CN116375487A - Preparation method of low-porosity SiC fiber unidirectional prepreg tape - Google Patents
Preparation method of low-porosity SiC fiber unidirectional prepreg tape Download PDFInfo
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- CN116375487A CN116375487A CN202310361570.2A CN202310361570A CN116375487A CN 116375487 A CN116375487 A CN 116375487A CN 202310361570 A CN202310361570 A CN 202310361570A CN 116375487 A CN116375487 A CN 116375487A
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 62
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
The invention discloses a preparation method of a low-porosity SiC fiber unidirectional prepreg tape, which aims at solving the technical problem of how to reduce the porosity of the unidirectional prepreg tape, and adopts the technical scheme that: preparing a composite coating on the surface of continuous SiC fibers, unwinding the composite coating onto a material tray to obtain unwinding wires, sealing the unwinding wires and the material tray, placing the material tray in an autoclave, introducing ceramic slurry, applying pressure and maintaining pressure to obtain the leached fibers, winding the leached fibers on a winding roller, drying to obtain SiC fiber unidirectional prepreg tapes with uniform slurry distribution and low porosity, laminating, and forming, and curing in an autoclave, carbonizing at high temperature and vacuum melting and siliconizing to obtain the MI-SiC/SiC ceramic matrix composite. According to the invention, through the process of vacuumizing and pressurizing at the stage of dipping the SiC bundle filaments with the surface coating into the slurry, air in the fibers and bubbles in the slurry are removed, so that the slurry fully permeates into the fiber bundles, and the density and the slurry distribution uniformity of the SiC fiber unidirectional prepreg tape can be remarkably improved.
Description
Technical Field
The invention belongs to the technical field of preparation of ceramic matrix composite materials, and particularly relates to a preparation method of a low-porosity SiC fiber unidirectional prepreg tape.
Background
The continuous fiber reinforced ceramic matrix composite has the outstanding advantages of high temperature resistance, high specific strength and high specific modulus, has fracture characteristics similar to those of metal, and has high reliability, thus formingThe material is an urgent material for novel aerospace device hot junction components and nuclear industry radiation-resistant componentsSand building army, auspicious instead of Zhang Zhaofu, fiber-toughened high-temperature ceramic matrix composite (Cf, siC/SiC) should With research progress, aeronautical manufacturing technology, 2017)。
The continuous silicon carbide fiber reinforced silicon carbide ceramic matrix composite (SiC/SiC) is one of the structural materials with the most excellent high temperature resistance at present. The preparation method of the material mainly comprises the following steps ofLiu Hu, yang Jinhua, jiao Jian, aircraft engine coupling Continuous SiC/SiC composite material preparation process and application prospect, and aviation systemManufacturing technique, 2017): chemical vapor infiltration (ChemicalVaporInfiltration, CVI), melt infiltration (MeltInfiltration, MI), nano-infiltration transient eutectic (Nano-InfiltrationandTransientEutectic, NITE), sol-Gel (Sol-Gel), precursor impregnation cracking (PrecursorImpregnationandPyrolysis, PIP), CVI+PIP and NITE+PIP.
Among these technologies, the SiC/SiC composite material (MI-SiC/SiC) prepared by the MI process has the performance advantages of low porosity, high thermal conductivity, high interlaminar shear strength, etc., and the process has the outstanding advantages of short preparation period and low cost, so that it has been applied to manufacture of aero-engines and industrial gas turbine hot end components abroad.
The universal electric (GE) company in the United states developed a unidirectional Prepreg tape-infiltration (Prepreg-MI) process and developed to
Is a brand MI-SiC/SiC composite material product which has been successfully applied to turbine outer rings, combustion chambers and other hot junction components of aeroengines and industrial gas turbinesDong Shaoming, hu Jianbao, zhang Xiangyu, siC/SiC composite MI process Preparation technique, aeronautical manufacturing technique, 2014,6). The unidirectional prepreg tape-MI process mainly comprises the following steps: (1) Firstly, preparing an interface layer on the surface of SiC fiber by adopting a Chemical Vapor Deposition (CVD) technology; (2) Mixing SiC powder, carbon powder, resin binder, surfactant and solvent to obtain ceramic slurry, immersing the slurry into coated SiC fiber bundles, and wet winding to obtain the final productSiC fiber unidirectional prepreg tape; (3) Forming a composite material preform after the unidirectional prepreg layers are stacked, and then curing to realize shaping; (4) Carbonizing the resin by pyrolysis, and discharging other organic components in a gaseous state to form a preform with a large number of micropores, so as to provide a channel for subsequent siliconizing; (5) And finally, heating the silicon powder or the silicon block to a molten state (higher than 1410 ℃), and allowing liquid silicon to infiltrate into the porous fiber preform under the action of capillary force, so that silicon carbide is generated by the reaction of silicon and carbon, and the compact MI-SiC/SiC composite material is prepared.
In the MI process, molten silicon enters the matrix under the action of capillary force, and the liquid silicon reacts with carbon in the preform to generate SiC. The reaction formula is as follows:
Si(l)+C(s)＝SiC(s)
after cooling, the MI-SiC/SiC matrix consists of SiC powder added into the preform, siC generated by the reaction of molten silicon and carbon, and a small amount of residual silicon (about 5%), and the matrix also contains 2% -5% of pores.
MI-SiC/SiC is mainly used in a high-temperature oxidation service environment, and the porosity is required to be as low as possible. The pores can obviously reduce the strength, elastic modulus and heat conductivity of the composite material, and can seriously damage the high-temperature oxidation resistance of the composite material, and even provide diffusion channels for the oxidizing atmosphere to reach the inside of the composite material, so that the inside of the composite material is oxidized, brittle fracture is generated, and the service reliability is seriously reduced.
One of the main sources of voids in MI-SiC/SiC composites is that the ceramic slurry cannot be fully immersed in the fiber bundles when preparing SiC fiber unidirectional prepreg tapes (typical commercial continuous SiC fiber specifications are 500 filaments per bundle, each filament diameter being about 15 μm), thereby forming voids. The pores will partially heal during the subsequent autoclave densification process, but are difficult to completely eliminate. In the case of melt siliconizing, the capillary force is low at the site containing larger pores, and the filling is not easy, resulting in residual pores in the final MI-SiC/SiC composite material.
When MI-SiC/SiC is prepared by adopting the technical route of GE company in the United states, siC fiber tows with a coating are continuously passed through a slurry tank under normal pressure, the slurry is permeated into the SiC fiber tows, and then single-layer arrangement is carried out on a winding roller to form a unidirectional prepreg tape.
Because of the high viscosity of the ceramic slurry, small gaps among monofilaments in the SiC fiber bundle filaments, short time (1-5 seconds) for the SiC fiber bundle filaments to pass through the slurry tank, bubbles in the slurry and other factors, the slurry often cannot completely infiltrate into the SiC fiber bundle filaments, and the dried unidirectional prepreg tape contains a certain amount of pores. How to reduce the porosity of unidirectional prepreg tapes is one of the key techniques for preparing high quality MI-SiC/SiC composites.
Disclosure of Invention
The invention aims to provide a preparation method of a low-porosity SiC fiber unidirectional prepreg tape, which aims to solve the technical problems.
The invention aims to solve the technical problems, and is realized by adopting the following technical scheme:
a preparation method of a low-porosity SiC fiber unidirectional prepreg tape comprises the following steps:
1) Preparing a composite coating on the surface of the continuous SiC fiber to obtain a coated continuous fiber A;
2) Unwinding the material A onto a material tray to obtain a rewinding wire B;
3) Placing the B and the material tray into an autoclave, sealing, vacuumizing the autoclave, introducing ceramic slurry into the autoclave, completely covering the fiber on the liquid level, and finally applying pressure in the autoclave and maintaining the pressure to obtain a fiber C immersed with the slurry;
4) Taking out the C from the autoclave, winding the continuous fibers fully immersed in the ceramic slurry on a winding roller in a single layer in a wet state, and drying to obtain a SiC fiber unidirectional prepreg tape D with uniform slurry distribution and low porosity;
5) And (3) stacking and forming the D, and sequentially carrying out autoclave curing, high-temperature carbonization under inert atmosphere and vacuum melting siliconizing to obtain the MI-SiC/SiC ceramic matrix composite E.
Preferably, the composite coating in the step 1) is a BN coating and Si coating from the surface layer of the fiber to the outside 3 N 4 The coating and the C coating are prepared by adopting a chemical vapor deposition method.
Preferably, the BN is coatedThe thickness of the layer is 200nm-600nm, the Si 3 N 4 The thickness of the coating is 100nm-500nm, and the thickness of the C coating is 5nm-50nm.
Preferably, the ceramic slurry in the step 3) comprises silicon carbide powder, carbon powder, a resin binder, a dispersing agent and a solvent, wherein the vacuumizing pressure in the autoclave is-0.1 MPa, the pressurizing pressure range is 3MPa-6MPa, and the pressure is maintained for 10min.
Preferably, the solid content of the ceramic slurry is 20% -50%, the granularity of the silicon carbide powder is 0.5-5 μm, the granularity of the carbon powder is 0.1-5 μm, and the resin binder is any one of epoxy resin, phenolic resin or furfural resin.
Preferably, the single piece thickness of the SiC fiber unidirectional prepreg tape D in the step 4) is 0.2mm-0.6mm.
Preferably, the curing pressure of the autoclave in the step 5) is 0.5MPa to 2MPa; the temperature is 80-150 ℃ and the heat preservation time is 0.5-10 h; high-temperature carbonization is carried out in any inert atmosphere, the temperature is 900-1300 ℃, and the heat preservation time is 0.5-5 h; the melt siliconizing temperature is 1410-1450 ℃, and the siliconizing time is 1-60 min.
The beneficial effects of the invention are as follows:
1. according to the invention, through a process of vacuumizing and pressurizing at the stage of dipping the SiC bundle filaments with the surface coating into the slurry, air in the fibers and bubbles in the slurry are removed, so that the slurry fully permeates into the fiber bundles, and the density and the slurry distribution uniformity of the SiC fiber unidirectional prepreg tape can be remarkably improved;
2. the unidirectional prepreg tape can remarkably improve the performance consistency of the MI-SiC/SiC composite material, thereby improving the service reliability of MI-SiC/SiC components;
3. the invention has simple process and low cost, is suitable for mass production, and has the value of engineering application.
Drawings
FIG. 1 is a schematic view of coated fiber unwinding to a tray;
wherein: 1-fiber drum, 2-spinneret of unwinding system, 3-tray.
Detailed Description
In order that the manner in which the above recited features, objects and advantages of the present invention are obtained, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings. Based on the examples in the embodiments, those skilled in the art can obtain other examples without making any inventive effort, which fall within the scope of the invention.
Specific embodiments of the present invention are described below with reference to the accompanying drawings.
Example 1
A preparation method of a low-porosity SiC fiber unidirectional prepreg tape comprises the following steps:
1) Preparing a 400nm thick BN interface layer on the surface of the continuous SiC fiber by using a CVD method, wherein the BN layer plays roles of load transfer, crack deflection, fiber debonding and the like in the composite material, and preparing Si on the surface of the BN interface layer 3 N 4 The coating is used for resisting corrosion damage of liquid silicon to the BN coating and the SiC fibers during melt siliconizing; finally at Si 3 N 4 Preparing a pyrolytic carbon boundary layer with the thickness of 30nm on the surface of the coating to promote liquid silicon to infiltrate into the preform, so as to obtain continuous SiC fiber A with the composite coating;
2) Unwinding the coated continuous SiC fibers A into a stainless steel material tray to obtain recoil filaments B; close packing of the fiber bundles should be avoided during unwinding to affect subsequent slurry penetration.
3) Placing the recoil wire B and a material tray into an autoclave, sealing, vacuumizing the autoclave to-0.1 MPa, introducing ceramic slurry containing silicon carbide powder, carbon powder, resin binder, dispersing agent and solvent into the autoclave, completely covering the fiber by the liquid level, and finally applying pressure to 3MPa in the autoclave and maintaining the pressure for 10min to obtain a leached fiber C;
the ceramic slurry contains 25wt.% of SiC powder, and the particle size (D50) is 0.8 μm;10wt.% of C powder having a particle size (D50) of 0.1 μm;12wt.% of a phenolic resin and a curing agent; 3wt.% of dispersant Polyethylenimine (PEI); the solvent is absolute ethyl alcohol.
4) Taking out the C from the autoclave, winding the continuous fibers fully impregnated with the ceramic slurry on a winding roller with the diameter of 400mm and the length of 600mm in a single layer in a wet state, and drying to obtain a SiC fiber unidirectional prepreg tape D with the length of 1256mm, the width of 500mm and the thickness of 0.3mm, wherein the slurry is uniformly distributed and the porosity is low;
5) Cutting the D into sheets with the thickness of 200mm multiplied by 200mm, and stacking eight sheets of the D to form a prefabricated body, wherein the arrangement directions of fibers between two adjacent layers of the D are mutually perpendicular; sealing the preform with a vacuum bag, continuously vacuumizing the interior, curing in an autoclave under the conditions of a curing pressure of 1.2MPa, a curing temperature of 130 ℃ and a curing time of 2 hours to obtain a cured preform, wherein the dimensions of the preform are 200mm multiplied by 2.8mm, and the cured preform is subjected to N 2 Heat treatment is carried out for 1h at 1100 ℃ in the atmosphere to obtain a carbonized preform, in the process, the carbon-based resin adhesive is carbonized at high temperature, gas byproducts are removed, a large number of holes are introduced into a matrix, and a passage is provided for subsequent melt siliconizing; finally, melting and siliconizing at 1440 ℃ under 10Pa vacuum, preserving heat for 30min, cooling to room temperature along with a furnace, penetrating into the preform under the action of capillary force after silicon is melted at high temperature, reacting with carbon in the preform layer to generate SiC, and filling a small amount of rest gaps with liquid silicon to obtain the MI-SiC/SiC composite material.
The thickness of the BN coating can also be any value between 200nm and 600nm, and the Si 3 N 4 The thickness of the coating may also be any value between 100nm and 500nm, and the thickness of the C coating may also be any value between 5nm and 50nm.
The pressurizing pressure in step 3) may also be in any value between 2MPa and 10 MPa.
The solid content of the ceramic slurry can be any value between 20 and 50 percent, the granularity of the silicon carbide powder can be any value between 0.5 and 5 mu m, the granularity of the carbon powder can be any value between 0.1 and 5 mu m, and the resin binder is any one of epoxy resin, phenolic resin or furfural resin.
The single sheet thickness of the SiC fiber unidirectional prepreg tape D in the step 4) may also be any value between 0.2mm and 0.6mm.
The curing pressure of the autoclave in the step 5) is any value between 0.5MPa and 2MPa, the temperature is any value between 80 ℃ and 150 ℃, the heat preservation time is any value between 0.5h and 10h, the high-temperature carbonization is carried out in any inert atmosphere, the temperature is any value between 900 ℃ and 1300 ℃, the heat preservation time is any value between 0.5h and 5h, the temperature of the melt siliconizing is any value between 1410 ℃ and 1450 ℃, and the siliconizing time is any value between 1min and 60min.
The MI-SiC/SiC composite material obtained in the embodiment has the porosity of 1.8%, the volume fraction of SiC fibers of 24%, the tensile strength of the composite material of 351MPa and the fracture strain of 0.62%, and has excellent mechanical properties.
Example 2
1) Step 1) as in example 1;
2) Step 2) of example 1;
3) Placing the B and the material tray into an autoclave, sealing, vacuumizing the autoclave to-0.1 MPa, and introducing ceramic slurry containing SiC powder and C powder into the autoclave, wherein the liquid surface completely covers the fibers; applying pressure to the kettle to 6MPa by utilizing an air compressor, and maintaining the pressure for 10min to obtain leached fiber C, wherein the slurry formula is the same as that in step 3 of the embodiment 1;
4) Step 4) of example 1;
5) As in step 5 of example 1).
The MI-SiC/SiC composite material obtained in the embodiment has the porosity of 0.9%, the volume fraction of SiC fibers of 24%, the tensile strength of the composite material of 360MPa and the fracture strain of 0.71%, and has excellent mechanical properties.
The lower porosity of the composite compared to the results of example 1 suggests that increasing the impregnation pressure facilitates uniform impregnation of the slurry in the fiber preform, and ultimately improves the mechanical properties of the composite.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are only preferred embodiments of the present invention, and are not intended to limit the invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The preparation method of the low-porosity SiC fiber unidirectional prepreg tape is characterized by comprising the following steps of:
1) Preparing a composite coating on the surface of the continuous SiC fiber to obtain a coated continuous fiber A;
2) Unwinding the material A onto a material tray to obtain a rewinding wire B;
3) Placing the B and the material tray into an autoclave, sealing, vacuumizing the autoclave, introducing ceramic slurry into the autoclave, completely covering the fiber on the liquid level, and finally applying pressure in the autoclave and maintaining the pressure to obtain a fiber C immersed with the slurry;
4) Taking out the C from the autoclave, winding the continuous fibers fully immersed in the ceramic slurry on a winding roller in a single layer in a wet state, and drying to obtain a SiC fiber unidirectional prepreg tape D with uniform slurry distribution and low porosity;
5) And (3) stacking and forming the D, and sequentially carrying out autoclave curing, high-temperature carbonization under inert atmosphere and vacuum melting siliconizing to obtain the MI-SiC/SiC ceramic matrix composite E.
2. The method for preparing the unidirectional prepreg tape with the low-porosity SiC fibers according to claim 1, wherein the composite coating in the step 1) is a BN coating and Si coating from the surface layer of the fibers 3 N 4 The coating and the C coating are prepared by adopting a chemical vapor deposition method.
3. The method for preparing a unidirectional prepreg tape of low porosity SiC fiber according to claim 2, wherein the BN coating has a thickness of 200nm to 600nm, and the Si is 3 N 4 The thickness of the coating is 100nm-500nm, and the thickness of the C coating is 5nm-50nm。
4. The method for preparing the unidirectional prepreg tape with the low porosity SiC fibers according to claim 1, wherein the ceramic slurry in the step 3) comprises silicon carbide powder, carbon powder, a resin binder, a dispersing agent and a solvent, wherein the pressure of vacuumizing in the autoclave is-0.1 MPa, the pressurizing pressure is in the range of 3MPa-6MPa, and the pressure is maintained for 10min.
5. The method for preparing the unidirectional prepreg tape with the low porosity SiC fibers according to claim 4, wherein the solid content of the ceramic slurry is 20% -50%, the granularity of the silicon carbide powder is 0.5-5 μm, the granularity of the carbon powder is 0.1-5 μm, and the resin binder is any one of epoxy resin, phenolic resin or furfural resin.
6. The method for preparing the unidirectional prepreg tape of SiC fiber with low porosity according to claim 1, wherein the single piece thickness of the unidirectional prepreg tape D of SiC fiber in the step 4) is 0.2mm to 0.6mm.
7. The method for preparing the unidirectional prepreg tape of low-porosity SiC fiber according to claim 1, wherein the curing pressure of the autoclave in step 5) is 0.5MPa to 2MPa; the temperature is 80-150 ℃ and the heat preservation time is 0.5-10 h; high-temperature carbonization is carried out in any inert atmosphere, the temperature is 900-1300 ℃, and the heat preservation time is 0.5-5 h; the melt siliconizing temperature is 1410-1450 ℃, and the siliconizing time is 1-60 min.
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