A porous titanium carbide-nickel composite material with a dense layer-wall structure and a preparation method thereof

Abstract

The application discloses a kind of porous titanium carbide-nickel composite material of compact layer-wall structure and preparation method, belong to porous material technical field.Preparation method is: titanium carbide powder and nickel powder are added in the mixed solution of gelatin and polyvinylpyrrolidone and ultrasonic mixing, obtain mixed suspension, then carry out ball milling, defoaming, obtain mixed slurry;After the mixed slurry is carried out two-way freezing treatment, it is sequentially vacuum freeze-drying and sintering treatment, i.e. the porous titanium carbide-nickel composite material of the application is obtained.The porous titanium carbide-nickel composite material prepared by the application has the characteristics of uniform structure, layer-wall compactness, high porosity, excellent mechanical properties, etc., and can be used as a catalyst carrier, sound absorption, wave absorption, shock absorption and other materials, and has great application potential in metallurgy, chemical industry, biological implants and other fields.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of porous materials, and particularly relates to a porous titanium carbide-nickel composite material with a dense layer-wall structure and a preparation method. BACKGROUND

[0002] Porous ceramics have a series of advantages such as low density, large specific surface area, high temperature resistance and corrosion resistance, and can be widely applied to fields such as metallurgy, chemical industry, biological implants and the like as sound-absorbing, wave-absorbing, shock-absorbing and catalytic carriers. It is known that the mechanical properties of porous ceramics are inversely proportional to the porosity, and a biological bionic structure (layer-wall) is generated to obtain high-porosity high-strength porous materials. A two-way freezing method uses ice crystals as a template agent to prepare the porous material with the layer-wall structure and high porosity. However, the two-way freezing method for preparing the porous material still has the following problems: 1) the pores of the porous ceramics are unevenly distributed, so that the structure of the porous ceramics is irregular, thereby affecting the compressive strength; and 2) the layer-wall has low density, and there are pores of different sizes on the surface and inside the layer-wall, and the defects seriously affect the mechanical properties of the material, so that the structure of the material is easily damaged in the use process. The low density of the layer-wall has become an important factor restricting the improvement of the mechanical properties of the porous ceramic material. Therefore, designing a porous material with high layer-wall density and excellent mechanical properties has gradually become the focus and difficulty in the field of porous materials. SUMMARY

[0003] To solve the above problems in the prior art, the application provides a porous titanium carbide-nickel composite material with a dense layer-wall structure and a preparation method.

[0004] To achieve the above object, the application provides the following technical scheme.

[0005] The application provides a preparation method of a porous titanium carbide-nickel composite material with a dense layer-wall structure, comprising the following steps:

[0006] (1) titanium carbide powder and nickel powder are added into a mixed solution composed of gelatin and polyvinylpyrrolidone for ultrasonic mixing to obtain a mixed suspension, and then ball milling and defoaming are performed to obtain a mixed slurry with good stability;

[0007] (2) after the mixed slurry is subjected to two-way freezing treatment, vacuum freeze drying and sintering are sequentially performed, and the porous titanium carbide-nickel composite material is obtained.

[0008] Beneficial effects: the application of the bidirectional freezing technology, fully utilizes the theory of ice crystal nucleation, makes the particles spontaneously accumulate in the bidirectional freezing process, can form a good "layer-wall" structure, meanwhile, cooperates with sintering treatment, improves the density of the "layer-wall" structure, and further improves the compression strength of the porous titanium carbide-nickel composite material, and good porous material with layered structure can be obtained.

[0009] The principle of the bidirectional freezing technology in the application is that a wedge-shaped block with a certain angle (the material is polydimethylsiloxane (PDMS)) is added between the cold source and the slurry, so that the nucleation of ice crystals in the slurry is changed from two-dimensional plane nucleation to one-dimensional freezing line nucleation, compared with ordinary freezing, the technology can effectively improve the order of ice crystal growth, and further improve the order of the "layer-wall" structure of the porous material.

[0010] Further, the gelatin is gelatin powder, and the polyvinylpyrrolidone is polyvinylpyrrolidone powder.

[0011] Further, the specific preparation method of the mixed solution in step (1) is that the gelatin and polyvinylpyrrolidone are added to water and dissolved at 40-60℃, and the mixed solution is obtained.

[0012] Further, the shape of the nickel powder in step (1) is spherical.

[0013] The particle size of the titanium carbide powder is 1-30μm, and the particle size of the nickel powder is 20-50μm.

[0014] The molecular weight of the gelatin is 10000-100000, and the molecular weight of the polyvinylpyrrolidone is 20000-80000.

[0015] The titanium carbide powder and the nickel powder form a mixed powder.

[0016] The mass ratio of the titanium carbide powder to the nickel powder is (6-9) :(1-4).

[0017] The solid content of the mixed powder in the mixed suspension is 5-30vol.%.

[0018] The mass ratio of the mixed powder to polyvinylpyrrolidone is 100:(0.2-0.5).

[0019] The gelatin is 1-3wt.% of water.

[0020] Beneficial effects: the present application adopts spherical nickel powder as main raw material, the basic reason is that the spherical nickel powder is easy to migrate in the ice crystal growth process, and is accumulated in the pore of the layer wall, thereby improving the density of the porous green material; at the same time, the spherical nickel powder will melt on the surface during the sintering process of the green material, thereby bonding the titanium carbide particles.

[0021] Further, the ultrasonic time in step (1) is 10-45 min, and the power is 80-300 W; the ball milling is carried out at a speed of 150-200 r / min for 24-48 h; the medium of the ball milling is zirconium oxide grinding ball with a particle size of 1-5 mm; the mass ratio of the zirconium oxide grinding ball to the mixed powder of titanium carbide powder and nickel powder is 25: (10-12.5).

[0022] Beneficial effects: under the ball material ratio, the present application can better ensure the uniform distribution of each particle in the mixed slurry and better retain the shape and size of each particle.

[0023] Further, the defoaming in step (1) is carried out by using defoaming agent n-octanol at a speed of 10-15 r / min for 1-3 h; wherein, the mass ratio of the mixed suspension to n-octanol is 1000: (0.1-0.3).

[0024] Beneficial effects: the n-octanol in the present application is a long-chain alcohol, which has good surfactant function, can better reduce the surface tension of the mixed slurry, and thus the bubbles generated in the stirring process can easily overflow and break.

[0025] Further, the freezing rate of the bidirectional freezing treatment in step (2) is-3 to-5 ℃ / min, and the mixed slurry is cooled to complete solidification.

[0026] Beneficial effects: in the process of bidirectional freezing treatment, too high freezing rate will cause the particles in the slurry to not have enough time to migrate to the layer-wall of the porous material, thereby reducing the density of the layer-wall; too low freezing rate will cause the thickness of the layer-wall to be too large, which cannot control the pore of the layer-wall well; the present application sets the freezing rate to-3 to-5 ℃ / min, under this freezing rate, the thickness of the layer-wall can be controlled well, and the particles have enough time to migrate to the layer-wall during the freezing process, thereby realizing the preparation of the porous material with high-density layer-wall structure.

[0027] Further, the temperature of the vacuum freeze-drying in step (2) is-50 to-70 ℃, the time is 24-48 h, and the vacuum degree is 0.1-10 Pa.

[0028] Further, the sintering in step (2) is at a temperature of 1250-1450 DEG C at a heating rate of 2-6 DEG C / min for 1-3 hours, and the cooling rate after sintering is also 2-6 DEG C / min.

[0029] Beneficial effects: The application controls the heating rate in the sintering process to be 2-6 DEG C / min, which is beneficial to the volatilization of organic matter in the green body material in the sintering process, and helps the metal Ni in the skeleton to fully spread, thereby well filling the small pores in the skeleton, improving the density of the layer-wall, and further improving the overall performance of the skeleton.

[0030] The application also provides a layered porous titanium carbide-nickel composite material prepared by the preparation method.

[0031] Compared with the prior art, the application has the following beneficial effects:

[0032] The application adopts bidirectional freezing and vacuum freeze-drying technology to prepare a porous titanium carbide-nickel composite material with a dense layer-wall structure, which exhibits uniform organization, dense layer-wall, high porosity, and excellent mechanical properties, and the compressive strength in the direction perpendicular to the cold source can reach 13 MPa or above, and can be used as a catalyst carrier and a material for sound absorption, wave absorption, and shock absorption, and has great application potential in the fields of metallurgy, chemical industry, and biological implants.

[0033] The interlayer spacing, wall thickness, and layer-wall density of the ceramic material prepared by the preparation method of the application can be adjusted by controlling the solid content of the mixed powder in the suspension and the proportion of the two powders in the mixed powder, so as to meet the performance requirements of different application fields. BRIEF DESCRIPTION OF DRAWINGS

[0034] The accompanying drawings, which form a part of the present application, are intended to provide further understanding of the present application and are incorporated herein for explanation by way of the non-limiting examples. In the drawings:

[0035] Figure 1 FIG. 4 is a scanning electron microscope image of the wall structure of the porous titanium carbide-nickel composite material with a dense layer-wall structure prepared in Example 1;

[0036] Figure 2 FIG. 5 is an enlarged scanning electron microscope image of the wall structure of the porous titanium carbide-nickel composite material with a dense layer-wall structure prepared in Example 1;

[0037] Figure 3 FIG. 6 is a scanning electron microscope image of the layer-wall structure of the porous titanium carbide-nickel composite material with a dense layer-wall structure prepared in Example 1;

[0038] Figure 4 SEM photograph of the layer-wall structure of the porous titanium carbide-nickel composite material having a dense layer-wall structure prepared in Example 1, which is enlarged;

[0039] Figure 5 Compression stress-strain curve of the porous titanium carbide-nickel composite material having a dense layer-wall structure prepared in Example 1.

[0040] Figure 6 SEM photograph of the layer-wall structure of the porous titanium carbide-nickel composite material having a layered structure prepared in Comparative Example 1. DETAILED DESCRIPTION

[0041] The detailed description particularly describes various exemplary embodiments of the application, which description is not to be considered limiting in any way. Rather, the scope of the application includes certain aspects, characteristics, and embodiments of the application that are more fully described.

[0042] It should be understood that the terms used in the specification are for the purpose of describing particular embodiments only and are not intended to be limiting of the present application. In addition, where particular ranges of values are given, understand that each intervening value, to the upper or lower limit of the ranges is also specifically included. Each smaller range that falls within the broader ranges is also specifically included in the present application. The upper and lower limits of these smaller ranges can independently be included or excluded in the range.

[0043] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. Although preferred methods and materials are described, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application. All documents mentioned herein are incorporated by reference to disclose and describe the methods and / or materials in connection with which the documents are cited. In case of conflict, the present specification will control.

[0044] Various modifications and changes can be made to the specific embodiments of the present application described herein without departing from the scope or spirit of the application. Other embodiments of the application will be apparent to those of ordinary skill in the art from the description and examples presented herein. The description and examples are illustrative of the application and are not intended to limit the scope of the application.

[0045] As used herein, the terms "comprise", "comprising", "include", "including", "have", "having" and the like are open-ended and do not exclude additional elements or steps.

[0046] A porous titanium carbide-nickel composite material with a compact layer-wall structure, and a preparation method thereof, comprises the following steps:

[0047] 1) Gelatin and polyvinylpyrrolidone (PVP) are added to water to dissolve at 40-60°C (preferably 60°C) to obtain a mixed solution, and then 60-90 wt.% titanium carbide powder and 10-40 wt.% spherical nickel powder are added, and ultrasonic mixing treatment is performed at a power of 80-300 W (preferably 120 W) for 10-45 min (preferably 30 min) to obtain a mixed suspension;

[0048] The particle size of the titanium carbide powder is 1-30 μm, and the particle size of the spherical nickel powder is 20-50 μm; the molecular weight of the gelatin is 10,000-100,000, and the molecular weight of the polyvinylpyrrolidone is 20,000-80,000; in the obtained mixed suspension, the solid content of the titanium carbide-spherical nickel powder mixed powder is 5-30 vol.%, the mass ratio of the mixed powder to the polyvinylpyrrolidone is 100: (0.2-0.5), and the mass of the gelatin is 1-3 wt.% of the mass of the water;

[0049] 2) The mixed suspension is mixed with zirconia grinding balls with a particle size of 1-5 mm (preferably 4 mm), and ball milling treatment is performed at a rotating speed of 150-200 r / min (preferably 150 r / min) for 24-48 h (preferably 24 h), and then a defoaming agent n-octanol is added, and defoaming treatment is performed at a rotating speed of 10-15 r / min (preferably 10 r / min) for 1-3 h (preferably 2 h) to obtain a mixed slurry with uniform and stable particle dispersion;

[0050] The mass ratio of the zirconia grinding balls to the mixed powder of the titanium carbide powder and the nickel powder is 25: (10-12.5), and the mass ratio of the mixed suspension to the n-octanol is 1000: (0.1-0.3);

[0051] 3) A drop-in refrigerator is used to freeze the mixed slurry in two directions at a cooling rate of -3°C / min to -5°C / min (preferably -5°C / min), and then the frozen sample is moved into a vacuum freeze dryer for freeze drying for 24-48 h (preferably 48 h) to obtain a ceramic body with a layered porous structure, wherein the temperature of the vacuum freezing is -50 to -70°C (preferably -50°C), and the vacuum degree is 0.1-10 Pa (preferably 0.1 Pa);

[0052] The ceramic green body is heated to 1250-1450℃ (preferably 1450℃ / min) at a heating rate of 2-6℃ / min (preferably 5℃ / min) for 1-3h (preferably 2h) and then cooled to room temperature at a cooling rate of 2-6℃ / min (preferably 5℃ / min), to obtain the porous titanium carbide-nickel composite material with dense layer-wall structure.

[0053] The room temperature in the embodiments of the present application is 25±2℃ under normal circumstances.

[0054] The water in the embodiments of the present application is deionized water.

[0055] Embodiment 1

[0056] A method for preparing a layered titanium carbide-nickel porous ceramic composite material with an ordered dense layer-wall structure, comprising the following steps:

[0057] (1) 1.584g of gelatin powder and 0.23g of polyvinylpyrrolidone powder are added to 79.2mL of deionized water and heated to 60℃ for dissolution, and after complete dissolution, a mixed solution is obtained, and then 38.1g of titanium carbide powder and 9.5g of spherical nickel powder are weighed and added to the mixed solution, and ultrasonic mixing is performed at a power of 120W for 30min to obtain a mixed suspension;

[0058] (2) 100g of zirconia grinding balls with an average particle size of 4mm are weighed and mixed with the mixed suspension in step (1) and then added to a ball mill tank, and ball milling is performed at a speed of 150r / min for 24h, and then 0.02g of n-octanol is added for low-speed defoaming treatment at a speed of 10r / min for 2h to obtain a mixed slurry with uniform particle dispersion and good stability;

[0059] (3) The mixed slurry obtained in step (2) is subjected to bidirectional freezing treatment at a cooling rate of -5℃ / min using a drop-in refrigerator, and after the mixed slurry is completely solidified, it is placed in a vacuum freeze dryer with a vacuum degree of 0.1Pa and a temperature of -50℃ for freeze drying for 48h to obtain a porous ceramic green body with a layered structure, and finally it is heated to a temperature of 1450℃ at a heating rate of 5℃ / min, and then sintered at a constant temperature for 2h, and then cooled to room temperature at a cooling rate of 5℃ / min to obtain a porous titanium carbide-nickel composite material, and the characterization results are as follows:

[0060] The scanning electron microscope image of the wall structure of the porous composite material is as shown in Figure 1 The scanning electron microscope image of the wall structure of the porous composite material is as shown in Figure 1 It can be seen that the gray titanium carbide-nickel presents a lamellar structure. Figure 2 The scanning electron microscope image of the wall structure of the porous composite material is as shown in Figure 3A scanning electron microscope image of a layer-wall structure of a porous composite material, Figure 4 A magnified scanning electron microscope image of a layer-wall structure of a porous composite material. It can be seen that the titanium carbide particles of the porous composite material prepared in this embodiment are tightly combined, and the average spacing between the lamellae is 100 ± 10 μm. Figures 2-4 The average density of the porous material is 1.26 g / cm 3 , and the porosity is 76.6%, wherein the single layer-wall density is 95% (referring to the theoretical density of the material 5.4 g / cm 3 );

[0061] Figure 5 A compression stress-strain curve of a porous composite material, which is obtained from Figure 5 It can be seen that the compressive strength of the porous composite material perpendicular to the cold source direction reaches 13.3 MPa.

[0062] Example 2

[0063] A method for preparing a layered titanium carbide-nickel porous ceramic composite material with an ordered and dense layer-wall structure, comprising the following steps:

[0064] (1) 1.584 g of gelatin powder and 0.2505 g of polyvinylpyrrolidone powder are added to 79.2 mL of deionized water and heated to 60°C for dissolution. After complete dissolution, a mixed solution is obtained. Then 35.1 g of titanium carbide powder and 15 g of spherical nickel powder are added to the mixed solution, and ultrasonic mixing is performed at a power of 120 W for 30 min to obtain a mixed suspension;

[0065] (2) 105 g of zirconia grinding balls with an average particle size of 4 mm are weighed and mixed with the mixed suspension in step (1), and then added to a ball mill tank. Ball milling is performed at a speed of 150 r / min for 24 h. After ball milling, 0.02 g of n-octanol is added for low-speed defoaming at a speed of 10 r / min for 2 h to obtain a mixed slurry with uniform particle dispersion and good stability;

[0066] (3) The mixed slurry obtained in step (2) is subjected to bidirectional freezing treatment at a cooling rate of -5°C / min using a drop-in refrigeration machine. After the mixed slurry is completely solidified, it is placed in a vacuum freeze dryer with a vacuum degree of 0.1 Pa and a temperature of -50°C for freeze drying for 48 h to obtain a porous ceramic body with a layered structure. Finally, it is heated to a temperature of 1450°C at a heating rate of 5°C / min, and sintered at a constant temperature for 2 h. Then it is cooled to room temperature at a cooling rate of 5°C / min. A porous titanium carbide-nickel composite material is obtained, and the characterization results are as follows:

[0067] The gray titanium carbide-nickel in the porous ceramic composite prepared in this example presents a lamellar structure, the titanium carbide particles are closely combined, and the average spacing between the lamellas is 110±10 μm. The average density of the porosity is 1.107 g / cm 3 , the porosity is 79.5%, and the single-lamella-wall density is 97% (referring to the theoretical density of the material 5.4 g / cm 3 ); the compressive strength of the porous ceramic composite perpendicular to the cold source direction reaches 15 MPa.

[0068] Comparative Example 1

[0069] A method for preparing a lamellar titanium carbide-nickel porous ceramic composite with an ordered and dense lamella-wall structure, comprising the following steps:

[0070] (1) 1.584 g of gelatin and 0.23 g of polyvinylpyrrolidone are added to 79.2 mL of deionized water and heated to 60°C for dissolution. After complete dissolution, a mixed solution is obtained. Then 38.1 g of titanium carbide powder and 9.5 g of non-spherical nickel powder are added to the mixed solution, and ultrasonic mixing is performed at a power of 120 W for 30 min to obtain a mixed suspension;

[0071] (2) 100 g of zirconia grinding balls with an average particle size of 4 mm are mixed with the mixed suspension in step (1) and then added to a ball mill tank. Ball milling is performed at a speed of 150 r / min for 24 h. After ball milling, 0.02 g of n-octanol is added for low-speed defoaming treatment at a speed of 10 r / min for 2 h to obtain a mixed slurry with uniform particle dispersion and good stability;

[0072] (3) The mixed slurry obtained in step (2) is subjected to bidirectional freezing treatment at a cooling rate of -5°C / min using a drop-in refrigeration machine. After the mixed slurry is completely solidified, it is placed in a vacuum freeze dryer with a vacuum degree of 0.1 Pa and a temperature of -50°C for freeze drying for 48 h to obtain a porous ceramic body with a lamellar structure. Finally, it is sintered at a temperature of 1450°C for 2 h at a heating rate of 5°C / min, and then cooled to room temperature at a cooling rate of 5°C / min to obtain a porous titanium carbide-nickel composite material. The characterization results are as follows:

[0073] The average spacing between the lamellas in the porous composite material prepared in this comparative example is 48±5 μm. The average density of the porosity is 2.13 g / cm 3 , the porosity is 60.5%, and the single-lamella-wall density is 50% (referring to the theoretical density of the material 5.4 g / cm 3The compressive strength of this porous composite material perpendicular to the cold source direction is only 6.3 MPa.

[0074] Comparative Example 2

[0075] The preparation method of a layered titanium carbide-nickel porous ceramic composite material with an ordered dense layer-wall structure is different from that in Example 1 only in that the cooling rate of bidirectional freezing in step (3) is -1℃ / min.

[0076] The remaining steps are the same as in Example 1.

[0077] The gray titanium-nickel carbide composite material prepared in this comparative example exhibits a layered structure with an average interlayer spacing of 120 ± 5 μm. The average density of this porous composite was determined to be 1.053 g / cm³ by measuring the sample's volume and mass. 3 The porosity is 80.5%, with a single-layer-wall compaction density of 65.8% (referencing the material's theoretical density of 5.4 g / cm³). 3 The porous ceramic composite material exhibits a compressive strength of 8.58 MPa perpendicular to the cold source direction.

[0078] Comparative Example 3

[0079] The preparation method of a layered titanium carbide-nickel porous ceramic composite material with an ordered dense layer-wall structure is different from that in Example 1 only in that the cooling rate of bidirectional freezing in step (3) is -6℃ / min.

[0080] The remaining steps are the same as in Example 1.

[0081] The gray titanium carbide-nickel composite material prepared in this comparative example exhibits a layered structure with tightly bonded titanium carbide particles and an average interlayer spacing of 80.5 μm. The average density of this porous composite material was determined to be 2.16 g / cm³ by measuring the sample's volume and mass. 3 The porosity is 60%, with a single-layer-wall compaction of 97.5% (referencing the material's theoretical density of 5.4 g / cm³). 3 The porous ceramic composite material exhibits a compressive strength of 16.65 MPa perpendicular to the cold source direction.

[0082] The above are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A method for producing a porous titanium carbide-nickel composite material of a dense layer-wall structure, characterized by, The method comprises the following steps: (1) adding titanium carbide powder and nickel powder into a mixed solution composed of gelatin and polyvinylpyrrolidone, and mixing ultrasonically to obtain a mixed suspension, then performing ball milling and defoaming to obtain a mixed slurry; the shape of the nickel powder in step (1) is spherical; (2) performing bidirectional freezing treatment on the mixed slurry, and then sequentially performing vacuum freeze drying and sintering to obtain the porous titanium carbide-nickel composite material. In step (2), the freezing rate of the bidirectional freezing treatment is -3 to -5 ℃ / min, and the mixed slurry is cooled to complete solidification.

2. The method of claim 1, wherein the method is characterized by: In step (1), the specific preparation method of the mixed solution is as follows: the gelatin and polyvinylpyrrolidone are added into water and dissolved at 40 to 60 ℃ to obtain the mixed solution.

3. The method of claim 2, wherein the method is characterized by: The particle size of the titanium carbide powder is 1 to 30 μm, and the particle size of the nickel powder is 20 to 50 μm. The molecular weight of the gelatin is 10,000 to 100,000, and the molecular weight of the polyvinylpyrrolidone is 20,000 to 80,000. The titanium carbide powder and the nickel powder form a mixed powder; The mass ratio of the titanium carbide powder to the nickel powder is (6 to 9) to (1 to 4); The solid content of the mixed powder in the mixed suspension is 5 to 30 vol.%; The mass ratio of the mixed powder to the polyvinylpyrrolidone is 100 to (0.2 to 0.5); The gelatin is 1 to 3 wt.% of water.

4. The method of claim 1, wherein the method is characterized by: In step (1), the ultrasonic time is 10 to 45 min, and the power is 80 to 300 W; The ball milling is performed at a speed of 150 to 200 r / min for 24 to 48 h; The medium of the ball milling is a zirconium oxide grinding ball with a particle size of 1 to 5 mm; The mass ratio of the zirconium oxide grinding ball to the mixed powder of the titanium carbide powder and the nickel powder is 25 to (10 to 12.5).

5. The method of claim 1, wherein the method is characterized by: In step (1), the defoaming is performed by using a defoaming reagent n-octanol at a speed of 10 to 15 r / min for 1 to 3 h; The mass ratio of the mixed suspension to the n-octanol is 1000 to (0.1 to 0.3).

6. The method of claim 1, wherein the method is characterized by: In step (2), the temperature of the vacuum freeze drying is -50 to -70 ℃, the time is 24 to 48 h, and the vacuum degree is 0.1 to 10 Pa.

7. The method of claim 1, wherein the method is characterized by: In step (2), the sintering is performed at a temperature of 1250 to 1450 ℃ at a heating rate of 2 to 6 ℃ / min for 1 to 3 h.

8. A layered porous titanium carbide-nickel composite material prepared by the method according to any one of claims 1 to 7.

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