dipping and cracking, so that the obtained component has low densification degree, contains about 10% of air holes inside, and influences the ablation resistance of the component in a high-temperature environment. The invention provides a preparation method of a ceramic matrix composite thin-wall annular component based on a prepreg-infiltration process, which is characterized in that the ceramic matrix composite component is obtained through preparation of fiber prepregs, metal mold paving and molding and carbonization infiltration technology, and the composite component prepared by the method has extremely low porosity, so that the component has excellent high-temperature ablation resistance and high-temperature durability in the application field of aerospace thermal structural materials.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic drawing showing the laying-up of a metal mold and a fiber prepreg used in the present invention,
FIG. 2 is a schematic diagram of the assembly of a porous annular blank with a sizing tool;
FIG. 3 is an SEM microcosmic morphology picture of a ceramic matrix composite annular thin-walled member prepared in example 1 of the present invention;
in fig. 1 to 2, 1 is a metal mold, 2 is a stripper ring, 3 is prepreg laying, 4 is a BN tooling, and 5 is a porous annular blank.
Detailed Description
The invention provides a preparation method of a ceramic matrix composite annular thin-wall member, which comprises the following steps:
a) Arranging carbon fiber cloth or silicon carbide fiber in a chemical vapor deposition furnace, introducing a carbon source and hydrogen, and depositing to obtain fiber cloth deposited with pyrolytic carbon;
b) Introducing silane gas and hydrogen gas for deposition to obtain fiber cloth deposited with a silicon-carbon composite interface;
c) Coating prepreg slurry on the surface of the fiber cloth deposited with the silicon-carbon composite interface to obtain fiber prepreg;
the prepreg comprises phenolic resin, siC ceramic particles and an organic solvent;
d) Molding the fiber prepreg on the surface of a mold to obtain a resin-based annular blank;
e) Sequentially carbonizing and infiltrating the resin-based annular blank to obtain a ceramic matrix composite annular blank;
f) And performing dimension processing on the upper end face and the lower end face of the annular ceramic matrix composite blank to obtain the annular thin-wall ceramic matrix composite member.
The invention firstly adopts a chemical vapor deposition method to prepare the fiber prepreg, and comprises the following specific steps:
vertically hanging unidirectional fiber cloth in a vertical chemical vapor deposition furnace by using a carbon rope, electrifying and heating to a deposition temperature, introducing a vapor carbon source and hydrogen into a hearth, maintaining at the deposition temperature, performing chemical vapor deposition, and naturally cooling to obtain carbon fiber cloth for depositing a pyrolytic carbon (PyC) interface layer;
in the invention, the unidirectional fiber cloth is preferably carbon fiber cloth or silicon carbide fiber cloth; the gaseous carbon source is preferably propane and/or propylene; the volume flow ratio of the carbon source to the hydrogen is preferably 2: 3-1: 1, a step of; the temperature of the chemical vapor deposition is preferably 900 to 1100 ℃, more preferably 950 to 1050 ℃, such as 900 ℃,950 ℃,1000 ℃,1050 ℃,1100 ℃, preferably a range value with any of the above values as an upper limit or a lower limit; the time for the chemical vapor deposition is preferably 10 to 15 hours, more preferably 12 to 13 hours.
Then vertically hanging the obtained fiber cloth for depositing the PyC interface layer in a vertical chemical vapor deposition furnace, electrifying and heating to a deposition temperature, introducing silane gas, hydrogen and argon into a hearth, maintaining at the deposition temperature, performing chemical vapor deposition, and naturally cooling to obtain the fiber cloth for depositing the PyC/SiC composite interface;
in the present invention, the silane gas is preferably a trichloromethylsilane gas; the volume flow ratio of the silane gas to the hydrogen gas is preferably 1: (5 to 10), more preferably 1: (6-9), such as 1:5,1:6,1:7,1:8,1:9 or 1:10, preferably a range value having any of the above values as an upper or lower limit; the temperature of the chemical vapor deposition is preferably 900 to 1200 ℃, more preferably 1000 to 1100 ℃, such as 900 ℃,950 ℃,1000 ℃,1050 ℃,1100 ℃,1150 ℃,1200 ℃, preferably a range value with any of the above values as an upper limit or a lower limit; the time for the chemical vapor deposition is preferably 10 to 15 hours, more preferably 12 to 13 hours.
In the two-time deposition process, in order to enable the carbon fiber cloth to be vertically suspended in the vapor deposition furnace, the porous carbon foam flat plates are preferably clamped at two sides of the carbon fiber cloth, the porosity of the porous carbon foam flat plates is 85-90%, and the thickness of the porous carbon foam flat plates is 9-10 mm.
And preparing a composite interface layer PyC/SiC on the surface of the carbon fiber or the SiC fiber through two-step deposition. The roles of the composite interface include: firstly, pyC is deposited on the surface of the fiber to provide proper interface bonding energy to play a role in reinforcing the fiber, so that a material with good mechanical properties is obtained; secondly, the PyC/SiC composite interface can effectively block the reaction of the melt on the fiber in the subsequent infiltration step, and ensure the integrity of the fiber, thereby ensuring that the material has good mechanical properties.
And coating prepreg slurry on the surface of the fiber cloth of the PyC/SiC composite interface, and standing to obtain the fiber prepreg. The prepreg is commonly used for molding resin-based materials, the annular component is a ceramic-based material, and the prepreg slurry contains phenolic resin, siC ceramic particles and an organic solvent. The organic solvent is preferably absolute ethyl alcohol, and the particle size of the SiC ceramic particles is less than 10 microns; the mass ratio of the phenolic resin to the SiC ceramic particles in the prepreg slurry is preferably (0.3-0.6): 1, more preferably (0.4 to 0.5), and the mass fraction of the organic solvent in the prepreg slurry is preferably 20 to 40%, and still more preferably 25 to 35%.
In the invention, after the fiber prepreg is formed, the weight of the fiber prepreg is increased by 80-150%, preferably 100-120% compared with the fiber cloth deposited with the silicon-carbon composite interface; and after the coating is finished, standing for 4 to 5 hours under the room temperature ventilation condition to obtain the fiber prepreg.
After the fiber prepreg is obtained, the fiber prepreg is molded by using a mold to prepare a molded blank, and the specific steps are as follows:
paving release paper on the surface of a metal mold shown in fig. 1, putting a release ring into the mold, paving the prepared carbon fiber prepreg layer by layer along the upper part of the release ring, and paving the prepreg circularly according to the paving angles of the metal mold of 0 DEG and 90 DEG;
wrapping the metal mold with a separating film, wrapping a layer of airfelt, adhering sealing adhesive tapes at the upper end and the lower end of the metal mold, and sealing the molded prepreg with a vacuum bag;
vacuumizing the vacuum bag, fully removing air between the layers of the prepreg, placing the prepreg into autoclave equipment, applying air pressure, heating, and preserving heat for a certain time to obtain the resin-based annular blank.
In the present invention, the outer diameter D of the metal mold is the desired inner diameter D of the annular member product minus the thickness h of the release paper, i.e., d=d-h.
In the present invention, the molding pressure is preferably 1 to 2MPa; the molding temperature is preferably 180-200 ℃, more preferably 190-195 ℃; the holding time for the molding is preferably 1 to 3 hours, more preferably 2 to 2.5 hours.
After the resin-based annular blank is obtained, the ceramic matrix composite component is prepared by adopting an infiltration reaction method. Specifically, the resin-based annular blank is changed into a ceramic-based annular blank by two steps of carbonization and infiltration, the resin-based annular blank is subjected to carbonization heat treatment, resin is crosslinked and cracked to form porous carbon, a porous matrix is formed, and then molten silicon powder is infiltrated into the porous matrix by infiltration, and a SiC ceramic matrix is formed by chemical reaction. The method comprises the following specific steps:
and (3) placing the obtained resin-based annular blank into a carbonization furnace, and carbonizing under an argon atmosphere to obtain a porous annular blank.
In the present invention, the temperature of the carbonization is preferably 800 to 1000 ℃, more preferably 850 to 950 ℃, and the heating rate of the carbonization is preferably 0.3 to 0.6 ℃/min, more preferably 0.4 to 0.5 ℃/min when the temperature is below 600 ℃, and the heating rate of the carbonization is preferably 0.9 to 1.2 ℃/min, more preferably 1 to 1.1 ℃/min when the temperature is above 600 ℃; the holding time for the carbonization is preferably 0.5 to 2 hours, more preferably 1 to 1.5 hours.
And (3) assembling and shaping the porous annular blank, as shown in fig. 2, putting the porous annular blank into an infiltration furnace, uniformly coating an infiltration agent on the outer wall of the annular blank, performing infiltration reaction, and naturally cooling to obtain the annular blank of the ceramic matrix composite material.
In the invention, the shaping tool is made of boron nitride material, the infiltration agent comprises silicon powder and is prepared from polyvinyl alcohol aqueous solution, and the mass concentration of the polyvinyl alcohol aqueous solution is preferably 3-8%, more preferably 5-6%; the mass ratio of the silicon powder to the polyvinyl alcohol aqueous solution is preferably (8-10): 1, more preferably 9:1, a step of; the mass ratio of the silicon powder to the porous annular blank in the infiltration agent is preferably (2.5-3.5): 1, more preferably 3:1.
in the present invention, the infiltration is preferably performed under a vacuum environment, and the temperature of the infiltration is preferably 1450 to 1550 ℃, more preferably 1500 ℃; the soaking and soaking heat preservation time is preferably 20-40 min, more preferably 30-35 min.
After the annular ceramic matrix composite blank is obtained, the net sizes of the inner diameter and the outer diameter of the blank are molded, and the annular ceramic matrix composite member can be obtained by only mechanically or laser processing the upper end face and the lower end face of the blank.
The invention also provides a ceramic matrix composite annular thin-wall member, which is prepared according to the preparation method, has the wall thickness of 2-5 mm, higher compactness, porosity less than 1%, higher mechanical strength and tensile strength more than 200MPa; the net shape of the inner and outer diameters of the annular part manufactured by the method has the characteristics of reducing machining allowance and production cost; the production period is shorter; because the annular component is designed by adopting continuous fibers, the annular component has high strength and long service life, and is beneficial to improving the use safety. The heat-resistant annular component can be applied to the fields of hot end components of aeroengines and hypersonic aircrafts, in particular to annular components such as turbine outer rings, flame tubes and the like of aeroengines.
For further explanation of the present invention, the following description is given in detail of a ceramic matrix composite annular thin-walled member and a method for preparing the same, but the following description is not to be construed as limiting the scope of the present invention.
Example 1
C with inner diameter of 226mm, wall thickness of 3mm and height of 35mm f The preparation method of the SiC composite annular member comprises the following steps:
1. selecting a carbon fiber unidirectional cloth of Dongli T300-6K in Japan, clamping two sides by porous carbon foam with volume fraction of 10% and thickness of 10mm, vertically hanging a plurality of carbon fiber unidirectional cloths in a PyC deposition furnace by using a carbon rope, introducing propane and hydrogen for deposition for 10 hours at 1000 ℃, and cooling along with furnace cooling;
2. filling the carbon fiber unidirectional cloth after PyC deposition into a SiC deposition furnace by adopting the method in the step 1, introducing trichloromethylsilane gas, hydrogen and argon at 1050 ℃, preserving heat for 10 hours, and then cooling along with the furnace;
3. mixing thermosetting phenolic resin, siC particles and absolute ethyl alcohol according to the mass ratio of 2:6:2, ball milling for 24 hours to prepare slurry, uniformly coating the slurry on SiC fiber unidirectional cloth formed by a deposition composite interface, and carrying out ventilation drying for 4 hours to obtain carbon fiber prepreg for standby;
4. manufacturing a metal mold by using P20 steel, wherein the outer diameter of the mold is 225mm, pasting release paper with the thickness of 0.5mm on a paving area on the surface of the mold, cutting a carbon fiber prepreg into a long rectangular shape, calculating the width and length of the rectangle according to the height and the perimeter of a component, and then paving the carbon fiber prepreg on the surface of the metal mold in sequence according to the 0 degree/90 degree (circumference/height) direction until reaching the preset thickness, wherein a gap of 2mm is reserved at a joint when paying attention to 90 degree prepreg paving so as to reduce wrinkles generated during hot press molding as shown in fig. 1;
5. wrapping the outer surface of the laid annular prepreg by using a separation film, sequentially winding polytetrafluoroethylene cloth and airfelt on the outer layer, adhering sealing adhesive tapes on the upper end and the bottom flange plane of the metal mold, sealing the prepreg on the surface of the metal mold by using a vacuum bag, and vacuumizing and keeping for 0.5h;
6. placing the metal mold into an autoclave, applying 1MPa pressure under the state of vacuum pumping, heating to 180 ℃ and preserving heat for 1h, naturally cooling, taking out the metal mold, and breaking vacuum to obtain a resin-based annular member blank;
7. taking down the resin-based annular member blank by using the demolding ring in the figure 1, carbonizing at 900 ℃ under the protection of argon atmosphere, wherein the heating rate is 0.5 ℃/min below 650 ℃,1 ℃/min above 650 ℃, and cooling along with a furnace after heat preservation for 1 hour to obtain a carbonized annular member porous blank;
8. assembling the carbonized porous blank body with BN tool shown in figure 2, and forming a porous blank on the outer wall of the porous blankCoating an infiltration agent prepared from silicon powder and 5% polyvinyl alcohol aqueous solution according to a mass ratio of 8:1, drying and fixing the infiltration agent on the surface of a porous green body, wherein the mass ratio of the infiltration agent to the porous green body is 2.5:1, placing the tool and the green body into an infiltration furnace, heating to 1550 ℃ in a vacuum state, preserving heat for 30min, and taking down C after natural cooling f SiC annular blank;
9. taking the inner molded surface of the blank as a reference, removing the upper and lower redundant parts of the blank in the height direction by laser cutting to obtain the final C f An annular member of SiC composite material.
10. The C obtained f The microscopic morphology of the SiC annular member after dissection and polishing is shown as figure 3, in figure 3, the black part is a continuous carbon fiber bundle, the gray part is a ceramic matrix, and the density of the material reaches 2.35g/cm 3 The porosity is only 0.5%, and the material has high mechanical strength, and the tensile strength at room temperature reaches 215MPa.
Example 2
SiC with inner diameter of 250mm, wall thickness of 4mm and height of 23.5mm f The preparation method of the SiC composite annular member comprises the following steps:
1. selecting a domestic third-generation SiC fiber unidirectional cloth, clamping two sides by a porous flat plate tool made of graphite, suspending in a vapor deposition furnace through a carbon rope, introducing propane and hydrogen at 1050 ℃ for deposition for 10 hours, and cooling along with furnace cooling;
2. loading the SiC fiber unidirectional cloth after PyC deposition into a SiC deposition furnace by adopting the method in the step 1, introducing trichloromethylsilane gas and hydrogen at 1050 ℃, preserving heat for 10 hours, and cooling along with the furnace;
3. mixing thermosetting phenolic resin, siC particles and absolute ethyl alcohol according to the mass ratio of 2:6:2, ball milling for 24 hours to prepare slurry, uniformly coating the slurry on SiC fiber unidirectional cloth formed by a deposition composite interface, and carrying out ventilation drying for 4 hours to obtain SiC fiber prepreg for standby;
4. manufacturing a metal mold by using P20 steel, wherein the outer diameter of the mold is 249mm, adhering release paper with the thickness of 0.5mm to a paving area on the surface of the mold, cutting the carbon fiber prepreg into a long rectangular shape, calculating the width and length of the rectangle according to the height and the perimeter of a component, adding 10mm machining allowance in the height direction, sequentially paving the metal mold on the surface of the metal mold according to the 0 degree/90 degree (circumference/height) direction until reaching the preset thickness, and reserving a gap with the thickness of 2mm at a joint when paying attention to 90 degree prepreg paving so as to reduce wrinkles generated during hot press molding;
5. wrapping the outer surface of the laid annular prepreg by using a separation film, sequentially winding polytetrafluoroethylene cloth and airfelt on the outer layer, adhering sealing adhesive tapes on the upper end and the bottom flange plane of the metal mold, sealing the prepreg on the surface of the metal mold by using a vacuum bag, and vacuumizing and keeping for 0.5h;
6. placing the metal mold into an autoclave, applying 1MPa pressure under the state of vacuum pumping, heating to 180 ℃ and preserving heat for 1h, naturally cooling, taking out the metal mold, and breaking vacuum to obtain a resin-based annular member blank;
7. taking down a resin-based annular member blank by using a demolding ring, carbonizing at 900 ℃ under the protection of argon atmosphere, wherein the heating rate is 0.5 ℃/min below 650 ℃,1 ℃/min above 650 ℃, and cooling along with a furnace after heat preservation for 1 hour to obtain a carbonized annular member porous blank;
8. coating an infiltration agent prepared from silicon powder and 5% polyvinyl alcohol aqueous solution according to a mass ratio of 8:1 on the outer wall of the porous blank, drying and fixing the infiltration agent on the surface of the porous blank, placing the tool and the blank into an infiltration furnace, heating to 1450 ℃ in a vacuum state, preserving heat for 30min, naturally cooling, and taking down SiC f SiC annular blank;
9. removing the rest part of the blank in the height direction by taking the inner molded surface of the blank as a reference through laser cutting to obtain the final SiC f An annular member of SiC composite material.
10. The SiC obtained f The density of the SiC composite material is 2.81g/cm 3 The porosity is 0.62%, and the room temperature tensile strength reaches 252MPa.
Comparative example 1
C with inner diameter of 226mm, wall thickness of 3mm and height of 35mm f The preparation method of the SiC composite annular member comprises the following steps:
selecting a carbon fiber unidirectional cloth of Japan Dongli T300-6K, adopting a PyC interface process manufacturing process similar to that of the embodiment (1), and shortening the preparation time of the SiC interface layer to 1h when different;
then preparing carbon fiber prepreg by adopting the same prepreg preparation process; then sequentially finishing the steps of paving, hot-press forming, carbonization and infiltration on the metal mold;
c obtained by the steps f The SiC annular component is obviously cracked after infiltration, and the crack penetrates through the whole height direction, because the SiC interface layer can effectively block the reaction erosion of liquid phase silicon to continuous fibers in the infiltration process, if the SiC interface layer is not present or has insufficient thickness, the continuous fibers are destroyed, the strength of the whole component is sharply reduced, the damage occurs in the cooling process, and the corrosion is carried out on C f The strength test result of the SiC material shows that the tensile strength of the material is only 48MPa.
Example 4
C with inner diameter of 226mm, wall thickness of 3mm and height of 35mm f The preparation method of the SiC composite annular member comprises the following steps:
selecting carbon fiber unidirectional cloth of Japan Toli T300-6K, and adopting the same deposition process as in the embodiment (1) to manufacture a PyC and SiC composite interface layer;
mixing thermosetting phenolic resin, siC particles and absolute ethyl alcohol according to the mass ratio of 4:2:4, ball milling for 24 hours to prepare slurry, uniformly coating the slurry on SiC fiber unidirectional cloth formed by a deposition composite interface, and carrying out ventilation drying for 4 hours to obtain carbon fiber prepreg for standby;
then sequentially finishing the steps of paving, hot-press forming, carbonization and infiltration on the metal mold according to the same technological parameters; c obtained by the steps f The density test result of the SiC annular member blank shows that the density is only 1.78g/cm 3 The porosity reaches 25%, and the room temperature tensile strength is only 110MPa.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The preparation method of the annular thin-wall component made of the ceramic matrix composite material comprises the following steps:
a) Arranging carbon fiber cloth or silicon carbide fiber in a chemical vapor deposition furnace, introducing a carbon source and hydrogen, and depositing to obtain fiber cloth deposited with pyrolytic carbon;
b) Introducing silane gas and hydrogen gas for deposition to obtain fiber cloth deposited with a silicon-carbon composite interface;
c) Coating prepreg slurry on the surface of the fiber cloth deposited with the silicon-carbon composite interface to obtain fiber prepreg;
the prepreg comprises phenolic resin, siC ceramic particles and an organic solvent;
d) Molding the fiber prepreg on the surface of a mold to obtain a resin-based annular blank;
e) Sequentially carbonizing and infiltrating the resin-based annular blank to obtain a ceramic matrix composite annular blank;
f) And performing dimension processing on the upper end face and the lower end face of the annular ceramic matrix composite blank to obtain the annular thin-wall ceramic matrix composite member.
2. The method according to claim 1, wherein the temperature of the deposition in the step a) is 900 to 1100 ℃ and the time of the deposition is 10 to 15 hours.
3. The method according to claim 1, wherein the temperature of the deposition in the step B) is 900 to 1200 ℃ and the time of the deposition is 10 to 15 hours.
4. The preparation method according to claim 1, wherein the mass ratio of the phenolic resin and the SiC ceramic particles in the prepreg slurry is (0.3 to 0.6): 1, the mass fraction of the organic solvent in the prepreg slurry is 20-40%.
5. The method of claim 4, wherein the weight of the fiber cloth deposited with the silicon-carbon composite interface is increased by 80-150% after the fiber prepreg is formed.
6. The method according to claim 1, wherein the carbonization is performed under an argon atmosphere at 800 to 1000 ℃ for 0.5 to 2 hours.
7. The preparation method according to claim 1, wherein the outer wall of the carbonized annular blank is coated with an infiltration agent for infiltration, and the infiltration agent comprises silicon powder and polyvinyl alcohol;
the mass ratio of Si powder in the infiltration agent to the carbonized annular blank is (2.5-3.5): 1.
8. the method according to claim 7, wherein the infiltration is performed under vacuum, the infiltration temperature is 1450 to 1550 ℃ and the incubation time is 20 to 40min.
9. The annular thin-walled component of ceramic matrix composite material prepared by the method of any one of claims 1-8.
10. The ceramic matrix composite annular thin-walled member of claim 9, wherein the ceramic matrix composite annular thin-walled member has a porosity of < 1%.
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