A TiO2 / Ni3Fe / Ti3C2T x / C aerogel

By grafting chitosan onto Ti3C2Tx nanosheets and encapsulating Ni3Fe chains to form a caterpillar-like structure, polySchiff base aerogels were grown in situ, solving the problems of complex preparation, high cost, and narrow bandwidth of existing microwave absorbing materials. This resulted in efficient and multifunctional electromagnetic wave absorption and thermal insulation performance, making it suitable for complex environments.

CN117985718BActive Publication Date: 2025-12-09NANCHANG HANGKONG UNIVERSITY
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Patent Information

Application Number
CN202410160447.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-02-05
Publication Date
2025-12-09
Estimated Expiration
2044-02-05

AI Technical Summary

Technical Problem

Existing microwave absorbing materials have complex preparation methods, high filling ratios and densities, high costs, narrow microwave absorption bandwidths, and limited functions, making them difficult to apply in complex environments.

Method used

By grafting chitosan onto Ti3C2Tx nanosheets and encapsulating Ni3Fe chains to form a caterpillar-like structure, polySchiff base aerogels were grown in situ using a carbonyl-amine condensation reaction. Finally, TiO2/Ni3Fe/Ti3C2Tx/C aerogels were prepared by pyrolysis, forming independent and dispersed micro-helical heterostructures.

Benefits of technology

It achieves lightweight and wide-bandwidth electromagnetic wave absorption performance, while also possessing radar stealth and heat insulation properties, making it suitable for complex scenarios. Furthermore, its manufacturing process is simple and low-cost, making it suitable for industrial production.

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Abstract

This invention relates to a TiO2 / Ni3Fe / Ti3C2T x / C aerogel was first induced by ethylene glycol polymerization to assemble Ni3Fe particles into microhelical Ni3Fe chains, and then etched to obtain Ti3C2T x Chitosan is grafted onto nanosheets and encapsulated with iron-nickel alloy chains to form caterpillar-like Ni3Fe / Ti3C2T. x -CS, and then cleverly utilizes the carbonyl amine condensation reaction to grow polySchiff base aerogel in situ on NFT, and finally obtains ultralight aerogel through calcination. The aerogel material of this invention not only has the advantages of ideal radar stealth, heat insulation, flame retardancy and mechanical properties, but also achieves an optimal reflection loss value of -61.6 dB at a filler ratio of 7.6 wt.%; and an effective microwave absorption bandwidth ( RL With a voltage of ≤-10 dB (8.16 GHz), it has extremely high application value in both civilian and military fields.
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Description

TECHNICAL FIELD

[0001] The application relates to a TiO2 / Ni3Fe / Ti3C2T x / C aerogel and belongs to the technical field of microwave wave-absorbing materials. BACKGROUND

[0002] Nowadays, with the accelerated development of 5G / 6G communication and wireless technology, electromagnetic wave pollution is getting worse. The military tension of some countries is rising, and national defense and security are becoming more and more important. Therefore, it is imperative to develop excellent wave-absorbing materials to solve these problems. At present, advanced wave-absorbing materials with strong absorption, wide frequency, thin thickness and low filling rate should be paid more attention to, which requires special morphological structure and synergistic effect between components.

[0003] Chinese patent "MOF-74 derivative polymer composite gel and preparation method thereof" (publication number: CN117209658A) first synthesizes Co-MOF-74 by a hydrothermal method, and then obtains MOF-74 derivatives by calcination. The obtained MOF-74 derivatives are added to an organic gel precursor solution, and the organic gel takes water and glycerol as the matrix, tetramethyl ethylenediamine as the catalyst, and the initiator potassium persulfate decomposes to generate primary free radicals and acrylamide monomers to add to form monomer radicals, thereby initiating polymerization of other monomers into chains, and chemically crosslinking with the crosslinking agent N,N-methylene bisacrylamide to finally obtain a composite gel. The method has a complex gel formation process, and the reagents used are expensive, which is difficult to form effective economic benefits and is not conducive to large-scale industrial production. Chinese patent "Natural polyphenol hydrogel with microwave absorption function and preparation method thereof" (publication number: CN116801602A) provides a relatively simple method for preparing a gel type wave-absorbing material, but due to the lack of magnetic materials, the effective wave-absorbing bandwidth is often not high, and it is difficult to realize the application of the wave-absorbing material in a more complex and variable environment. At present, the wave-absorbing material needs to be improved and further improved in terms of density, wave-absorbing intensity, effective wave-absorbing bandwidth and performance stability.

[0004] Ti3C2T x is a new member of the two-dimensional (2D) material family, and its molecular formula is M n+1 X n T x , wherein M is a transition metal, X is carbon or nitrogen, and T x is a surface group, usually -OH, -F or -O. Due to the layered structure of Ti3C2T x and its unique conductivity and hydrophilicity, Ti3C2T x is considered a strong contender for various applications, including energy storage, sensors, electromagnetic absorption and electromagnetic shielding. Therefore, in the present application, Ti3C2T xChitosan (CS) was grafted onto the nanosheets, and then the Ni3Fe chains were grafted onto Ti3C2T. x -CS encapsulation forms independent, dispersed caterpillar-like heterostructures, effectively preventing the self-stacking and oxidation of Ni3Fe chains. Then, the carbonyl-amine condensation reaction between chitosan and glutaraldehyde is cleverly utilized in the Ni3Fe / Ti3C2T... x A lightweight three-dimensional Schiff base polymer aerogel was grown in situ on a CS substrate, and finally, TiO2 / Ni3Fe / Ti3C2T was prepared by simple pyrolysis. x / C (NFTC) magnetic carbon aerogel.

[0005] Furthermore, the aerogel material obtained in this invention, under the electromagnetic synergistic effect of multidimensional and multi-component materials, forms TiO2 / Ni3Fe / Ti3C2T x / C magnetic carbon aerogel, with a filling ratio of only 7.6 wt.%, exhibits a minimum reflection loss of -61.6 dB and an effective absorption bandwidth of 8.16 GHz, demonstrating excellent microwave absorption performance with light weight and wide bandwidth. Meanwhile, the TiO2 / Ni3Fe / Ti3C2T... x Radar cross-section simulation results of / C magnetic carbon aerogel show that its radar stealth performance decreases by a maximum of 20.1 dB·m at 0°. 2 Furthermore, since this invention uses an aerogel material, it is lightweight, has a wide bandwidth, is simple to manufacture, and possesses excellent thermal insulation properties, with a thermal conductivity of 0.046 W / m·K. The aerogel material prepared by this invention combines excellent radar stealth and thermal insulation performance, can withstand 750 times its own weight, and also has certain flame-retardant properties, which greatly expands its application in complex scenarios. Summary of the Invention

[0006] This invention addresses the technical problems of existing microwave absorbing materials, such as complex preparation methods, high filling ratios and densities, high costs, narrow microwave absorption bandwidth, and limited functionality, which hinder their widespread application. It provides a TiO2 / Ni3Fe / Ti3C2T material. x A simple method for preparing / C magnetic carbon aerogel.

[0007] This invention relates to a TiO2 / Ni3Fe / Ti3C2T x / C aerogel is created by inducing Ni3Fe particles to assemble into micro-helical Ni3Fe chains through ethylene glycol polymerization, and by integrating Ti3C2T x After grafting chitosan (CS) onto nanosheets, micro-helical Ni3Fe chains are then encapsulated to form caterpillar-like Ni3Fe / Ti3C2T. x -CS(NFT), and then through a carbonyl amine condensation reaction, a polySchiff base is grown in situ on its surface to obtain Ni3Fe / Ti3C2T x / poly-Schiff base aerogel, and TiO2 / Ni3Fe / Ti3C2T x / C aerogel.

[0008] The specific process is as follows:

[0009] Step 1: Dissolve acetylacetone nickel (II) and acetylacetone iron (III) in ethylene glycol, then add N2H4·H2O dropwise into the solution, and transfer it to a stainless steel autoclave lined with polytetrafluoroethylene, and react at 140-180℃ for 8-12 h to prepare micro-spiral Ni3Fe chains;

[0010] Step 2: Dissolve LiF in hydrochloric acid solution, then add MAX (Ti3AlC2) precursor to the solution, and stir in a water bath at 35-45℃ for 22-26 h, then ultrasonic and centrifugal to obtain Ti3C2T x nanosheet dispersion solution;

[0011] Step 3: Add acetic acid to the Ti3C2T x nanosheet dispersion solution for acidification, then add chitosan (CS) to graft to the Ti3C2T x nanosheet dispersion solution, then add micro-spiral Ni3Fe chains, and further add glutaraldehyde dropwise, and stand at room temperature for 2-6 h to form a hydrogel through carbamoyl condensation reaction; then place the hydrogel in a freeze dryer, and freeze dry for 1-3 days to obtain Ni3Fe / Ti3C2T x / poly-Schiff base aerogel;

[0012] Step 4: Seal the Ni3Fe / Ti3C2T x / poly-Schiff base aerogel in a tube furnace, and heat at 600-900℃ for 2-3 h under nitrogen atmosphere, with a heating rate of 2-3 ℃ / min to obtain TiO2 / Ni3Fe / Ti3C2T -1 / C aerogel. x / C aerogel.

[0013] In step 1, the ratio of acetylacetone nickel (II), acetylacetone iron (III) and ethylene glycol in the A solution is 0.45-0.6 g: 0.2-0.35 g: 49-51 mL; and the amount of N2H4·H2O added dropwise in the B solution is 9-11 mL.

[0014] In step 2, the amount of LiF is 0.8-1.2 g, the concentration of hydrochloric acid is 8-10 mol / L, the amount of hydrochloric acid is 18-22 mL, the amount of Ti3AlC2 is 0.4-0.6 g, and the concentration of Ti3C2T x nanosheet dispersion aqueous solution in the D solution is 8-12 mg / mL.

[0015] In step 3, Ti3C2T x In the nanosheet dispersion solution D, the ratio of microspiral Ni3Fe chains to acetic acid is 0.04~0.06 g : 1.5~3 mL; in the hydrogel E, the ratio of chitosan to glutaraldehyde is 0.15~0.3 g : 1.5~3 mL.

[0016] The Ti3C2T x In the molecular formula, T is one or more of -OH, -F, and -O, and x is the total number of -OH, -F, and -O functional groups in T.

[0017] The beneficial method of the present invention:

[0018] 1. Unique preparation method: The Ni3Fe chain of this invention is coated with Ti3C2T x -CS nanosheets encapsulate the structure, forming independent, dispersed micro-helical heterostructures that effectively prevent the self-stacking and oxidation of Ni3Fe chains. Furthermore, the ingenious utilization of the carbonyl-amine condensation reaction between chitosan and glutaraldehyde in the caterpillar-like Ni3Fe / Ti3C2T structure... x A lightweight three-dimensional Schiff base polymer aerogel was grown in situ on a CS substrate, and then a uniform and stable TiO2 / Ni3Fe / Ti3C2T aerogel was prepared by drying and pyrolysis. x / C Magnetic carbon aerogel material.

[0019] 2. Excellent electromagnetic wave absorption capability: This invention, TiO2 / Ni3Fe / Ti3C2T x / C Aerogel material at 3.0 mm, optimal reflection loss value ( RL min The absorption bandwidth can reach -61.6 dB. Moreover, only 7.6 wt.% of aerogel material in the paraffin matrix can achieve an ultra-wide absorption bandwidth of 8.16 GHz, and the matching thickness is only 2.77 mm, which meets the requirements of "thin, light, wide and strong" for ideal absorbing materials. This has great potential for industrial production and application.

[0020] 3. Multi-scenario Applicability: The multi-functional properties compensate for the shortcomings of single application scenarios of materials, and the multi-functionality of materials is also a future development trend of metamaterials. At room temperature, the aerogel material of this invention was heated on a heating platform at 120°C for 50 minutes, and the highest surface temperature of the aerogel was only 41°C, demonstrating the excellent thermal insulation performance of the material. This provides a foundation for its application in harsh environments. Secondly, because the ordered arrangement of Ni3Fe magnetic particles enhances magnetic coupling and magnetic anisotropy, this greatly enhances the material's absorption of electromagnetic waves. In addition, the one-dimensional structure can act as an "antenna" to receive more incident electromagnetic waves and enter the absorbing material. Finally, Ti3C2T xThe combination of the magnetic material not only reduces the aggregation of the magnetic particles, improves the corrosion resistance, but also is beneficial to the synergy between the dielectric property and the magnetism, and further enhances the absorption of electromagnetic waves. The radar stealth performance of the aerogel material of the application has a maximum reduction of 20.1 dB·m at 0° 2 , and the thermal conductivity thereof is 0.046 W / m·K, indicating that the heat insulation property thereof is excellent. The aerogel wave-absorbing material has excellent radar stealth and heat insulation performance, and the density thereof is only 0.166 g / cm 3 , small density, can withstand 750 times of its own weight, and has certain flame retardant properties, which greatly expands its application in complex scenes.

[0021] 4. Great application prospect: the preparation process of the application is simple, the production cost is low, the compounding is uniform, which lays a solid foundation for the industrial large-scale production and commercial application of the TiO2 / Ni3Fe / Ti3C2T x / C magnetic carbon aerogel, and can provide new materials for the prevention and control of electromagnetic wave pollution and the military stealth field. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 It is a TiO2 / Ni3Fe / Ti3C2T x / C-700 multi-dimensional composite and multi-functional application schematic diagram prepared by the embodiment 1 of the application;

[0023] Figure 2 It is a colloidal phenomenon of the Ti3C2T x of the application;

[0024] Figure 3 It is a TiO2 / Ni3Fe / Ti3C2T x / C-700 physical picture of the embodiment 1 of the application;

[0025] Figure 4 It is a TiO2 / Ni3Fe / Ti3C2T x / C-700 and the embodiment 2 TiO2 / Ni3Fe / Ti3C2T x / C-800 aerogel material X-ray diffraction pattern of the application;

[0026] Figure 5 It is a scanning electron microscope image of the TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material of the embodiment 1 of the application at 5 μm;

[0027] Figure 6 It is a TiO2 / Ni3Fe / Ti3C2T xScanning electron microscope image of / C-700 aerogel material;

[0028] Figure 7 TiO2 / Ni3Fe / Ti3C2T prepared for Example 1 of the present invention x / C-700 and Example 2 TiO2 / Ni3Fe / Ti3C2T x Vibrating sample magnetometer (VSM) image of / C-800 aerogel material;

[0029] Figure 8 TiO2 / Ni3Fe / Ti3C2T prepared for Example 1 of the present invention x Microwave absorption image of / C-700 aerogel material;

[0030] Figure 9 TiO2 / Ni3Fe / Ti3C2T prepared for Example 2 of the present invention x Microwave absorption image of / C-800 aerogel material. DETAILED DESCRIPTION

[0031] Example 1

[0032] Step 1: 0.53 g of nickel (II) acetylacetonate and 0.24 g of iron (III) acetylacetonate were dissolved in 50 mL of ethylene glycol, and then 10 mL of N2H4·H2O was added dropwise to the solution. Then, the mixed solution was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and reacted at 160 °C for 10 h.

[0033] Step 2: 5 mL of deionized water was dissolved in 15 mL of concentrated hydrochloric acid (12 mol / L), and then 1.0 g of LiF was dissolved. The mixture was stirred in a water bath at 40 °C for 30 min, and then 0.5 g of Ti3AlC2 was gradually added to the above mixture and reacted for 24 h under water bath stirring. A 10 mg / mL Ti3C2T x nanosheet aqueous solution was prepared by ultrasonic treatment and centrifugation.

[0034] Step 3: 2 mL of acetic acid was added to the 10 mg / mL Ti3C2T x nanosheet aqueous solution to acidify, and then 0.2 g of chitosan was added to the above solution, ultrasonically dissolved, and then 0.05 g of Ni3Fe was added. Further, 2 mL of glutaraldehyde was added to the Ni3Fe / Ti3C2T x -CS solution, and left to stand at room temperature for 4 h to form a hydrogel. The above prepared gel was unidirectionally frozen under the action of liquid nitrogen, and then freeze-dried in a freeze dryer for 2 days to obtain a Ni3Fe / Ti3C2T x / poly-Schiff base aerogel.

[0035] Step 4: Ni3Fe / Ti3C2T x / poly-Schiff base aerogel was sealed in a tube furnace and heat treated at 700 °C for 2 h under nitrogen atmosphere with a heating rate of 2 °C min -1 , to obtain TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel.

[0036] Step 5: The prepared TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material was heated on a heating table at 120 °C for 50 min, and the temperature change of the sample was recorded every 10 min. The temperature change of the sample was recorded by an infrared thermal imager.

[0037] Step 6: A 200 g weight was placed on the prepared TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel, and the aerogel did not show any deformation.

[0038] Step 7: The TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel was directly placed on an alcohol lamp and burned for 30 s, only a small part of the aerogel showed red, and after 2 min, the red part disappeared, and the overall structure of the aerogel remained basically unchanged.

[0039] Step 8: The radar stealth performance of the TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel was simulated by computer simulation technology, and the reduction of the radar cross section area was calculated by the following formula;

[0040] ;

[0041] Step 9: The prepared TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material was immersed in melted paraffin with a base to form a ring. According to the density calculation of the aerogel, the material accounted for 7.6 wt.% of the total mass of the ring. The electromagnetic parameters of the material were measured by a vector network analyzer, and according to the transmission line theory, the reflection loss of the material to electromagnetic waves was calculated by the following equation;

[0042] ;

[0043] Example 2

[0044] Step 1: 0.53 g nickel (II) acetylacetonate and 0.24 g iron (III) acetylacetonate were dissolved in 50 mL ethylene glycol, then 10 mL N2H4·H2O was added dropwise into the solution, and then the mixed solution was transferred into a stainless steel autoclave lined with polytetrafluoroethylene and reacted at 160℃ for 10 h.

[0045] Step 2: 5 mL deionized water was dissolved in 15 mL concentrated hydrochloric acid (12 mol / L), and then 1.0 g LiF was dissolved, stirred in a water bath at 40℃ for 30 min, and then 0.5 g Ti3AlC2 was gradually added into the above mixed solution, and reacted for 24 h under water bath stirring, and then 10 mg / mL Ti3C2T x nanosheet aqueous solution was prepared by ultrasonic and centrifugal separation.

[0046] Step 3: 2 mL acetic acid was added to the 10 mg / mL Ti3C2T x nanosheet aqueous solution for acidification, and then 0.2 g chitosan was added into the above solution, ultrasonically dissolved, and then 0.05 g Ni3Fe was added, and further 2 mL glutaraldehyde was added into the Ni3Fe / Ti3C2T x -CS solution, and left to stand at room temperature for 4 h to form a hydrogel. The above prepared gel was unidirectionally frozen under the action of liquid nitrogen, and then freeze-dried in a freeze dryer for 2 days to obtain a Ni3Fe / Ti3C2T x / poly-Schiff base aerogel.

[0047] Step 4: The Ni3Fe / Ti3C2T x / poly-Schiff base aerogel was sealed in a tube furnace and heat-treated at 800℃ for 2 h under a nitrogen atmosphere, with a heating rate of 2℃ / min -1 , to obtain a TiO2 / Ni3Fe / Ti3C2T x / C-800 aerogel.

[0048] Step 5: Step 9 of Example 1 was repeated.

[0049] Specific description of the drawings

[0050] Figure 1 : Schematic diagram of multi-dimensional composite and multi-functional application of the TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material prepared in Example 1 of the present application.

[0051] The TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material is composed of zero-dimensional TiO2, one-dimensional Ni3Fe chain alloy and two-dimensional Ti3C2T xThe material is compounded. In addition, in the multifunctional test, 0.2667 g of TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material does not deform under the weight of 200 g, indicating that the material has good compression resistance; no obvious burning traces are found in the alcohol lamp open flame ignition test, showing that the material has good flame retardancy; the surface temperature of the aerogel is only 41 DEG C after heating on a heating table at 120 DEG C for 50 minutes, showing that the material has excellent thermal insulation performance.

[0052] Figure 2 The Ti3C2T x The dispersion liquid can be seen obvious Tyndall effect, show that the dispersion liquid has colloid characteristics.

[0053] Figure 3 The TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel prepared in the embodiment 1 of the present application can be placed on flowers, indicating that the aerogel has ultra-low density (0.166 g / cm 3 ).

[0054] Figure 4 The TiO2 / Ni3Fe / Ti3C2T x / C-700 (calcined at 700 DEG C) and the TiO2 / Ni3Fe / Ti3C2T x / C-800 (calcined at 800 DEG C) aerogel material of the embodiment 2 of the present application, by analyzing the X-ray diffraction spectrum of the aerogel material prepared in the embodiment, wherein the embodiment 1 mainly shows the derived peaks of A-TiO2, R-TiO2 and Ni3Fe, and only the derived peaks of R-TiO2 and Ni3Fe appear in the embodiment 2. There are almost no impurity peaks, indicating that the purity is high, the product of the present application is stable, and it is beneficial to industrial production and popularization.

[0055] Figure 5 The TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material of the embodiment 1 of the present application under 5 mu m, from the figure, it can be seen that the magnetic micro-spiral Ni3Fe chain is wrapped by Ti3C2T x , and is encapsulated in the carbon matrix.

[0056] Figure 6 The TiO2 / Ni3Fe / Ti3C2T x / C-700 aerogel material of the embodiment 1 of the present application under 100 mu m, it can be seen that the TiO2 / Ni3Fe / Ti3C2T xThe aerogel is a regular aerogel pore structure.

[0057] Figure 7 TiO2 / Ni3Fe / Ti3C2T prepared for Example 1 x TiO2 / Ni3Fe / Ti3C2T prepared for Example 2 x The VSM graph of the aerogel material of Example 1 TiO2 / Ni3Fe / Ti3C2T x The magnetic property of the aerogel of Example 1 TiO2 / Ni3Fe / Ti3C2T x The magnetic property of the aerogel of Example 2 TiO2 / Ni3Fe / Ti3C2T

[0058] Figure 8 TiO2 / Ni3Fe / Ti3C2T prepared for Example 1 x The simulated reflection loss graph of the aerogel coating of Example 1 TiO2 / Ni3Fe / Ti3C2T RL min -61.6 dB at 11.2 GHz (equivalent to microwave absorption rate, about 99.9999% of electromagnetic waves are absorbed), thickness of 3.00 mm.

[0059] Figure 9 TiO2 / Ni3Fe / Ti3C2T prepared for Example 2 x The simulated reflection loss graph of the aerogel coating of Example 2 TiO2 / Ni3Fe / Ti3C2T

[0060] Although the present application is disclosed above with preferred embodiments, it is not intended to limit the present application, and any person skilled in the art can make various modifications and modifications without departing from the spirit and scope of the present application, therefore the protection scope of the present application should be defined by the claims.

[0061] Note: This patent is supported by the National Natural Science Foundation (No. 22265021) and the China Aviation Science Foundation (No. 2020Z056056003).

Claims

1. A method for the preparation of TiO2 / Ni3Fe / Ti3C2T x / C aerogel, characterized by: The TiO2 / Ni3Fe / Ti3C2T x / C aerogel is prepared by using ethylene glycol polymerization to induce Ni3Fe particles to assemble into micro-spiral Ni3Fe chains, and Ti3C2T x nanosheets are grafted with chitosan, and then the micro-spiral Ni3Fe chains are wrapped to form caterpillar-like Ni3Fe / Ti3C2T x -CS, and then poly-Schiff base is grown in situ on the surface thereof through a carbamoylation condensation reaction to obtain Ni3Fe / Ti3C2T x / poly-Schiff base aerogel, and TiO2 / Ni3Fe / Ti3C2T x / C aerogel is prepared by calcination treatment. The specific process is as follows: Step 1: Dissolve acetylacetone nickel and acetylacetone iron in ethylene glycol, the valence of nickel and iron in the acetylacetone nickel and acetylacetone iron is divalent and trivalent, then add N2H4·H2O dropwise, and then transfer to a stainless steel autoclave lined with polytetrafluoroethylene, and react at 140-180℃ for 8-12h to obtain micro-spiral Ni3Fe chains; Step 2: Dissolve LiF in hydrochloric acid solution, then add Ti3AlC2 to it, and stir in water bath at 35-45 ℃ for 22-26 h, then obtain Ti3C2T x nanosheet dispersion solution; Step 3: In the Ti3C2T x nanosheet dispersion solution, acetic acid is added for acidification, and then chitosan is added to graft on the Ti3C2T x ; then micro-spiral Ni3Fe chains are added, and further glutaraldehyde is added dropwise, and the mixture is placed at room temperature for 2-6 h to form a hydrogel through carbamoyl condensation reaction; then the hydrogel is placed in a freeze dryer for 1-3 days to obtain a Ni3Fe / Ti3C2T x / poly-Schiff base aerogel. Step 4: Ni3Fe / Ti3C2T x / poly-Schiff base aerogel was sealed in a tube furnace, and was kept at 600-900 ℃ for 2-3 h under nitrogen atmosphere, with a heating rate of 2-3 ℃ / min -1 , to obtain TiO2 / Ni3Fe / Ti3C2T x / C aerogel.

2. A method of preparing a TiO2 / Ni3Fe / Ti3C2T x / C aerogel according to claim 1, characterized in that: In the step 1: the ratio of acetylacetone nickel, acetylacetone iron and ethylene glycol is 0.45-0.6g: 0.2-0.35g: 49-51mL; the amount of N2H4·H2O added is 9-11mL.

3. A method for preparing TiO2 / Ni3Fe / Ti3C2T x / C aerogel according to claim 1, characterized by: In the step 2, the amount of LiF is 0.8-1.2 g, the concentration of hydrochloric acid is 8-10 mol / L, the amount of hydrochloric acid is 18-22 mL, the amount of Ti3AlC2 is 0.4-0.6 g, the amount of Ti3C2T x The concentration of the nanosheet dispersion solution is 8-12 mg / mL.

4. A method for preparing TiO2 / Ni3Fe / Ti3C2T x / C aerogel according to claim 1, characterized by: In the step 3, the ratio of the use amount of micro-spiral Ni3Fe chains and acetic acid is 0.04-0.06g: 1.5-3mL; the ratio of the use amount of chitosan and glutaraldehyde is 0.15-0.3g: 1.5-3mL.

5. The preparation method of TiO2 / Ni3Fe / Ti3C2Tx / C aerogel according to claim 1, characterized in that: In the formula of Ti3C2Tx, T is one or several of -OH, -F or -O, and x is the total number of -OH, -F and -O functional groups in T.

Citation Information

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