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CN-121974406-A - Fe (Fe)3O4MXene composite material, preparation method and application

CN121974406ACN 121974406 ACN121974406 ACN 121974406ACN-121974406-A

Abstract

The invention belongs to the technical field of electromagnetic wave absorber composite materials, and relates to a Fe 3 O 4 /MXene composite material, a preparation method and application thereof. And finally, carrying out high-temperature annealing on the Fe 2 O 3 nano ring/MXene to obtain the Fe 3 O 4 nano ring/MXene composite material. The Fe 3 O 4 nano-ring/MXene composite material is prepared by adopting a hydrothermal method and a high Wen Tui fire method and taking Fe 2 O 3 nano-ring/MXene as a precursor. The special ring/sheet structure not only can break through the Snoek limit due to the nano ring with the special vortex magnetic structure, but also can improve the dielectric loss by the introduced two-dimensional dielectric material. The microwave absorption performance results indicate the possibility of practical application of the sample.

Inventors

  • LI XINGHUA
  • Bai Xiangqi
  • XING HONGNA
  • FENG JUAN
  • ZONG YAN
  • ZHU XIUHONG
  • ZHENG XINLIANG

Assignees

  • 西北大学

Dates

Publication Date
20260505
Application Date
20260310

Claims (9)

  1. 1. The preparation method of the Fe 3 O 4 /MXene composite material is characterized by comprising the following steps: preparing a few-layer MXene suspension; Preparing Fe 2 O 3 nano rings; Adding Fe 2 O 3 nano-rings into deionized water, uniformly stirring, adding a few layers of MXene suspension, continuously uniformly stirring to obtain a mixed solution, performing hydrothermal treatment on the mixed solution at the temperature of 140-200 ℃ and the pressure of 0.2-0.6 MPa, and washing and vacuum drying after the reaction is finished to obtain a Fe 2 O 3 nano-ring/MXene precursor; Performing high-temperature thermal annealing treatment on the Fe 2 O 3 nano-ring/MXene precursor in a mixed atmosphere of H 2 /Ar to obtain a Fe 3 O 4 nano-ring/MXene composite material; Wherein the mass ratio of the Fe 2 O 3 nano-ring to the few-layer MXene in the few-layer MXene suspension is 2-12:1.
  2. 2. The method of preparing a Fe 3 O 4 /MXene composite according to claim 1, wherein the preparation of the few layer MXene suspension is as follows: Adding LiF into an HCl solution, heating and stirring at 35-50 ℃, and reacting for 1-3 hours to prepare an HF solution; Adding MAX into HF solution, heating and stirring at 40-50 ℃ for reaction for 30-60 hours, centrifugally washing with HCl solution and deionized water in sequence until the solution is neutral after the reaction is finished, carrying out ice bath ultrasonic and centrifugal treatment on the washed solution under the protection of argon, and taking the supernatant of the centrifuged solution as a few-layer MXene suspension, wherein the concentration of MXene in the few-layer MXene suspension is 5-15 mg/mL, and the mass ratio of LiF to MAX is 2:1.
  3. 3. The method for preparing the Fe 3 O 4 /MXene composite material according to claim 2, wherein the molar concentration of the HCl solution is 8 mol/L-10 mol/L, the mass-volume ratio of LiF to the HCl solution is 1:15-25, and the mass-volume ratio of MAX to the HF solution is 1:30-50.
  4. 4. The method for preparing the Fe 3 O 4 /MXene composite material according to claim 1, wherein the preparation step of the Fe 2 O 3 nanoring is: Sequentially adding FeCl 3 ·6H 2 O、Na 2 SO 4 and NaH 2 PO 4 into deionized water, uniformly stirring, carrying out hydrothermal reaction at 180-230 ℃ for 30-60 h, obtaining a precipitate after the reaction is finished, washing the precipitate, and drying in vacuum to obtain a brownish red precursor which is Fe 2 O 3 nano-ring, wherein the millimole volume ratio of FeCl 3 ·6H 2 O、Na 2 SO 4 , naH 2 PO 4 and deionized water is 1:0.03-0.04:0.003-0.01.
  5. 5. The method for preparing the Fe 3 O 4 /MXene composite material according to claim 1, wherein the volume ratio of H 2 to Ar in the H 2 /Ar mixed atmosphere is 10:90, and the gas amount of the H 2 /Ar mixed gas is 50 sccm-200 sccm.
  6. 6. The method for preparing the Fe 3 O 4 /MXene composite material according to claim 1, wherein the annealing temperature in the high-temperature thermal annealing treatment is 400-450 ℃, and the heating rate of the high-temperature annealing treatment is 1-5 ℃.
  7. 7. The method for preparing Fe 3 O 4 /MXene composite according to claim 1, wherein, The concentration of the Fe 2 O 3 nano ring in the mixed solution is 0.9 mg/mL-1.2 mg/mL.
  8. 8. The Fe 3 O 4 /MXene composite material prepared by the method for preparing the Fe 3 O 4 /MXene composite material according to any one of claims 1-7.
  9. 9. The use of the Fe 3 O 4 /MXene composite according to claim 8 for electromagnetic wave absorption in 0.1 GHz-18 GHz.

Description

Fe 3O4/MXene composite material, preparation method and application Technical Field The invention belongs to the technical field of electromagnetic wave absorber composite materials, and particularly relates to a Fe 3O4/MXene composite material, a preparation method and application thereof. Background In order to solve the problem of electromagnetic wave radiation pollution caused by the use of excessive electronic equipment, microwave absorbing materials (wave absorbing materials for short) are often adopted to convert excessive electromagnetic waves into heat energy or other forms of energy to be dissipated. Along with the development and the demand of scientific technology, the requirements on the novel microwave absorbing material are also higher and higher, namely, the absorbing thickness is thin, the weight is light, the absorbing frequency range is wide, the absorbing efficiency is high, the filling ratio is low, the high temperature resistance and the oxidation resistance are realized, and the like. However, the conventional wave-absorbing material cannot meet the conditions, and it is important to develop a novel material or adjust the micro-nano structure of the material. As the simplest ferrite, fe 3O4 has the advantages of high curie temperature, low cost, simple preparation, good chemical stability, and the like, and has been widely studied. However, under the limit of Snoek,Is the complex magnetic permeability of the material,Is the frequency at which the frequency is to be determined,Is the gyromagnetic ratio of the magnetic resonance imaging device,Saturation magnetization), the natural resonant frequency of Fe 3O4 is in the MHz range, and its complex permeability drops sharply with increasing frequency, limiting the application in the GHz region. In particular, how to achieve high-efficiency microwave absorption performance with a small absorber thickness and a wide effective absorption width remains a challenge for Fe 3O4. In general, there are two methods for enhancing the microwave absorption performance of Fe 3O4, one is to adjust the anisotropy of the magnetic field by introducing shape anisotropy, although the high-frequency magnetism of the magnetic material is improved to some extent, the regulation of the high-frequency dielectric performance cannot be realized, and the magnetic material is easy to aggregate due to the strong magnetic interaction of the magnetic material, and the other is to combine the ferromagnetic Fe 3O4 with the dielectric material to form a multifunctional magnetic/electric double-loss composite material, while the controllable regulation of the high-frequency dielectric performance is realized, the aggregation of the magnetic material is reduced, but the introduction of the dielectric material can reduce the high-frequency magnetism of the magnetic material, thereby affecting the impedance matching and the wave absorbing performance thereof. Based on the above, a Fe 3O4/MXene composite material, a preparation method and application thereof are provided for solving the problems. Disclosure of Invention Aiming at the defects of the prior art, the invention aims to provide the Fe 3O4/MXene composite material, the preparation method and the application thereof, wherein the Fe 3O4 nano ring and the MXene are compounded by a hydrothermal-high Wen Tui fire method, so that the regulation and control of high-frequency dielectric property are realized, the high-frequency magnetism is improved, the agglomeration of magnetic materials is reduced, the influence of the component ratio of the Fe 3O4 nano ring and the MXene in the composite material on the microwave absorption property is researched, on one hand, the magnetic anisotropy is regulated to improve the magnetic loss property, and on the other hand, the defect of weak dielectric loss capacity of Fe 3O4 is overcome, and the wave absorption property of Fe 3O4 is realized. In order to solve the technical problems, the invention provides a preparation method of a Fe 3O4/MXene composite material, which comprises the following steps: preparing a few-layer MXene suspension; Preparing Fe 2O3 nano rings; Adding Fe 2O3 nano-rings into deionized water, uniformly stirring, adding a few layers of MXene suspension, continuously uniformly stirring to obtain a mixed solution, performing hydrothermal treatment on the mixed solution at the temperature of 140-200 ℃ and the pressure of 0.2-0.6 MPa, and washing and vacuum drying after the reaction is finished to obtain a Fe 2O3 nano-ring/MXene precursor; Performing high-temperature thermal annealing treatment on the Fe 2O3 nano-ring/MXene precursor in a mixed atmosphere of H 2/Ar to obtain a Fe 3O4 nano-ring/MXene composite material; Wherein the mass ratio of the Fe 3O4 nano-ring to the few-layer MXene in the few-layer MXene suspension is 2-12:1. The mass ratio of the Fe 3O4 nanoring to the few-layer MXene in the few-layer MXene suspension is limited to 2-12:1, because the proportion