CN111825471A - Method for preparing continuous carbon fiber toughened ultrahigh-temperature ceramic matrix composite material through electrophoretic deposition - Google Patents
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Abstract
The invention belongs to the field of ultra-high temperature ceramic matrix composite materials, and particularly relates to a method for preparing a continuous carbon fiber toughened ultra-high temperature ceramic matrix composite material by electrophoretic deposition, wherein a polydopamine coating is prepared on carbon fibers; secondly, the polyethyleneimine is adsorbed on the surface of the ultra-high temperature ceramic powder and the ultra-high temperature ceramic powder is electrified; then, uniformly depositing the charged ultrahigh-temperature ceramic powder on the carbon fiber containing the polydopamine coating by an electrophoretic deposition technology; finally, obtaining the compact continuous carbon fiber toughening ultra-high temperature ceramic matrix composite material through hot pressing sintering. The invention has the advantages that: firstly, the ultrahigh-temperature ceramic powder is effectively introduced into the carbon fiber bundle, so that the problem of difficult densification in the preparation of the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material is solved; and secondly, the chemical corrosion of the carbon fiber is avoided, the matrix components are optimized, a good fiber-matrix interface is obtained, and the fracture resistance and the ultrahigh temperature resistance of the composite material are improved.
Description
Technical Field
The invention belongs to the field of ultrahigh-temperature ceramic-based composite materials, and particularly relates to a method for preparing a continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material by electrophoretic deposition.
Background
With the rapid development of aerospace technologies, advanced technologies using hypersonic missiles, atmospheric vehicles, aerospace planes and the like as application backgrounds gradually become development trends. When flying at a high supersonic speed, the aerodynamic heating makes the surface local temperature of the aircraft very high, and particularly the temperature of key parts of the nose cone, the wing leading edge, the fuselage belly and the like of the aircraft can reach more than 2000 ℃. Although the traditional high-temperature resistant materials (such as carbon fiber reinforced carbon-based composite materials, carbon fiber toughened silicon carbide-based composite materials and the like) have excellent high-temperature mechanical properties, the high-mach-number-based high-temperature resistant materials are difficult to apply to a long-term ultrahigh temperature environment, particularly a severe environment of an oxygen atmosphere, and provide a new challenge for the existing thermal structural materials.
And the ultra-high temperature ceramics (such as zirconium diboride, hafnium diboride, tantalum diboride, zirconium carbide, hafnium carbide, zirconium nitride, hafnium nitride and the like) have high melting point (3000 ℃), high hardness (20 GPa), high stability and excellent oxidation resistance, and have larger potential application value in extreme service environments. However, the ultrahigh-temperature ceramic has greater brittleness and is sensitive to cracks, and the fracture is often expressed as brittle catastrophic failure; in order to improve the fracture resistance, fibers are introduced into the fiber for toughening. The fiber can absorb a large amount of fracture energy through mechanisms such as fiber debonding, fiber pulling-out, fiber bridging and the like, and increase the propagation path of cracks, so that the inherent brittleness of the ceramic is overcome, the fracture toughness of the composite material is improved, and the catastrophic damage is avoided.
The fiber toughened ultrahigh-temperature ceramic-based composite material is divided into a short fiber toughened ultrahigh-temperature ceramic-based composite material and a continuous fiber toughened ultrahigh-temperature ceramic-based composite material from the aspect of the length of the fiber. The short fiber toughened ultrahigh-temperature ceramic-based composite material has the advantage of small anisotropy, but because the fiber length is short, the capacity of absorbing fracture energy through mechanisms such as fiber debonding, fiber bridging, fiber pulling-out and the like is limited, the fracture toughness of the ultrahigh-temperature ceramic-based composite material is difficult to be greatly improved, and the problem that the continuous fiber toughened ultrahigh-temperature ceramic-based composite material is expected to solve is solved.
However, for the continuous fiber toughened ultrahigh-temperature ceramic matrix composite material, the matrix is difficult to fill the inside of the fiber bundle in the preparation process, so that the obtained composite material has the problems of porosity on a microscopic level and difficult densification. In addition, in order to obtain a highly densified ultrahigh-temperature ceramic-based composite material, a sintering aid (such as zirconium disilicide, molybdenum disilicide, silicon nitride, and the like) is generally added into raw material powder to promote densification, but at a relatively high sintering temperature (about 1600 ℃), the sintering aid is easy to chemically react with carbon fibers, which not only reduces the mechanical strength of the fibers, but also easily forms a relatively strong fiber-matrix bonding interface, so that the carbon fibers are difficult to absorb fracture energy through mechanisms such as fiber debonding, fiber extraction, fiber bridging, and the like, and finally, the improvement on the fracture performance of the fiber-toughened ultrahigh-temperature ceramic-based composite material is not ideal.
Therefore, in order to effectively improve the fracture toughness of the fiber-toughened ultra-high temperature ceramic matrix composite, the problem of difficult preparation of the continuous carbon fiber-toughened ultra-high temperature ceramic matrix composite needs to be solved; secondly, the problem of erosion of the fibers by chemical reactions during sintering should be avoided, and a fiber-matrix interface with moderate interface bonding strength is obtained to maximize the toughening effect of the fibers.
Disclosure of Invention
The invention aims to provide a method for preparing a continuous carbon fiber toughened ultra-high temperature ceramic-based composite material by electrophoretic deposition, which solves the problem of difficult preparation of the continuous carbon fiber toughened ultra-high temperature ceramic-based composite material and avoids the problem that fibers are easy to be corroded by a matrix phase in the preparation process of the composite material and obtains a good fiber-matrix bonding interface, thereby preparing the carbon fiber toughened ultra-high temperature ceramic-based composite material with better fracture performance.
In order to realize the purpose of the invention, the technical scheme is as follows:
a method for preparing continuous carbon fiber toughening ultra-high temperature ceramic matrix composite material by electrophoretic deposition, firstly preparing polydopamine coating on carbon fiber by utilizing the characteristic of dopamine oxidative autopolymerization; secondly, polyethyleneimine is adsorbed on the surface of the ultrahigh-temperature ceramic powder containing the sintering aid, and the ultrahigh-temperature ceramic powder is electrified; then, uniformly depositing the charged ultrahigh-temperature ceramic powder on the carbon fiber containing the polydopamine coating by an electrophoretic deposition technology; finally, obtaining the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material through hot-pressing sintering; the method comprises the following specific steps:
1) preparing a polydopamine coating on the heat-treated carbon fiber by taking dopamine as a raw material to obtain the polydopamine coating carbon fiber;
further, the preparation method of the polydopamine coating is that the carbon fiber after heat treatment is soaked in dopamine aqueous solution for 6 to 48 hours;
2) preparing ultra-high temperature ceramic ethanol-based slurry by using ultra-high temperature ceramic powder and polyethyleneimine, wherein the ultra-high temperature ceramic powder contains a sintering aid, and the polyethyleneimine is adsorbed on the surface of the ultra-high temperature ceramic powder through self-assembly and charges the ultra-high temperature ceramic powder;
furthermore, the adding mass ratio of the ultrahigh-temperature ceramic powder to the polyethyleneimine is 1-50; the sintering aid accounts for 5-50% of the ultrahigh-temperature ceramic powder by mass;
3) placing the polydopamine coating carbon fiber in the ultra-high temperature ceramic ethanol-based slurry, applying an electric field, and under the action of the electric field force, gathering the charged ultra-high temperature ceramic powder to the polydopamine coating fiber and continuously depositing the charged ultra-high temperature ceramic powder on the polydopamine coating fiber to obtain the ultra-high temperature ceramic powder coated carbon fiber;
furthermore, the strength of the electric field is 20-2000 volts per meter;
4) and placing the obtained ultrahigh-temperature ceramic powder coated carbon fiber in a high-temperature hot pressing furnace, applying a pressure of 20-50MPa, keeping the temperature at 1200-1400 ℃ for 10-60 minutes for rapid densification, and then sintering the carbon fiber at 1400-1700 ℃ for 10-120 minutes to ensure that pyrolytic carbon from the polymer and the sintering aid perform sufficient chemical reaction, thereby finally obtaining the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material.
The invention has the beneficial effects that:
1) the method comprises the steps of adsorbing polyethyleneimine on the surface of ultra-high temperature ceramic powder, electrifying the ultra-high temperature ceramic powder, and uniformly depositing the electrified ultra-high temperature ceramic powder on carbon fibers containing a polydopamine coating by an electrophoretic deposition technology; by the method, the ultrahigh-temperature ceramic powder can be effectively introduced into the fiber bundle, and the problem that the continuous carbon fiber toughened ultrahigh-temperature ceramic matrix composite material is difficult to densify in preparation is solved on a microscopic level.
2) The pyrolytic carbon derived from the polymer avoids the problem that carbon fibers are corroded by the chemical reaction of a matrix phase in the densification process, so that the carbon fibers keep the original performance, a good fiber-matrix combination interface is obtained, the effects of toughening mechanisms such as fiber pulling-out, fiber bridging, fiber debonding and the like are improved, and the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material with better fracture performance is obtained.
3) The pyrolytic carbon derived from the polymer and the sintering aid with lower melting point in the matrix are subjected to chemical reaction, so that a nano-scale ultrahigh-temperature phase is generated in situ, the matrix components are optimized, and the high-temperature resistance of the composite material is improved.
4) The coating condition of the ultrahigh-temperature ceramic powder can be conveniently optimized by adjusting the electric field intensity, the deposition time and the like of electrophoretic deposition so as to prepare the continuous carbon fiber toughened ultrahigh-temperature ceramic matrix composite material with higher performance. In addition, the anisotropy of the continuous carbon fiber toughened ultrahigh-temperature ceramic matrix composite material can be easily reduced by adjusting the direction of the carbon fibers, and the comprehensive mechanical property of the composite material is further improved.
5) The invention utilizes the electrophoretic deposition technology, has the advantages of green safety, lower cost, high efficiency and the like, and can be realized in the fiber spinning process.
Drawings
FIG. 1 is a scanning electron micrograph of an ultra-high temperature ceramic powder coated carbon fiber of an example;
FIG. 2 is a scanning electron micrograph of a continuous carbon fiber toughened ultra high temperature ceramic matrix composite of an example taken along the length of the fibers;
FIG. 3 is a scanning electron micrograph of a continuous carbon fiber toughened ultra high temperature ceramic matrix composite of an embodiment taken along a cross-sectional direction of the fibers;
FIG. 4 is a back-scattered electron photograph of the fiber-matrix bonding interface region of the example.
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Preparing the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material by using an electrophoretic deposition technology: firstly, preparing a polydopamine coating on carbon fibers by utilizing the characteristic of oxidative self-polymerization of dopamine; secondly, polyethylene imine is adsorbed on the surface of the ultra-high temperature ceramic powder and the ultra-high temperature ceramic powder is electrified; then, uniformly depositing the charged ultrahigh-temperature ceramic powder on the carbon fiber containing the polydopamine coating by an electrophoretic deposition technology; finally, obtaining the continuous carbon fiber toughened ultra-high temperature ceramic matrix composite material through high temperature hot pressing sintering; the method comprises the following specific steps:
firstly, preparing polydopamine coating carbon fiber: soaking the T700 carbon fiber subjected to heat treatment in dopamine aqueous solution for 24 hours;
secondly, electrophoretic deposition is carried out: preparing ultrahigh-temperature ceramic ethanol-based slurry by using ultrahigh-temperature ceramic powder and polyethyleneimine, wherein the ultrahigh-temperature ceramic powder contains zirconium diboride and zirconium disilicide; the adding mass ratio of the ultrahigh-temperature ceramic powder to the polyethyleneimine is 4; the mass percent of the zirconium disilicide accounting for the ultrahigh-temperature ceramic powder is 12 percent; the polyethyleneimine is adsorbed on the surface of the ultra-high temperature ceramic powder through self-assembly, so that the ultra-high temperature ceramic powder is charged; and then placing the carbon fiber with the polydopamine coating in the ethanol-based slurry of the ultra-high temperature ceramic, applying an electric field with the strength of 1000 volts per meter, and under the action of the electric field force, gathering the charged ultra-high temperature ceramic powder to the carbon fiber with the polydopamine coating and continuously depositing the charged ultra-high temperature ceramic powder on the carbon fiber with the polydopamine coating to obtain the carbon fiber coated with the ultra-high temperature ceramic powder. As shown in fig. 1, the ultra-high temperature ceramic powder is uniformly coated, which proves that the ultra-high temperature ceramic powder is successfully and uniformly coated on the polydopamine coating fiber, and the coating thickness can reach more than 30 micrometers; and also can optimize the coating condition by adjusting the electric field intensity, the electrophoretic deposition time, the slurry concentration and the like.
And finally, carrying out high-temperature hot-pressing sintering: placing the obtained ultrahigh-temperature ceramic powder coated carbon fiber in a stone high-temperature hot-pressing furnace, applying the pressure of 40MPa, and keeping the temperature at 1350 ℃ for 30 minutes for rapid densification; then sintering at 1600 ℃ for 30min to allow the pyrolytic carbon derived from the polymer to undergo a sufficient chemical reaction with the zirconium disilicide; finally obtaining the continuous carbon fiber toughened zirconium diboride-based composite material. As shown in fig. 2 and fig. 3, the ultrahigh-temperature ceramic matrix is well distributed between the fibers, and no obvious holes or defects are observed, which proves that the ultrahigh-temperature ceramic powder can be effectively introduced into the fiber bundle by the method, and a compact composite material can be obtained; as shown in fig. 4, the fiber-matrix bonding interface is regular and clear, and the carbon fiber maintains a perfect original profile, which proves that the invention can effectively avoid the chemical corrosion of the fiber, and obtain a good fiber-matrix bonding interface, which is beneficial to the exertion of the toughening mechanism of the carbon fiber and the improvement of the fracture resistance of the composite material. In addition, the black phase in the matrix shown in fig. 4 is silicon carbide, the size is nanometer, and the black phase is randomly and uniformly distributed in the matrix, which proves that pyrolytic carbon derived from the polymer and zirconium disilicide undergo a chemical reaction, and the ultrahigh-temperature nanometer silicon carbide and zirconium carbide matrix phase is generated in situ, so that the high-temperature resistance of the composite material is favorably improved. In conclusion, the method for preparing the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material by electrophoretic deposition solves the problem that the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material is difficult to prepare; the chemical corrosion of the fiber is avoided, a good fiber-matrix bonding interface is obtained, and the toughening effect of the carbon fiber is effectively improved; the high-temperature-resistant composite material is derived from pyrolytic carbon of a polymer, and a sintering aid with a lower melting point in a matrix phase can be converted into an ultrahigh-temperature phase, so that the high-temperature resistance of the composite material is improved; furthermore, it can be realized during the fiber spinning process.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (8)
1. A method for preparing a continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material by electrophoretic deposition is characterized by firstly preparing a polydopamine coating on carbon fibers by utilizing the characteristic of oxidative autopolymerization of dopamine; secondly, polyethyleneimine is adsorbed on the surface of the ultrahigh-temperature ceramic powder containing the sintering aid, and the ultrahigh-temperature ceramic powder is electrified; then, uniformly depositing the charged ultrahigh-temperature ceramic powder on the carbon fiber containing the polydopamine coating by an electrophoretic deposition technology; and finally, obtaining the continuous carbon fiber toughened ultrahigh-temperature ceramic matrix composite material through hot-pressing sintering.
2. The method for preparing the continuous carbon fiber toughened ultra-high temperature ceramic matrix composite material according to claim 1, comprising the following specific steps:
1) preparing a polydopamine coating on the heat-treated carbon fiber by taking dopamine as a raw material to obtain the polydopamine coating carbon fiber;
2) preparing ultra-high temperature ceramic ethanol-based slurry by using ultra-high temperature ceramic powder and polyethyleneimine, wherein the ultra-high temperature ceramic powder contains a sintering aid, and the polyethyleneimine is adsorbed on the surface of the ultra-high temperature ceramic powder through self-assembly and charges the ultra-high temperature ceramic powder;
3) placing the polydopamine coating carbon fiber in the ultra-high temperature ceramic ethanol-based slurry, applying an electric field, and under the action of the electric field force, gathering the charged ultra-high temperature ceramic powder to the polydopamine coating fiber and continuously depositing the charged ultra-high temperature ceramic powder on the polydopamine coating fiber to obtain the ultra-high temperature ceramic powder coated carbon fiber;
4) and placing the obtained ultrahigh-temperature ceramic powder coated carbon fiber in a high-temperature hot pressing furnace, applying a pressure of 20-50MPa, keeping the temperature at 1200-1400 ℃ for 10-60 minutes for rapid densification, and then sintering the carbon fiber at 1400-1700 ℃ for 10-120 minutes to ensure that pyrolytic carbon from the polymer and the sintering aid perform sufficient chemical reaction, thereby finally obtaining the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material.
3. The method for preparing the continuous carbon fiber toughened ultra-high temperature ceramic matrix composite material according to the claim 1 or 2, wherein the poly-dopamine coating is prepared by soaking the heat-treated carbon fiber in dopamine aqueous solution for 6-48 hours.
4. The method for preparing the continuous carbon fiber toughened ultrahigh-temperature ceramic-based composite material by the electrophoretic deposition according to claim 1 or 2, wherein the adding mass ratio of the ultrahigh-temperature ceramic powder to the polyethyleneimine is 1-50; the sintering aid accounts for 5-50% of the ultrahigh-temperature ceramic powder by mass.
5. The method for preparing the continuous carbon fiber toughened ultra-high temperature ceramic-based composite material by electrophoretic deposition according to claim 3, wherein the ratio of the added mass of the ultra-high temperature ceramic powder to the added mass of the polyethyleneimine is 1-50; the sintering aid accounts for 5-50% of the ultrahigh-temperature ceramic powder by mass.
6. The method for preparing the continuous carbon fiber toughened ultra-high temperature ceramic matrix composite material according to the claim 1, 2 or 5, wherein the electric field intensity in the electrophoretic deposition technology is 20-2000 volts per meter.
7. The method for preparing the continuous carbon fiber toughened ultra-high temperature ceramic matrix composite material according to claim 3, wherein the electric field intensity in the electrophoretic deposition technology is 20-2000 volts per meter.
8. The method for preparing the continuous carbon fiber toughened ultra-high temperature ceramic matrix composite material according to claim 4, wherein the electric field intensity in the electrophoretic deposition technology is 20-2000V/m.
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Cited By (6)
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| CN112341204A (en) * | 2020-11-10 | 2021-02-09 | 大连理工大学 | Continuous fiber interweaved and laminated zirconium diboride-based composite material and preparation method thereof |
| CN112341230A (en) * | 2020-11-10 | 2021-02-09 | 大连理工大学 | Hierarchical toughening ultra-high temperature ceramic matrix composite inspired by leaves and preparation method thereof |
| CN113024259A (en) * | 2021-03-18 | 2021-06-25 | 大连理工大学 | Carbon fiber toughened ultrahigh-temperature ceramic-based composite material capable of avoiding thermal mismatch and preparation method thereof |
| CN113395860A (en) * | 2021-06-30 | 2021-09-14 | Oppo广东移动通信有限公司 | Shell, preparation method thereof and electronic equipment |
| CN114634368A (en) * | 2022-05-13 | 2022-06-17 | 浙江星辉新材料科技有限公司 | High-density carbon fiber plate and preparation method thereof |
| WO2022134214A1 (en) * | 2020-12-22 | 2022-06-30 | 苏州宏久航空防热材料科技有限公司 | Continuous electrophoretic deposition modified carbon fiber reinforced multi-matrix composite material and preparation method therefor |
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