CN110317073B - Preparation method of multi-stage fiber synergistic toughened antioxidant ceramic matrix composite material - Google Patents
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Abstract
The invention relates to a preparation method of a multilevel fiber synergistically toughened antioxidant ceramic matrix composite, which comprises the steps of mixing a micro-nano scale reinforcement into precursor slurry to prepare mixed slurry, brushing the mixed slurry on the surface of a fiber containing an interface layer to obtain a multilevel fiber prepreg, cutting, paving and hot-pressing the prepreg to prepare a prefabricated body, treating the prefabricated body at high temperature to obtain a porous body, circularly dipping and carbonizing the porous body in precursor resin containing antioxidant components to obtain a semi-densified multilevel toughened prefabricated body, and then densifying by adopting a infiltration process to obtain the multilevel fiber synergistically toughened ceramic matrix composite, wherein the antioxidant property and the toughness of the multilevel fiber synergistically toughened ceramic matrix composite are obviously improved.
Description
Technical Field
The invention relates to a preparation method of a multistage fiber synergistic toughening antioxidant ceramic matrix composite, belonging to the preparation technology of fiber toughening ceramic matrix composites.
Background
The continuous fiber reinforced ceramic matrix composite has the defects of large brittleness, insufficient damage toughness and short fatigue life due to holes, cracks and the like formed in a matrix in the high-temperature use process, and is difficult to meet the requirement of the fatigue performance of the next generation engine material. Therefore, in the current stage, research attempts are made to develop a ceramic matrix composite material with higher high temperature resistance and higher damage tolerance by adopting technical approaches such as nanofiber multistage toughening and the like.
The nano-fiber is introduced into a brittle matrix between fiber layers and between bundles as a second reinforcement, and can increase the crack propagation distance, improve the brittleness of a micro-zone matrix, improve the reinforcing effect of a reinforcing phase in a multi-scale manner, improve the oxidation resistance, the mechanical property and the like of the ceramic matrix composite material through toughening mechanisms such as crack deflection, bridging and the like, so that the nano-reinforcement is also often applied to the performance optimization of the ceramic matrix composite material. In the prior art, a ball milling mixing method is adopted to introduce a micro-nano scale reinforcement into a matrix slurry, and a hot isostatic pressing sintering method and other methods are adopted to form a ceramic matrix composite material, so that the toughening and reinforcing effects of the nano reinforcement are realized; meanwhile, a layer of carbon is provided on the surface of the whisker, so that the chemical bonding of the whisker and the ceramic composite material is inhibited, and the toughening and reinforcing effects of the nano reinforcement are further improved.
Meanwhile, in order to improve the oxidation resistance of the ceramic matrix composite material and prevent the oxidation component from damaging fibers through channels such as cracks, pores and the like formed in the high-temperature use process, in part of researches, the SiBCN, boron powder and the like are introduced into the ceramic matrix composite material, B, N components are formed in the SiC matrix in a high-temperature environment, a compact oxide film is formed on the surface of the composite material, oxygen permeation and oxidation reaction are inhibited, and the high-temperature oxidation resistance of the ceramic matrix composite material is improved.
The invention content is as follows:
the invention provides a preparation method of a multi-stage fiber synergistic toughening antioxidant ceramic matrix composite, which is characterized in that the toughness of the ceramic matrix composite is improved by introducing a multi-stage reinforcement, the antioxidation of the ceramic matrix composite is improved by introducing an antioxidant component, the introduction of a nano reinforcement is protected by designing a technological process, the introduction of one or more antioxidant components is realized by different impregnation processes, and finally, the rapid densification is realized by a infiltration process.
The purpose of the invention is realized by the following technical approaches:
the preparation method of the multi-stage fiber synergistic toughening antioxidant ceramic matrix composite material comprises the following steps:
step one, preparing mixed slurry
Uniformly mixing high-carbon-residue resin, a micro-nano-scale reinforcement and absolute ethyl alcohol according to a mass ratio of 5-10: 1: 10-20, and uniformly mixing by adopting an ultrasonic and mechanical stirring method to obtain mixed slurry for later use;
step two, preparing an interface layer on the surface of the continuous fiber fabric
The type of the interface layer is a composite interface layer of one or more of pyrolytic carbon (PyC), Boron Nitride (BN) or silicon carbide (SiC);
step three, preparation of prepreg
Introducing the mixed slurry prepared in the step one into the continuous fiber fabric after the step two is finished through a wet prepreg preparation process to obtain a prepreg;
step four, preparation of multi-stage fiber synergistic toughening preform
Placing the prepreg in the third step into a hot-press forming die for forming, wherein the hot-press forming temperature is 150-400 ℃, the forming pressure is about 1-5 MPa, the pressure maintaining time is about 1-5 h, and after the pressure maintaining is finished, a preform with the multi-stage fibers toughened in a synergistic manner is obtained;
step five, preparation of multi-stage fiber synergistic toughening porous body
Putting the prefabricated body synergistically toughened by the multilevel fibers obtained in the fourth step into a high-temperature furnace, and heating to over 1000 ℃ to obtain a porous body synergistically toughened by the multilevel fibers;
step six, precursor resin impregnation
Putting the multi-stage fiber synergistic toughening porous body into a vacuum impregnation box, vacuumizing the impregnation box by using a vacuum pump, then injecting precursor resin into the impregnation box, and soaking for 3-5 hours after the multi-stage fiber synergistic toughening porous body is completely immersed in a precursor solution;
seventhly, putting the soaked multi-stage fiber synergistic toughened porous body into a high-temperature furnace, and heating to over 1000 ℃ to obtain a preliminarily densified multi-stage fiber synergistic toughened porous body;
step eight, infiltration densification
And putting the preliminarily densified multi-stage fiber synergistic toughening porous body into a graphite crucible, and preparing the multi-stage fiber synergistic toughening antioxidant ceramic matrix composite material by adopting a melting siliconizing mode.
In one implementation, the mixing time of the ultrasonic and mechanical stirring in the step one is 1-5 hours.
In one embodiment, the thickness of the single-layer interface layer in the second step is 100 to 500nm, and the total thickness of the interface layer is about 1 to 2 μm.
In one implementation, the introduction in step three is performed by a method of multiple brushing, and then the prepreg is dried for 5-30 hours at room temperature.
In one implementation, the fibers forming the continuous fiber fabric are carbon fibers or silicon carbide fibers.
In one implementation, the high carbon residue resin is one or a mixture of phenolic resin, furan resin or polyimide resin.
In one implementation, the micro-nano-scale reinforcement is one or a mixture of several of nano-silicon carbide fibers, nano-silicon carbide whiskers and chopped carbon fibers.
In one implementation, the precursor resin is one or a mixture of two of a silicon boron carbon nitrogen precursor and a boron nitride precursor.
In one implementation, the operations of step six and step seven are repeated before step eight is performed.
In one implementation, the process temperature for melt siliconizing is 1400-1800 ℃.
The technical scheme of the invention has the following advantages and characteristics:
1. according to the method, the nano reinforcement is dispersed in the high-carbon-residue resin to prepare the mixed slurry, and the mixed slurry is used for preparing the prepreg;
2. according to the invention, the precursor is introduced into the porous body after hot-pressing carbonization for impregnation, and the oxidation-resistant base layer is formed on the surface of the pyrolytic carbon layer of the nano reinforcement to protect the multi-stage reinforcement, and the oxidation-resistant base layer is cracked at high temperature to form a self-healing phase, so that the oxidation resistance of the ceramic matrix composite is improved;
3. according to the method for impregnating and cracking the precursor after the hot-pressing carbonization, one or more precursor components can be respectively introduced through different steps, and the introduction content of each component can be effectively controlled;
4. the final densification process in the invention adopts a melt siliconizing process, so that the porosity of the final molding material is reduced, and the densification efficiency is effectively improved.
Detailed Description
Example 1
The preparation method of the multi-stage fiber synergistic toughening antioxidant ceramic matrix composite material comprises the following steps:
uniformly mixing phenolic resin, silicon carbide whiskers and absolute ethyl alcohol according to a mass ratio of 5:1:15, and mixing for 2 hours in an ultrasonic and mechanical stirring manner to obtain slurry for later use;
step two, depositing an interface layer on the surface of the continuous fiber, wherein the combination mode of the interface layer is a composite interface layer of pyrolytic carbon (PyC)/Boron Nitride (BN)/silicon carbide (SiC), the thickness of the pyrolytic carbon (PyC) interface is about 100nm, the thickness of the Boron Nitride (BN) interface is 400nm, and the thickness of the silicon carbide (SiC) interface is 500 nm;
and step three, introducing the prepared slurry into the fibers prepared in the step two through a wet preparation process to prepare the prepreg. The slurry introduction amount is strictly controlled in the brushing process, the uniformity of slurry distribution in the prepreg is ensured by adopting a method of multiple brushing, and then the prepreg is dried for 12 hours at room temperature to obtain the multilevel fiber prepreg;
cutting the multistage fiber prepreg prepared in the step three according to a target size, and paving; and placing the laid prepreg into a hot-pressing forming die for hot-pressing forming. The hot press molding temperature is 160 ℃, the molding pressure is about 3MPa, the pressure maintaining time is about 3h, and the multistage fiber synergistic toughening preform is prepared after the pressure maintaining is finished;
and step five, placing the resin-based preform prepared in the step four into a high-temperature furnace for high-temperature heat treatment to obtain a porous body synergistically toughened by the multilevel fibers, wherein the maximum temperature of the porous body preparation is 1000 ℃.
Putting the porous body prepared in the fifth step into a vacuum impregnation box, vacuumizing the impregnation box by using a vacuum pump, then injecting a silicon-boron-carbon-nitrogen precursor into the impregnation box, and soaking for 4 hours after the precursor solution completely immerses the sample;
and step seven, placing the sample soaked in the step six into a high-temperature furnace for high-temperature heat treatment to obtain a porous body, wherein the maximum temperature for preparing the porous body is about 1200 ℃.
Step eight, repeating the step six and the step seven 1 times, and performing preliminary densification on the prepared sample;
and step nine, placing the semi-densified sample prepared in the step eight into a graphite crucible, and obtaining the multi-stage fiber synergistically toughened antioxidant ceramic matrix composite material by adopting a melting siliconizing mode, wherein the high-temperature melting siliconizing process temperature is about 1460 ℃.
The multi-stage fiber synergistic toughened antioxidant ceramic matrix composite can be effectively prepared by the process, the preparation efficiency is obviously higher than that of a precursor impregnation cracking process, and the material density can reach 2.7g/cm3The bending strength, tensile strength, fracture toughness and oxidation resistance of the steel are obviously improved.
Example 2
The preparation method of the multi-stage fiber synergistic toughening antioxidant ceramic matrix composite material comprises the following steps:
uniformly mixing furan resin, silicon carbide whiskers and absolute ethyl alcohol according to the mass ratio of 10:1:20, and mixing for 5 hours in an ultrasonic and mechanical stirring manner to obtain slurry for later use;
step two, depositing an interface layer on the surface of the continuous fiber, wherein the combination mode of the interface layer comprises the combination of composite interface layers such as pyrolytic carbon (PyC)/Boron Nitride (BN)/silicon carbide (SiC)/pyrolytic carbon (PyC), and the like, the thickness of a single-layer interface layer is about 300nm, and the total thickness of the interface layer is about 1.2 mu m;
and step three, introducing the prepared slurry into the fibers prepared in the step two through a wet prepreg preparation process to prepare the prepreg. The slurry introduction amount is strictly controlled in the brushing process, the uniformity of slurry distribution in the prepreg is ensured by adopting a method of multiple brushing, and then the prepreg is dried for 20 hours at room temperature to obtain the multilevel fiber prepreg;
cutting the multistage fiber prepreg prepared in the step three according to a target size, and paving; and placing the laid prepreg into a hot-pressing forming die for hot-pressing forming. The hot-press molding temperature is 200 ℃, the molding pressure is about 3MPa, the pressure maintaining time is about 3h, and a multi-level fiber synergistically toughened preform is prepared after the pressure maintaining is finished;
and step five, placing the resin-based preform prepared in the step four into a high-temperature furnace for high-temperature heat treatment to obtain a porous body synergistically toughened by the multilevel fibers, wherein the maximum temperature of the porous body preparation is 1000 ℃.
Putting the porous body prepared in the fifth step into a vacuum impregnation box, vacuumizing the impregnation box by using a vacuum pump, then injecting a boron nitride precursor into the impregnation box, and soaking for 5 hours after the precursor solution completely immerses the sample;
seventhly, putting the sample soaked in the step six into a high-temperature furnace for carbonization, and putting the sample into the high-temperature furnace for high-temperature heat treatment to obtain a porous body; the maximum temperature for porous body preparation was about 1200 ℃.
Step eight, repeating the step six and the step seven for 2 times, and performing preliminary densification on the prepared sample;
and step nine, placing the semi-densified sample prepared in the step eight into a graphite crucible, and obtaining the multi-stage fiber synergistically toughened antioxidant ceramic matrix composite material by adopting a high-temperature melting siliconizing mode, wherein the high-temperature melting siliconizing process temperature is about 1460 ℃.
Claims (7)
1. A preparation method of a multi-level fiber synergistic toughening antioxidant ceramic matrix composite material is characterized by comprising the following steps: the method comprises the following steps:
step one, preparing mixed slurry
Uniformly mixing high-carbon-residue resin, a micro-nano-scale reinforcement and absolute ethyl alcohol according to a mass ratio of 5-10: 1: 10-20, and uniformly mixing by adopting an ultrasonic and mechanical stirring method to obtain mixed slurry for later use;
the high-carbon-residue resin is one or a mixture of more of phenolic resin, furan resin or polyimide resin;
the micro-nano scale reinforcement is one or a mixture of several of nano silicon carbide fiber, nano silicon carbide whisker and chopped carbon fiber;
step two, preparing an interface layer on the surface of the continuous fiber fabric
The type of the interface layer is one or more of pyrolytic carbon (PyC), Boron Nitride (BN) or silicon carbide (SiC);
step three, preparation of prepreg
Introducing the mixed slurry prepared in the step one into the continuous fiber fabric after the step two is finished through a wet prepreg preparation process to obtain a prepreg;
step four, preparation of multi-stage fiber synergistic toughening preform
Placing the prepreg in the third step into a hot-press forming die for forming, wherein the hot-press forming temperature is 150-400 ℃, the forming pressure is 1-5 MPa, the pressure maintaining time is 1-5 h, and after the pressure maintaining is finished, obtaining a prefabricated body with the multi-stage fibers toughened in a synergistic manner;
step five, preparation of multi-stage fiber synergistic toughening porous body
Putting the prefabricated body synergistically toughened by the multilevel fibers obtained in the fourth step into a high-temperature furnace, and heating to over 1000 ℃ to obtain a porous body synergistically toughened by the multilevel fibers;
step six, precursor resin impregnation
Putting the multi-stage fiber synergistic toughening porous body into a vacuum impregnation box, vacuumizing the impregnation box by using a vacuum pump, then injecting precursor resin into the impregnation box, and soaking for 3-5 hours after the multi-stage fiber synergistic toughening porous body is completely immersed in a precursor solution;
the precursor resin is one or a mixture of two of a silicon-boron-carbon-nitrogen precursor and a boron nitride precursor;
seventhly, putting the soaked multi-stage fiber synergistic toughened porous body into a high-temperature furnace, and heating to over 1000 ℃ to obtain a preliminarily densified multi-stage fiber synergistic toughened porous body;
step eight, infiltration densification
And putting the preliminarily densified multi-stage fiber synergistic toughening porous body into a graphite crucible, and preparing the multi-stage fiber synergistic toughening antioxidant ceramic matrix composite material by adopting a melting siliconizing mode.
2. The method for preparing the multi-stage fiber synergistic toughened antioxidant ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: and in the step one, the mixing time of the ultrasonic and mechanical stirring is 1-5 hours.
3. The method for preparing the multi-stage fiber synergistic toughened antioxidant ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: in the second step, the single-layer thickness of the interface layer is 100-500 nm, and the total thickness of the interface layer is 1-2 μm.
4. The method for preparing the multi-stage fiber synergistic toughened antioxidant ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the introduction in the third step is to use a method of brushing for multiple times, and then the prepreg is dried for 5-30 hours at room temperature.
5. The method for preparing the multi-stage fiber synergistic toughened antioxidant ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the fibers of the formed continuous fiber fabric are carbon fibers or silicon carbide fibers.
6. The method for preparing the multi-stage fiber synergistic toughened antioxidant ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: and before the step eight is carried out, repeating the operations of the step six and the step seven.
7. The method for preparing the multi-stage fiber synergistic toughened antioxidant ceramic matrix composite material according to claim 1, wherein the method comprises the following steps: the process temperature of the melting siliconizing is 1400-1800 ℃.
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| CN111233503A (en) * | 2020-02-26 | 2020-06-05 | 中南大学 | Preparation method of fiber-toughened ceramic matrix composite |
| CN111393178B (en) * | 2020-02-27 | 2021-11-16 | 哈尔滨工业大学 | SiCfPreparation method of @ BN core-shell structure chopped fiber |
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