CN111170752A - Preparation method of silicon carbide ceramic matrix composite and silicon carbide ceramic matrix composite - Google Patents
Preparation method of silicon carbide ceramic matrix composite and silicon carbide ceramic matrix composite Download PDFInfo
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Abstract
According to the preparation method of the silicon carbide ceramic-based composite material, the surface of carbon fiber is subjected to oxidation treatment, silicon carbide nano particles are grafted on the surface of the carbon fiber by adopting a silane coupling agent grafting method, and a polycarbosilane precursor solution is impregnated, cured and pyrolyzed on the surface of the carbon fiber after the silicon carbide nano particles are grafted, so that the carbon fiber reinforced silicon carbide ceramic-based composite material is formed. The silicon carbide ceramic matrix composite material adopts a silane coupling agent grafting method to prepare the silicon carbide nano particle grafted carbon fiber, so that the wettability between the fiber reinforcement and the matrix is enhanced, the fiber and the matrix have proper interface bonding strength, the effective transmission of load between the ceramic matrix and the fiber reinforcement is ensured, and the fiber is protected from physical and chemical damages to a certain extent.
Description
Technical Field
The invention relates to the technical field of material modification treatment, in particular to a preparation method of a silicon carbide ceramic matrix composite material and the silicon carbide ceramic matrix composite material.
Background
Advanced ceramic materials are more and more emphasized by people due to the advantages of high strength, high temperature resistance, chemical corrosion resistance, light specific gravity and the like, but the brittleness problem limits the application of the materials in a plurality of high-end fields. In order to solve the defect of high brittleness of the ceramic material, the carbon fiber is adopted as a reinforcement to prepare the ceramic matrix composite material, so that respective advantages of the carbon fiber and the silicon carbide can be combined to the greatest extent, and the carbon fiber plays roles in high strength, high modulus and high stability, so that the composite material plays a great role potential in the fields of military and aerospace aircrafts.
However, untreated carbon fibers have poor wettability, low reactivity and high inertness on the surface, resulting in poor interfacial properties with the matrix. It is therefore desirable to surface modify carbon fibers to improve the interfacial properties of the composite. The precursor impregnation pyrolysis method is one of the mainstream processes for preparing the carbon fiber reinforced silicon carbide ceramic matrix composite at present, and has the characteristics of short process, low equipment requirement, capability of preparing thick walls, complex shapes, precision parts and the like, which are favored by material workers, but the characteristics of high strength, high modulus and high stability of the carbon fibers in the composite are difficult to exert in the process because the carbon fibers are inevitably physically and chemically damaged in the process, so that the overall performance of the composite is restricted.
Disclosure of Invention
Therefore, it is necessary to provide a method for preparing a silicon carbide ceramic matrix composite with good mechanical properties, aiming at the defects existing in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a silicon carbide ceramic matrix composite, which comprises the following steps:
carrying out oxidation treatment on the surface of the carbon fiber;
grafting silicon carbide nano particles on the surface of the carbon fiber by adopting a silane coupling agent grafting method;
and (3) soaking the surface of the carbon fiber grafted with the silicon carbide nano particles in a polycarbosilane precursor solution, and then curing and pyrolyzing the carbon fiber to form the carbon fiber reinforced silicon carbide ceramic-based composite material.
In some preferred embodiments, in the step of oxidizing the surface of the carbon fiber, the steps are specifically:
immersing the carbon fiber in acetone, heating, refluxing and drying to obtain dried carbon fiber;
immersing the dried carbon fiber in a concentrated acid solution, and taking out after immersing at a proper temperature;
and washing the carbon fiber to be neutral by using deionized water, and drying to obtain the oxidized carbon fiber.
In some preferred embodiments, in the step of immersing the carbon fiber in acetone, and performing heating reflux and drying to obtain the dried carbon fiber, the heating reflux temperature is 60-90 ℃, the reflux time is 15-20 hours, the drying is drying, the drying temperature is 60-90 ℃, and the drying time is 6-12 hours.
In some preferred embodiments, in the step of immersing the dried carbon fiber in a concentrated acid solution, immersing at a suitable temperature and then taking out, the concentrated acid solution is concentrated nitric acid, the immersion temperature is 60-90 ℃, and the immersion time is 1-3 hours.
In some preferred embodiments, in the step of washing the carbon fiber with deionized water to neutrality and drying to obtain the oxidized carbon fiber, the drying is drying at a temperature of 60 to 90 ℃ for 6 to 12 hours.
In some preferred embodiments, in the step of grafting the silicon carbide nanoparticles on the surface of the carbon fiber by using a silane coupling agent grafting method, specifically:
modifying the silicon carbide nanoparticles by using an aminosilane coupling agent to enable the surfaces of the silicon carbide nanoparticles to be provided with amino groups, and grafting the silicon carbide nanoparticles to the surfaces of the carbon fibers by utilizing the reaction of the amino groups and the hydroxyl groups and the carboxyl groups on the surfaces of the oxidized carbon fibers.
In some preferred embodiments, the polycarbosilane precursor solution is a polycarbosilane-xylene solution or a polycarbosilane-toluene solution, and the mass concentration of the polycarbosilane in the polycarbosilane precursor solution is 30-70%.
In some preferred embodiments, in the step of dipping the surface of the carbon fiber grafted with the silicon carbide nanoparticles in a polycarbosilane precursor solution, and then curing and pyrolyzing the carbon fiber to form the carbon fiber reinforced silicon carbide ceramic matrix composite, the dipping temperature is 30 to 60 ℃, the dipping time is 1 to 2 hours, the curing temperature is 100 to 200 ℃, the curing time is 1 to 3 hours, the pyrolyzing temperature is 1200 to 1400 ℃, and the pyrolyzing time is 1 to 2 hours.
In addition, the invention also provides a silicon carbide ceramic matrix composite material which is prepared by the preparation method.
The invention adopts the technical scheme that the method has the advantages that:
the preparation method of the silicon carbide ceramic-based composite material provided by the invention comprises the steps of carrying out oxidation treatment on the surface of carbon fiber, grafting silicon carbide nano particles on the surface of the carbon fiber by adopting a silane coupling agent grafting method, impregnating, curing and pyrolyzing a polycarbosilane precursor solution on the surface of the carbon fiber grafted with the silicon carbide nano particles to form the carbon fiber reinforced silicon carbide ceramic-based composite material, the silicon carbide ceramic matrix composite adopts the silane coupling agent grafting method to prepare the silicon carbide nano particle grafted carbon fiber, obviously increases the wettability between the carbon fiber and the silicon carbide ceramic matrix, improves the interface bonding force between the carbon fiber reinforcement and the ceramic matrix, ensures the effective transfer of the load between the ceramic matrix and the fiber reinforcement, and the silicon carbide nano particles on the surface of the carbon fiber can protect the carbon fiber inside the carbon fiber from being easily damaged by physical and chemical. In the stress process of the composite material, the cracks transferred to the carbon fibers by the matrix deflect at the interface layer to generate a fiber pulling-out phenomenon, the stress at the tips of the cracks is released through the interface energy consumed by pulling out the fibers, and the consumed interface energy is properly increased due to the existence of the silicon carbide nano particles, so that the fibers can play a role in strengthening and toughening.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a scanning electron microscope image of carbon fiber grafted silicon carbide nanoparticles prepared in example 1 of the present invention.
Fig. 2 is a scanning electron microscope image of the carbon fiber grafted silicon carbide nanoparticles prepared in example 2 of the present invention.
Fig. 3 is a scanning electron microscope image of the carbon fiber grafted silicon carbide nanoparticles prepared in example 3 of the present invention.
Fig. 4 is a scanning electron microscope image of the carbon fiber grafted silicon carbide nanoparticles prepared in example 4 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a silicon carbide ceramic matrix composite, which comprises the following steps:
step S110: and carrying out oxidation treatment on the surface of the carbon fiber.
Specifically, in the step of oxidizing the surface of the carbon fiber, specifically:
step S111: immersing the carbon fiber in acetone, heating, refluxing and drying to obtain dried carbon fiber, wherein the heating and refluxing temperature is 60-90 ℃, the refluxing time is 15-20 hours, the drying is drying, the drying temperature is 60-90 ℃, and the drying time is 6-12 hours.
Step S112: immersing the dried carbon fiber in a concentrated acid solution, taking out the carbon fiber after immersion at a proper temperature, wherein the concentrated acid solution is concentrated nitric acid, the immersion temperature is 60-90 ℃, and the immersion time is 1-3 h:
step S113: and washing the carbon fiber to be neutral by using deionized water, and drying to obtain the oxidized carbon fiber, wherein the drying is drying at the temperature of 60-90 ℃ for 6-12 h.
It can be understood that the surface and reactivity of the carbon fiber can be improved by oxidizing the surface of the carbon fiber, and the interface performance between the carbon fiber and the matrix can be improved.
Step S120: and grafting silicon carbide nano particles on the surface of the carbon fiber by adopting a silane coupling agent grafting method.
Specifically, the silicon carbide nanoparticles are modified by using an aminosilane coupling agent, so that amino groups are arranged on the surfaces of the silicon carbide nanoparticles, and the silicon carbide nanoparticles are grafted to the surfaces of the carbon fibers by utilizing the reaction of the amino groups and the hydroxyl groups and the carboxyl groups on the surfaces of the oxidized carbon fibers.
It can be understood that, in order to enhance the surface effect of the carbon fiber and the combination with the polymer matrix, the invention introduces the silicon carbide nano particles on the surface of the carbon fiber, on one hand, because the silicon carbide is not only a strong covalent bond type carbide, but also an engineering ceramic material with excellent performance, the silicon carbide is widely applied in the fields of semiconductor manufacturing and ceramic matrix composite engineering; on the other hand, the silicon carbide has the characteristics of corrosion resistance, high temperature resistance, high strength, good heat conductivity, impact resistance and the like, so that physical and chemical damages to the carbon fibers in the process can be reduced, the carbon fibers have the characteristic of high strength in the composite material, and the improvement of the overall mechanical property of the composite material is facilitated.
According to the invention, the silicon carbide nano particle grafted carbon fiber is prepared by adopting a silane coupling agent grafting method, so that the bonding interface between the carbon fiber and the silicon carbide ceramic matrix is obviously increased, the interface bonding force between the carbon fiber reinforcement and the ceramic matrix is improved, and the effective transfer of the load between the ceramic matrix and the fiber reinforcement is ensured.
Step S130: and (3) soaking the surface of the carbon fiber grafted with the silicon carbide nano particles in a polycarbosilane precursor solution, and then curing and pyrolyzing the carbon fiber to form the carbon fiber reinforced silicon carbide ceramic-based composite material.
Further, the polycarbosilane precursor solution is polycarbosilane-xylene solution or polycarbosilane-toluene solution, and the mass concentration of the polycarbosilane in the polycarbosilane precursor solution is 30-70%. Specifically, the dipping temperature is 30-60 ℃, the dipping time is 1-2 h, the curing temperature is 100-200 ℃, the curing time is 1-3 h, the pyrolysis temperature is 1200-1400 ℃, and the pyrolysis time is 1-2 h.
It can be understood that, the silicon carbide nanoparticles on the surface of the carbon fiber can protect the carbon fiber inside the carbon fiber from being easily damaged by physical and chemical properties, in the stress process of the composite material, the cracks transferred from the matrix to the carbon fiber deflect at the interface layer to generate the fiber extraction phenomenon, and the consumed interface can be properly increased due to the existence of the nanoparticles, thereby being beneficial to the improvement of the mechanical property of the composite material.
The detailed technical scheme is described by combining specific embodiments.
Example 1:
in this embodiment, a preparation method of a silicon carbide ceramic matrix composite is as follows:
(1) completely immersing the carbon fiber in acetone, heating and refluxing for 18h at 80 ℃, drying for 10h at 70 ℃ to obtain dried carbon fiber, completely immersing the dried carbon fiber in concentrated nitric acid, soaking for 2h at 60 ℃, taking out the carbon fiber from the concentrated nitric acid, washing the carbon fiber to be neutral by using deionized water, and drying for 10h at 80 ℃ to obtain the oxidized carbon fiber.
(2) Dispersing 5g of silicon carbide nano particles into ethanol, and modifying the silicon carbide nano particles by using 5% of silane coupling agent gamma-aminopropyltriethoxysilane; and (2) soaking the carbon fiber subjected to the concentrated nitric acid oxidation treatment in the step (1) in a gamma-aminopropyltriethoxysilane-modified silicon carbide nanoparticle solution, and grafting the silicon carbide nanoparticles to the surface of the carbon fiber by utilizing the reaction of amino groups and hydroxyl and carboxyl on the surface of the oxidized carbon fiber.
(3) The carbon fiber reinforced silicon carbide ceramic matrix composite is prepared by adopting a precursor impregnation pyrolysis method. Firstly, the carbon fiber bundle with the surface grafted with the silicon carbide nano particles prepared in the step (2) is fastened on a graphite frame, a polycarbosilane-xylene solution with the mass concentration of 50% is soaked for 1h at the temperature of 60 ℃, then the carbon fiber bundle is cured for 2h at the temperature of 180 ℃, and finally the carbon fiber bundle is insulated for 1h at the temperature of 1400 ℃ for pyrolysis, so that the silicon carbide nano particle modified carbon fiber reinforced silicon carbide ceramic-based composite material is finally prepared.
The scanning electron microscope image of the carbon fiber grafted silicon carbide nanoparticles prepared after the above operation is shown in fig. 1, and it can be seen that uniform silicon carbide nanoparticles are grafted on the surface of the carbon fiber.
Example 2:
in this embodiment, a preparation method of a silicon carbide ceramic matrix composite is as follows:
(1) completely immersing the carbon fiber in acetone, heating and refluxing for 20h at 90 ℃, drying for 12h at 60 ℃ to obtain dried carbon fiber, completely immersing the dried carbon fiber in concentrated nitric acid, soaking for 1.5h at 60 ℃, taking out from the concentrated nitric acid, washing the carbon fiber to be neutral by using deionized water, and drying for 12h at 60 ℃ to obtain the oxidized carbon fiber.
(2) Dispersing 10g of silicon carbide nano particles into ethanol, and modifying the silicon carbide nano particles by using 5% of silane coupling agent gamma-aminopropyltriethoxysilane; and (2) soaking the carbon fiber subjected to the concentrated nitric acid oxidation treatment in the step (1) in a gamma-aminopropyltriethoxysilane-modified silicon carbide nanoparticle solution, and grafting the silicon carbide nanoparticles to the surface of the carbon fiber by utilizing the reaction of amino groups and hydroxyl and carboxyl on the surface of the oxidized carbon fiber.
(3) The carbon fiber reinforced silicon carbide ceramic matrix composite is prepared by adopting a precursor impregnation pyrolysis method. Firstly, fastening the carbon fiber bundle with the surface grafted with the silicon carbide nano particles prepared in the step (2) on a graphite frame, soaking in polycarbosilane-xylene solution with the mass concentration of 50% for 1h at the temperature of 60 ℃, then curing for 1.5h at the temperature of 200 ℃, finally preserving heat for 2h at the temperature of 1200 ℃ for pyrolysis, and finally preparing the silicon carbide nano particle modified carbon fiber reinforced silicon carbide ceramic-based composite material.
The scanning electron microscope image of the carbon fiber grafted silicon carbide nanoparticles prepared after the above operation is shown in fig. 2.
Example 3:
in this embodiment, a preparation method of a silicon carbide ceramic matrix composite is as follows:
(1) completely immersing the carbon fiber in acetone, heating and refluxing for 15h at 60 ℃, drying for 6h at 80 ℃ to obtain dried carbon fiber, completely immersing the dried carbon fiber in concentrated nitric acid, soaking for 1.5h at 60 ℃, taking out from the concentrated nitric acid, washing the carbon fiber to be neutral by using deionized water, and drying for 12h at 60 ℃ to obtain the oxidized carbon fiber.
(2) Dispersing 20g of silicon carbide nano particles into ethanol, and modifying the silicon carbide nano particles by using 8% of silane coupling agent gamma-aminopropyltriethoxysilane; and (2) soaking the carbon fiber subjected to the concentrated nitric acid oxidation treatment in the step (1) in a gamma-aminopropyltriethoxysilane-modified silicon carbide nanoparticle solution, and grafting the silicon carbide nanoparticles to the surface of the carbon fiber by utilizing the reaction of amino groups and hydroxyl and carboxyl on the surface of the oxidized carbon fiber.
(3) The carbon fiber reinforced silicon carbide ceramic matrix composite is prepared by adopting a precursor impregnation pyrolysis method. Firstly, the carbon fiber bundle with the surface grafted with the silicon carbide nano particles prepared in the step (2) is fastened on a graphite frame, a polycarbosilane-xylene solution with the mass concentration of 40% is soaked for 1h at the temperature of 60 ℃, then the carbon fiber bundle is cured for 2h at the temperature of 180 ℃, and finally the carbon fiber bundle is insulated for 1h at the temperature of 1200 ℃ for pyrolysis, so that the silicon carbide nano particle modified carbon fiber reinforced silicon carbide ceramic-based composite material is finally prepared.
The scanning electron microscope image of the carbon fiber grafted silicon carbide nanoparticles prepared after the above operation is shown in fig. 3, and it can be seen that uniform silicon carbide nanoparticles are grafted on the surface of the carbon fiber.
Example 4:
in this embodiment, a preparation method of a silicon carbide ceramic matrix composite is as follows:
(1) completely immersing the carbon fiber in acetone, heating and refluxing for 15h at 60 ℃, drying for 8h at 75 ℃ to obtain dried carbon fiber, completely immersing the dried carbon fiber in concentrated nitric acid, soaking for 1.5h at 70 ℃, taking out from the concentrated nitric acid, washing the carbon fiber to be neutral by using deionized water, and drying for 12h at 60 ℃ to obtain the oxidized carbon fiber.
(2) Dispersing 50g of silicon carbide nano particles into ethanol, and modifying the silicon carbide nano particles by using 10% of silane coupling agent gamma-aminopropyltriethoxysilane; and (2) soaking the carbon fiber subjected to the concentrated nitric acid oxidation treatment in the step (1) in a gamma-aminopropyltriethoxysilane-modified silicon carbide nanoparticle solution, and grafting the silicon carbide nanoparticles to the surface of the carbon fiber by utilizing the reaction of amino groups and hydroxyl and carboxyl on the surface of the oxidized carbon fiber.
(3) The carbon fiber reinforced silicon carbide ceramic matrix composite is prepared by adopting a precursor impregnation pyrolysis method. Firstly, the carbon fiber bundle with the surface grafted with the silicon carbide nano particles prepared in the step (2) is fastened on a graphite frame, a polycarbosilane-xylene solution with the mass concentration of 50% is soaked for 1h at the temperature of 60 ℃, then the carbon fiber bundle is cured for 2h at the temperature of 200 ℃, finally the temperature is kept for 1h at the temperature of 1300 ℃ for pyrolysis, and finally the silicon carbide nano particle modified carbon fiber reinforced silicon carbide ceramic-based composite material is prepared.
The scanning electron microscope image of the carbon fiber grafted silicon carbide nanoparticles prepared after the operation is shown in fig. 4, and it can be seen that the silicon carbide nanoparticles on the surface of the carbon fiber are agglomerated.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
Of course, the positive electrode material of the preparation method of the silicon carbide ceramic matrix composite material of the invention can also have various changes and modifications, and is not limited to the specific structure of the above embodiment. In conclusion, the scope of the present invention should include those changes or substitutions and modifications which are obvious to those of ordinary skill in the art.
Claims (9)
1. The preparation method of the silicon carbide ceramic matrix composite is characterized by comprising the following steps:
carrying out oxidation treatment on the surface of the carbon fiber;
grafting silicon carbide nano particles on the surface of the carbon fiber by adopting a silane coupling agent grafting method;
and (3) soaking the surface of the carbon fiber grafted with the silicon carbide nano particles in a polycarbosilane precursor solution, and then curing and pyrolyzing the carbon fiber to form the carbon fiber reinforced silicon carbide ceramic-based composite material.
2. The method for preparing the silicon carbide ceramic matrix composite according to claim 1, wherein the step of oxidizing the surface of the carbon fiber comprises:
immersing the carbon fiber in acetone, heating, refluxing and drying to obtain dried carbon fiber;
immersing the dried carbon fiber in a concentrated acid solution, and taking out after immersing at a proper temperature;
and washing the carbon fiber to be neutral by using deionized water, and drying to obtain the oxidized carbon fiber.
3. The method for preparing the silicon carbide ceramic matrix composite material according to claim 2, wherein in the step of immersing the carbon fibers in acetone, and performing heating reflux and drying to obtain the dried carbon fibers, the heating reflux temperature is 60-90 ℃, the reflux time is 15-20 hours, the drying is drying, the drying temperature is 60-90 ℃, and the drying time is 6-12 hours.
4. The method for preparing the silicon carbide ceramic matrix composite according to claim 2, wherein in the step of immersing the dried carbon fibers in a concentrated acid solution, taking out the carbon fibers after immersing at a suitable temperature, the concentrated acid solution is concentrated nitric acid, the immersing temperature is 60-90 ℃, and the time is 1-3 hours.
5. The method for preparing the silicon carbide ceramic matrix composite according to claim 2, wherein in the step of washing the carbon fiber with deionized water to neutrality and drying to obtain the oxidized carbon fiber, the drying is drying at a temperature of 60-90 ℃ for 6-12 hours.
6. The method for preparing the silicon carbide ceramic matrix composite material according to claim 1, wherein in the step of grafting the silicon carbide nanoparticles on the surface of the carbon fiber by using a silane coupling agent grafting method, the method specifically comprises the following steps:
modifying the silicon carbide nanoparticles by using an aminosilane coupling agent to enable the surfaces of the silicon carbide nanoparticles to be provided with amino groups, and grafting the silicon carbide nanoparticles to the surfaces of the carbon fibers by utilizing the reaction of the amino groups and the hydroxyl groups and the carboxyl groups on the surfaces of the oxidized carbon fibers.
7. The method for preparing the silicon carbide ceramic matrix composite according to claim 1, wherein the polycarbosilane precursor solution is polycarbosilane-xylene solution or polycarbosilane-toluene solution, and the mass concentration of the polycarbosilane in the polycarbosilane precursor solution is 30-70%.
8. The method for preparing the silicon carbide ceramic-based composite material according to claim 1, wherein in the step of impregnating the surface of the carbon fiber grafted with the silicon carbide nanoparticles into the polycarbosilane precursor solution, and then curing and pyrolyzing the carbon fiber to form the carbon fiber reinforced silicon carbide ceramic-based composite material, the impregnation temperature is 30 to 60 ℃, the impregnation time is 1 to 2 hours, the curing temperature is 100 to 200 ℃, the curing time is 1 to 3 hours, the pyrolysis temperature is 1200 to 1400 ℃, and the pyrolysis time is 1 to 2 hours.
9. A silicon carbide ceramic matrix composite material prepared by the preparation method of any one of claims 1 to 8.
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