CN113480313B - MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof - Google Patents

MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof Download PDF

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CN113480313B
CN113480313B CN202110905498.6A CN202110905498A CN113480313B CN 113480313 B CN113480313 B CN 113480313B CN 202110905498 A CN202110905498 A CN 202110905498A CN 113480313 B CN113480313 B CN 113480313B
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mxene
zirconium
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杨良伟
朱申
刘伟
陈昊然
宋环君
于艺
于新民
刘俊鹏
孙同臣
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Aerospace Research Institute of Materials and Processing Technology
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Abstract

The invention relates to a preparation method of an MXene toughened ultrahigh-temperature ceramic composite material, which comprises the following steps: preparing MAX phase powder into expanded MX phase powder; preparing MXene/zirconium-silicon precursor solution by using the expanded MX-phase powder and the zirconium-silicon precursor solution; curing and cracking the MXene/zirconium silicon precursor solution at high temperature to prepare MXene-doped ZrC/SiC powder; and carrying out hot-pressing sintering reaction on the ZrC/SiC powder to obtain the MXene toughened ultrahigh-temperature ceramic matrix composite. The invention also relates to the ultrahigh-temperature ceramic matrix composite material prepared by the method. The invention utilizes the expanded MX-phase powder with weakened interlayer acting force and intact layered structure and the zirconium-silicon precursor solution to prepare the ultrahigh-temperature ceramic composite material with obviously improved properties such as fracture toughness and the like.

Description

MXene toughened ultrahigh-temperature ceramic composite material and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of ultrahigh-temperature ceramic composite materials, in particular to an MXene toughened ultrahigh-temperature ceramic composite material and a preparation method thereof.
Background
The aerospace craft, as a type of aerospace craft flying in a near space or space, has a flying speed often reaching Ma5 or even higher, is also called aerospace craft, can realize tasks such as quick remote transportation, accurate striking and remote real-time investigation, and has a very high strategic significance for national maintenance ownership. Therefore, many countries including the united states, russia, europe, etc. invest a lot of manpower and material resources to develop relevant research and development.
When the aerospace vehicle enters the atmosphere again at a super high speed, a large amount of kinetic energy is converted into heat energy, so that the surface temperature of the aerospace vehicle is rapidly increased to 2800 ℃ at most, and the surface is strongly washed. Therefore, in the face of the above-mentioned extremely severe environments, extremely high requirements are placed on the thermal protection material. The superhigh temperature ceramic is a multi-element composite material formed by carbides, borides, nitrides and the like of zirconium, hafnium and the like, has the melting point of more than 2500 ℃, has the advantages of high strength and the like, and can be used for thermal protection structural parts of aerospace craft nose cones, leading edges and the like. However, the ultra-high temperature ceramics have the typical brittleness characteristic of ceramics, and are easy to crack particularly under the environment of rapid temperature rise, and a penetrating crack is formed in the matrix, so that the integral failure is caused. Therefore, the improvement of fracture toughness becomes the key of the performance improvement of the ultrahigh-temperature ceramic under the extreme environment.
MAX phase powder is a layered ceramic material with excellent ductility, wherein M represents transition metal, A represents 13 or 14 group element, and X represents carbon element or nitrogen element, MXene can be obtained by layered stripping, and the MAX phase powder can be used for toughening ultrahigh temperature ceramic. However, conventional mixing tends to agglomerate very easily, showing a very uneven dispersion. In order to improve the toughness of the ultrahigh-temperature ceramic, the problem that MXene is poor in dispersion in an ultrahigh-temperature ceramic matrix under the prior art is solved.
Therefore, in view of the above disadvantages, it is desirable to provide an MXene toughened ultra high temperature ceramic composite and a method for preparing the same.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the technical problem that MXene is poor in dispersion in an ultrahigh-temperature ceramic matrix under the condition of the prior art.
(II) technical scheme
In order to solve the technical problem, the invention provides a preparation method of an MXene toughened ultrahigh-temperature ceramic composite material, which comprises the following steps:
(1) preparing MAX phase powder into expanded MX phase powder;
(2) mixing the expanded MX-phase powder with a zirconium-silicon precursor solution under a vacuum condition to form an expanded MXene/zirconium-silicon precursor solution, and performing ultrasonic treatment to obtain an MXene/zirconium-silicon precursor solution;
(3) performing high-temperature curing cracking reaction by taking the MXene/zirconium-silicon precursor solution as a reactant to prepare MXene-doped ZrC/SiC powder;
(4) and carrying out hot-pressing sintering reaction on the MXene-doped ZrC/SiC powder to obtain the MXene-toughened ultrahigh-temperature ceramic-based composite material.
The second aspect of the invention also provides an MXene toughened ultrahigh-temperature ceramic composite material, which is prepared by the preparation method of the first aspect of the invention; preferably, the density of the MXene toughened ultrahigh-temperature ceramic composite material is 80-95%, and the fracture toughness is not lower than 2.4 MPa.m1/2。
(III) advantageous effects
The technical scheme of the invention has the following advantages:
(1) the method adopts hydrofluoric acid as a reaction solvent, so that the A layer in the MAX phase is etched, and the complete layered structure can be still maintained while the interlayer acting force is weakened, thereby forming expanded MX phase powder;
(2) the invention adopts vacuum condition to ensure that the zirconium-silicon precursor solution is fully impregnated into the interlayer of the expanded MX phase to prepare the expanded MX phase/zirconium-silicon precursor solution. Under the action of ultrasound, the expanded MX phase is completely stripped, and the uniform dispersion of single-layer MXene in the zirconium-silicon precursor solution is realized;
(3) the cracking-hot pressing sintering method technology is introduced to prepare the high-density ultrahigh-temperature ceramic to obtain the MXene toughened ultrahigh-temperature ceramic composite material, and the fracture toughness of the ultrahigh-temperature ceramic composite material is remarkably improved.
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The drawings of the present invention are provided for illustrative purposes only, and the scale and size in the drawings are not necessarily consistent with those of actual products.
Fig. 1 is an X-ray diffraction pattern (XRD pattern) of the MXene toughened ultra high temperature ceramic composite of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a preparation method of an MXene toughened ultrahigh-temperature ceramic composite material, which comprises the following steps:
(1) preparing MAX phase powder into expanded MX phase powder;
(2) mixing the expanded MX-phase powder with a zirconium-silicon precursor solution under a vacuum condition to form an expanded MX-phase/zirconium-silicon precursor solution, and performing ultrasonic treatment to obtain an MXene/zirconium-silicon precursor solution; the zirconium-silicon precursor solution is obtained by dissolving a polymer mainly containing zirconium and silicon as solutes in a solvent. The polymer can be converted into ZrC/SiC ceramic through pyrolysis treatment. The zirconium-silicon precursor solution can be dispersed in a solvent such as xylene to form a polymer solution with certain fluidity (the zirconium-silicon precursor solution is purchased from chemical institute of Chinese academy of sciences).
In the step, starting from a MAX phase, preparing the MAX into an expanded MX phase, increasing the interlayer distance, weakening the interlayer acting force, and then enabling the zirconium-silicon precursor solution with certain viscosity to smoothly enter an interlayer region of the expanded MX phase by constructing a vacuum environment. Meanwhile, ultrasonic treatment is carried out on the expanded MX phase/zirconium silicon precursor solution, so that the expanded MX phase is completely stripped into MXene, and the MXene is ensured to be completely and uniformly dispersed in the zirconium silicon precursor solution. By adjusting the mass ratio of the expanded MX phase to the zirconium-silicon precursor solution, the ratio of MXene in the subsequent MXene toughened ultrahigh-temperature ceramic composite material can be adjusted, so that the fracture toughness of the composite material is influenced. Generally, the lower the mass ratio of the expanded MX phase to the zirconium silicon precursor solution, the lower the ratio of MXene in the MXene-toughened ultrahigh temperature ceramic composite, and the poorer the fracture toughness of the composite.
(3) Carrying out high-temperature curing cracking reaction by taking the MXene/zirconium silicon precursor solution as a reactant to prepare MXene-doped ZrC/SiC powder;
(4) and carrying out hot-pressing sintering reaction on the MXene-doped ZrC/SiC powder to obtain the MXene-toughened ultrahigh-temperature ceramic-based composite material.
According to some preferred embodiments, the preparation method of the expanded MX phase powder includes mixing the MAX phase powder with hydrofluoric acid, and etching the MAX phase a layer with hydrofluoric acid to weaken an MXene interlaminar force, thereby obtaining the expanded MX phase powder. Meanwhile, the expanded MX-phase powder is still in a layered structure ceramic and is not peeled into a single layer or a few layers of MXene.
Preferably, the mass ratio of the MAX phase powder to the hydrofluoric acid is 1:10-1: 100.
According to some preferred embodiments, the MAX phase is a class of layered ceramic materials having excellent ductility, including but not limited to Ti3Al2C、Ti3SiC2、Ti3ZnC2And the like.
According to some preferred embodiments, the particle size of the MAX phase powder is 1-50 μm.
The expanded MX-phase powder with the particle size of 1-50 mu m can be prepared by adopting hydrofluoric acid etching and other methods by the technical personnel in the field. The grain diameter is limited to be 1-50 mu m so as to adjust the MXene size subsequently, and therefore the influence of the MXene size on the toughness performance of the ultrahigh-temperature ceramic is examined. Generally, the larger the MAX phase powder particle size and the larger the subsequent MXene size, the smaller the amount of MXene in the same mass, and the poorer the fracture toughness of the MXene toughened ultrahigh temperature ceramic composite material.
According to some preferred embodiments, in the step (2), the MXene/zirconium silicon precursor solution is prepared by:
(I) placing the expanded MX-phase powder and the magnetons in a first container, adding a zirconium-silicon precursor solution into a second container, sealing the first container and the second container, and vacuumizing; the mass ratio of the expanded MX-phase powder to the silicon-zirconium precursor solution is 1:1-1: 100;
(II) after the vacuum degree of the first container is stabilized at 1-100Pa, dropwise adding the zirconium-silicon precursor solution in the second container into the first container filled with the expanded MX-phase powder under the vacuum condition, and magnetically stirring at the rotation speed of 100-1000 rpm;
(III) after the zirconium-silicon precursor solution is completely dripped into the first container, continuously stirring the first container in vacuum for 1-100min to ensure that the zirconium-silicon precursor solution can enter an expansion MX phase interlayer region to obtain an expansion MX phase/silicozirconium precursor solution;
(IV) carrying out ultrasonic treatment on the expanded MX phase/zirconium silicon precursor solution for 1-100min to obtain an MXene/zirconium silicon precursor solution.
According to some preferred embodiments, in step (II), the dropping rate of the dropping is 0.1 to 100 mL/min.
According to some preferred embodiments, in the step (3), the curing temperature for curing is 100-300 ℃, the curing time is 10-100min, the cracking temperature for cracking is 1400-1800 ℃, and the cracking time is 10-100 min.
According to some preferred embodiments, in the step (4), the temperature of the hot-pressing sintering reaction is 1800-2400 ℃, and the pressure is 10-100 MPa.
By adjusting the sintering temperature and pressure, the density of the MXene toughened ultrahigh-temperature ceramic composite material can be adjusted. Generally, the higher the temperature, the higher the pressure, and the higher the densification.
The pyrolysis-hot pressing sintering method is well known in the art, and the determination of the process parameters can be performed by a person skilled in the art according to specific requirements.
The second aspect of the invention provides an ultrahigh-temperature ceramic composite material, which is prepared according to the preparation method of the first aspect of the invention; preferably, the density of the MXene toughened ultrahigh-temperature ceramic composite material is 80-95%, and the fracture toughness is not lower than 2.4MPa ·m1/2. The MXene toughened ultrahigh-temperature ceramic composite material prepared by the method has higher toughness, and is represented by remarkable improvement of fracture toughness performance.
Example 1
(1) Preparing expanded MX phase powder: ti with a particle size of 5 μm3AlC2Mixing the powder with hydrofluoric acid to make hydrofluoric acid and Al layer generate etching reaction to obtain expanded Ti with reduced TiC interlayer acting force and layered structure3C2And (3) powder.
(2) MXene/zirconium silicon precursor solution: placing the 10.0g of the expanded MX-phase powder and the magnetons into a 250mL round-bottom flask, adding a zirconium-silicon precursor solution (purchased from chemical institute of Chinese academy of sciences) into a long-neck funnel, sealing the round-bottom flask, and vacuumizing, wherein the mass ratio of the expanded MX-phase powder to the zirconium-silicon precursor solution is 1: 10; after the round-bottom flask is vacuum-stabilized at 10Pa, slowly dropwise adding the zirconium-silicon precursor solution in the long-neck funnel into the round-bottom flask filled with the expanded MX-phase powder at a dropwise adding speed of 5.0mL/min, and magnetically stirring at a rotating speed of 300 rpm; after the zirconium-silicon precursor solution is completely dripped into the round-bottom flask, continuously stirring the round-bottom flask in vacuum for 10min to ensure that the zirconium-silicon precursor solution can enter an interlayer region of an expanded MX phase; and collecting the expanded MXene/zirconium silicon precursor solution obtained by the treatment, and carrying out ultrasonic treatment for 30min to obtain the MXene/zirconium silicon precursor solution.
(3) MXene toughened ultrahigh-temperature ceramic composite material: placing 100mL of MXene/zirconium silicon precursor solution in a corundum crucible, raising the temperature by program control, and curing and cracking in an inert atmosphere at the curing temperature of 200 ℃, the curing time of 60min, the cracking temperature of 1400 ℃ and the cracking time of 60min to obtain 25.0g of MXene-doped ZrC/SiC powder; hot-pressing and sintering the MXene-doped ZrC/SiC powder at 1800 ℃ and 20MPa to obtain the product with the density of 80 percent and the density of 3.2g/cm3The MXene toughened ultrahigh-temperature ceramic composite material.
(4) And (3) testing mechanical properties: the obtained MXene toughened ultrahigh-temperature ceramic composite material is subjected to mechanical property test, and the fracture toughness is 2.81 MPa.m1/2(see FIG. 1).
Example 2
(1) Expanded MX phase powder: ti with a particle size of 5 μm3A1C2Mixing the powder with hydrofluoric acid to make hydrofluoric acid and Al layer generate etching reaction to obtain expanded Ti with reduced TiC interlayer acting force and layered structure3C2And (3) powder.
(2) MXene/zirconium silicon precursor solution: placing the 10.0g of the expanded MX-phase powder and the magnetons into a 250mL round-bottom flask, adding a zirconium-silicon precursor solution into a long-neck funnel, sealing the round-bottom flask, and vacuumizing, wherein the mass ratio of the expanded MX-phase to the zirconium-silicon precursor solution is 1: 5; after the round-bottom flask is vacuum-stabilized at 10Pa, slowly dropwise adding the zirconium-silicon precursor solution in the long-neck funnel into the round-bottom flask filled with the expanded MX-phase powder at a dropwise adding speed of 5.0mL/min, and magnetically stirring at a rotating speed of 300 rpm; after the zirconium-silicon precursor solution is completely dripped into the round-bottom flask, continuously stirring the round-bottom flask in vacuum for 10min, thereby ensuring that the zirconium-silicon precursor solution can enter an interlayer region of an expanded MX phase; and collecting the expanded MXene/zirconium silicon precursor solution obtained by the treatment, and carrying out ultrasonic treatment for 30min to obtain the MXene/zirconium silicon precursor solution.
(3) MXene toughened ultrahigh-temperature ceramic composite material: placing 100mL of MXene/zirconium silicon precursor solution in a corundum crucible, raising the temperature by program control, and curing and cracking in an inert atmosphere at the curing temperature of 200 ℃ for 60min and the cracking temperature of 1400 ℃ for 60min to obtain 25.0g of MXene-doped ZrC/SiC powder; hot-pressing and sintering the MXene-doped ZrC/SiC powder at 1800 ℃ and 20MPa to obtain the product with the density of 81 percent and the density of 3.26g/cm3The MXene toughened ultrahigh-temperature ceramic composite material.
(4) And (3) testing mechanical properties: the obtained MXene toughened ultrahigh-temperature ceramic composite material is subjected to mechanical property test, and the fracture toughness is 3.02 MPa.m1/2。
Compared with the example 1, when the MXene/zirconium silicon precursor solution is prepared, the proportion of the expanded MXene phase powder and the hafnium-tantalum precursor is adjusted, and the content of the MXene phase powder is increased, so that the content of MXene in the matrix of the MXene toughened ultrahigh-temperature ceramic composite material is increased, and the fracture toughness performance of the composite material is improved.
Example 3
This example 3 is substantially the same as example 1 except that: the Ti3AlC2The particle size was 20 μm.
Example 4
This example 4 is substantially the same as example 3 except that: the hot-pressing sintering temperature is 2000 ℃, and the hot-pressing sintering pressure is 50 MPa.
Example 5
This example 5 is substantially the same as example 3 except that: the Ti3AlC2The particle size was 50 μm.
Example 6
This example 6 is substantially the same as example 5 except that: the hot-pressing sintering temperature is 2000 ℃, and the hot-pressing sintering pressure is 50 MPa.
Example 7
(1) Preparing expanded MX phase powder: ti with the particle size of 20 mu m3AlC2Mixing the powder with hydrofluoric acid to make hydrofluoric acid and Al layer generate etching reaction to obtain expanded Ti with laminated structure and reduced TiC interlayer acting force3C2And (3) powder.
(2) MXene/zirconium silicon precursor solution: placing the 10.0g of the expanded MX-phase powder and the magnetons into a 250mL round-bottom flask, adding a zirconium-silicon precursor solution into a long-neck funnel, wherein the mass ratio of the expanded MX-phase to the zirconium-silicon precursor solution is 1:10, slowly dropwise adding the zirconium-silicon precursor solution into the round-bottom flask filled with the expanded MX-phase powder at a dropwise adding speed of 5.0mL/min, and magnetically stirring at a rotating speed of 300 rpm; and after the zirconium-silicon precursor solution is completely dripped into the round-bottom flask, continuously stirring the round-bottom flask in vacuum for 10min, so that the zirconium-silicon precursor solution can enter an expanded MX phase interlayer region to obtain the MXene/zirconium-silicon precursor solution.
(3) MXene toughened ultrahigh-temperature ceramic composite material: 100mL of MXene/zirconium pre-silicaPlacing the precursor solution in a corundum crucible, raising the temperature by program control, and carrying out curing and cracking under an inert atmosphere, wherein the curing temperature is 200 ℃, the curing time is 60min, the cracking temperature is 1400 ℃, and the cracking time is 60min, so as to obtain 25.0g of MXene-doped ZrC/SiC powder; hot-pressing and sintering the MXene-doped ZrC/SiC powder at 1800 ℃ and 20MPa to obtain the product with 82% density and 3.01g/cm density3The MXene toughened ultrahigh-temperature ceramic composite material.
(4) And (3) testing mechanical properties: the obtained MXene toughened ultrahigh-temperature ceramic composite material is subjected to mechanical property test, and the fracture toughness is 2.18 MPa.m1/2。
It can be seen that comparing example 3 with example 7, example 3 employs vacuum conditions and sonication, resulting in improved fracture toughness properties of the composite.
Example 8
(1) MAX/zirconium silicon precursor solution: 10.0g of Ti having a particle size of 20 μm3AlC2Placing the powder and the magneton in a 250mL round-bottom flask, adding the zirconium-silicon precursor solution into a long-neck funnel, and adding Ti3AlC2The mass ratio of the precursor solution to the zirconium-silicon precursor solution is 1:10, and the zirconium-silicon precursor solution in the long-neck funnel is slowly dripped to the Ti-containing solution3AlC2Dripping 5.0mL/min powder into a round-bottom flask, and magnetically stirring at the rotating speed of 300 rpm; after the zirconium silicon precursor solution is completely dripped into the round-bottom flask, continuously stirring the round-bottom flask in vacuum for 10min, thereby ensuring that the zirconium silicon precursor solution can enter Ti3AlC2And obtaining MAX/zirconium silicon precursor solution in the phase interlamination area.
(3) MAX phase toughened ultrahigh-temperature ceramic composite material: putting 100mL of MAX/zirconium-silicon precursor solution into a corundum crucible, raising the temperature by program control, and curing and cracking under an inert atmosphere, wherein the curing temperature is 200 ℃, the curing time is 60min, the cracking temperature is 1400 ℃, and the cracking time is 60min, so as to obtain 25.0g of MAX doped ZrC/SiC powder; carrying out hot-pressing sintering on the MAX doped ZrC/SiC powder at 1800 ℃ and 20MPa to prepare the ZrC/SiC powder with the density of 78 percent and the density of 2.85g/cm3The MAX toughened ultrahigh temperature ceramic composite material.
(4) And (3) testing mechanical properties: the obtained MAX toughened ultrahigh-temperature ceramic composite material is subjected to mechanical property test, and the fracture toughness is 1.81 MPa.m1/2。
Figure BDA0003199861220000111
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (12)

1. The preparation method of the MXene toughened ultrahigh-temperature ceramic composite material is characterized by comprising the following steps of:
(1) preparing MAX phase powder into expanded MX phase powder; the particle size of the expanded MX-phase powder is 1-50 μm; the expanded MX-phase powder is of a layered structure;
(2) mixing the expanded MX-phase powder with a zirconium-silicon precursor solution under a vacuum condition to enable the zirconium-silicon precursor solution to enter an interlayer region of the expanded MX-phase powder to form an expanded MX-phase/zirconium-silicon precursor solution, and performing ultrasonic treatment to obtain an MXene/zirconium-silicon precursor solution;
(3) carrying out high-temperature curing cracking reaction by taking the MXene/zirconium silicon precursor solution as a reactant to prepare MXene-doped ZrC/SiC powder;
(4) and carrying out hot-pressing sintering reaction on the MXene-doped ZrC/SiC powder to obtain the MXene-toughened ultrahigh-temperature ceramic-based composite material.
2. The method of claim 1, wherein: the preparation method of the expanded MX-phase powder comprises the steps of mixing MAX-phase powder with hydrofluoric acid, and etching the MAX-phase A layer by hydrofluoric acid to obtain the expanded MX-phase powder.
3. The method of claim 1, wherein: the mass ratio of the MAX phase powder to the hydrofluoric acid is 1:10-1: 100.
4. The method of claim 1, wherein: the MAX phase is Ti3Al2C、Ti3SiC2、Ti3ZnC2One or more of (a).
5. The method of claim 1, wherein: the particle size of the MAX phase powder is 1-50 μm.
6. The method of claim 1, wherein: in the step (2), the preparation method of the MXene/zirconium silicon precursor solution comprises the following steps:
(I) placing the expanded MX-phase powder and magnetons into a first container, adding a zirconium-silicon precursor solution into a second container, sealing the first container and the second container, and vacuumizing;
(II) after the vacuum degree of the first container is stabilized at 1-100Pa, dropwise adding the zirconium-silicon precursor solution in the second container into the first container filled with the expanded MX-phase powder under the vacuum condition, and magnetically stirring at the rotation speed of 100-1000 rpm;
(III) after the zirconium-silicon precursor solution is completely dripped into the first container, continuously stirring the first container in vacuum for 1-100min to obtain an expanded MX phase/silicon-zirconium precursor solution;
(IV) carrying out ultrasonic treatment on the expanded MX phase/zirconium silicon precursor solution for 1-100min to obtain an MXene/zirconium silicon precursor solution.
7. The method of claim 6, wherein: the mass ratio of the expanded MX-phase powder to the silicon-zirconium precursor solution is 1:1-1: 100.
8. The method of claim 6, wherein: in the step (II), the dropping speed of the dropping is 0.1-100 mL/min.
9. The method of claim 1, wherein: in the step (3), the curing temperature is 100-300 ℃, the curing time is 10-100min, the cracking temperature is 1400-1800 ℃, and the cracking time is 10-100 min.
10. The method of claim 1, wherein: in the step (4), the temperature of the hot-pressing sintering reaction is 1800-2400 ℃, and the pressure is 10-100 MPa.
11. An MXene toughened ultrahigh-temperature ceramic composite material is characterized in that: the ultrahigh-temperature ceramic composite material is prepared according to the preparation method of any one of claims 1 to 10.
12. The MXene toughened ultra high temperature ceramic composite of claim 11 wherein: the density of the MXene toughened ultrahigh-temperature ceramic composite material is 80-95%; fracture toughness of not less than 2.4 MPa.m1/2。
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