CN110283570B - FeCo @ MXene core-shell structure composite wave-absorbing material and preparation method thereof - Google Patents
FeCo @ MXene core-shell structure composite wave-absorbing material and preparation method thereof Download PDFInfo
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- CN110283570B CN110283570B CN201910644641.3A CN201910644641A CN110283570B CN 110283570 B CN110283570 B CN 110283570B CN 201910644641 A CN201910644641 A CN 201910644641A CN 110283570 B CN110283570 B CN 110283570B
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Abstract
The material is a core-shell structure formed by coating magnetic FeCo nano particles with laminated MXene, and the mass ratio of the FeCo nano particles to the MXene is 1: 2-4; wherein MXene has a lamellar microstructure, the surface of the MXene is rich in functional groups, FeCo can be coated on the surface of the MXene to form a microscopic core-shell structure of a dielectric-magnetic two-phase heterojunction, and the MXene has an obvious dielectric polarization loss characteristic; meanwhile, the FeCo coated on the MXene surface not only has a high-frequency natural resonance effect and a strong magnetic loss mechanism, but also balances the difference between the complex dielectric spectrum and the complex magnetic conductivity spectrum of the composite material and is beneficial to matching with the space impedance, so that the material shows the wide-frequency strong electromagnetic wave absorption characteristic, and the reflectivity result shows that the bandwidth superior to-10 dB reaches 8.8 GHz.
Description
Technical Field
The invention belongs to the field of functional materials, and particularly relates to a FeCo @ MXene core-shell structure composite wave-absorbing material and a preparation method thereof.
Background
In the military field, as the radar detection technology is rapidly developed, the radar stealth technology is increasingly and closely concerned, and the adoption of the wave-absorbing material is an effective way for realizing radar stealth; in the civil field, the development of wireless communication technology and the popularization of corresponding products bring convenience to daily life of people, and meanwhile, the problems of serious electromagnetic pollution and electromagnetic interference are also generated, and the use of the wave-absorbing material is an effective means for solving the problems of electromagnetic interference and electromagnetic pollution. A large number of researches show that the high-performance wave-absorbing material simultaneously has multiple electromagnetic wave attenuation mechanisms such as dielectric loss, conductance loss, magnetic loss and the like.
MXene is a dielectric wave-absorbing material with better performance because of having a two-dimensional layered microstructure, small density, large specific surface area and large conductivity. But the single MXene phase material has no magnetic loss mechanism and limited wave absorbing performance. CN 106750277A discloses an MXene-polyaniline composite wave-absorbing material and a preparation method thereof; CN 107660114A discloses a preparation method of a molybdenum disulfide/MXene layered composite wave-absorbing material; CN 107645065A discloses a preparation method of an onion carbon/MXene layered wave-absorbing composite material. The MXene is compounded with other wave-absorbing materials, so that the wave-absorbing performance of the MXene is improved to a certain extent. However, the composite polyaniline, molybdenum disulfide and onion carbon are still dielectric wave-absorbing materials, and MXene cannot introduce a magnetic loss mechanism, so that the degree of improving the MXene wave-absorbing performance is limited.
Disclosure of Invention
The technical problem solved by the invention is as follows: the invention overcomes the defects of the prior art and provides a FeCo @ MXene core-shell structure composite wave-absorbing material and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a FeCo @ MXene core-shell structure composite wave-absorbing material is a lamellar MXene with the surface coated with magnetic FeCo nano particles.
Preferably, the mass ratio of the magnetic FeCo nanoparticles to the lamellar MXene is 1: 2-4.
The preparation method of the FeCo @ MXene core-shell structure composite wave-absorbing material comprises the following steps: uniformly dispersing bivalent iron salt, bivalent cobalt salt and lamellar MXene powder in an alcohol solvent to form a mixed solution, then sequentially adding a reducing agent and inorganic base, adjusting the pH value to 11-13, stirring and dispersing to form a reaction solution, transferring the reaction solution to a closed container, heating to 120-180 ℃, reacting for 3-6 hours, cooling to room temperature after the reaction is finished, washing, and drying to obtain the FeCo MXene core-shell structure composite wave-absorbing material.
Preferably, the ferrous salt is selected from one or more of ferrous nitrate, ferrous chloride and ferrous sulfate and hydrates of the three.
Preferably, the divalent cobalt salt is selected from one or more of cobalt nitrate, cobalt chloride and cobalt sulfate and hydrates of the three.
Preferably, the reducing agent is hydrazine hydrate. More preferably, the hydrazine hydrate and Fe in the mixed solution2+The mass ratio of (A) to (B) is 2-3: 1.
Preferably, the mass ratio of the flaky layered MXene powder to the divalent cobalt salt reduced to elemental cobalt is 1-2: 1.
Preferably, in the mixed solution, Fe2+And Co2+The mass ratio of the Co to the Co is 0.8-1.2: 12+The mass concentration of the substance(s) is 0.01-0.1 mol/L, and the Co is2+The amount concentration of the substance(s) is 0.02-0.04 mol/L.
Preferably, the alcohol organic solvent is one or both of ethanol and ethylene glycol.
Preferably, the base is an inorganic base.
Preferably, the reaction temperature is 160 ℃, and more preferably, the reaction time is 4 hours.
Preferably, the preparation method of the lamellar MXene powder comprises the following steps: adding the MAX phase powder of the transition metal carbide into hydrofluoric acid solution, stirring and reacting for 12-24h under the ultrasonic assistance effect, standing after the reaction is finished, removing supernatant, washing and precipitating, filtering, and drying to obtain lamellar MXene powder.
Preferably, the transition metal carbide MAX phase powder has a particle size of 200 meshes and is Ti3SiC2Or Ti3AlC2 。
Preferably, the hydrofluoric acid solution is 40% by mass.
The invention has the beneficial effects that:
(1) in the FeCo @ MXene core-shell structure composite wave-absorbing material provided by the invention, MXene has a lamellar microstructure, the surface of MXene is rich in functional groups, FeCo can be coated on the surface of MXene to form a dielectric-magnetic two-phase heterojunction microstructure core-shell structure, and the characteristic of obvious dielectric polarization loss is further possessed; in addition, the FeCo coated on the MXene surface not only has a high-frequency natural resonance effect and a magnetic loss mechanism, but also balances the difference between the complex dielectric spectrum and the complex permeability spectrum of the composite material and is beneficial to matching with the space impedance, so that the FeCo @ MXene core-shell structure material shows the wide-frequency strong electromagnetic wave absorption characteristic, and the reflectivity result shows that the bandwidth superior to-10 dB reaches 8.8 GHz;
(2) the preparation method provided by the invention has the advantages of mild process conditions and low production cost, and is beneficial to industrial production.
Drawings
FIG. 1 is a scanning electron micrograph of lamellar MXene in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a FeCo @ MXene core-shell structure composite wave-absorbing material prepared in example 1 of the present invention;
FIG. 3 is an electromagnetic parameter diagram of the FeCo @ MXene core-shell structure composite wave-absorbing material obtained in example 1 of the invention at a frequency band of 2-18 GHz;
FIG. 4 is a wave-absorbing performance diagram of FeCo @ MXene core-shell structure composite wave-absorbing material with different thicknesses obtained in example 1 of the invention in a frequency band of 2-18 GHz.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
Example 1
The embodiment comprises the following steps:
(1) weighing 5g of Ti3SiC2 Pouring MAX phase powder into a 500 mL polytetrafluoroethylene beaker containing 40% by mass of hydrofluoric acid solution, and magnetically stirring and reacting for 24 hours at a rotating speed of 300 r/min under the ultrasonic assistance of 40W; after the reaction is finished, standing the mixed solution for 2 hours, removing supernatant, washing the black precipitate for 3 times by using deionized water, filtering and drying at 80 ℃ in vacuum for 2 hours to obtain MXene powder, wherein the microstructure of the powder is shown in figure 1, and thus, the MXene prepared by the method disclosed by the invention is in a lamellar microstructure with uniform appearance.
(2) 2.3g of CoCl were weighed out separately2•6H2O and 2.8g FeSO4·7H2O, and dissolving in a glass flask filled with 150 mL of glycol solvent; adding the lamellar MXene powder obtained in the step (1), and magnetically stirring at the rotating speed of 300 r/min for uniform dispersion for 2h to form a mixed solution; slowly adding 10mL of 80% hydrazine hydrate solution and NaOH compound into the mixed solution, adjusting the pH value to 11, and continuously magnetically stirring and dispersing at the rotating speed of 400 r/min for 1 h to obtain reaction liquid; transferring the reaction solution into a 200mL reaction kettle containing a polytetrafluoroethylene lining, sealing, and putting the reaction solution into an air-blast drying oven to react for 4 hours at the temperature of 160 ℃ so that the generated magnetic FeCo nanoparticles are coated on the surface of lamellar MXene; finally, theWashing the black precipitate obtained by the reaction with deionized water, and drying at 80 ℃ in vacuum for 1 h to obtain the FeCo @ MXene core-shell structure composite wave-absorbing material, wherein the tested micro-morphology of the composite wave-absorbing material is shown in FIG. 2. Comparing fig. 1 and fig. 2, it can be seen that nano FeCo particles are successfully synthesized and uniformly coated on the surface of lamellar MXene, and a core-shell microstructure with FeCo particles as a shell and MXene as a core is formed.
The electromagnetic parameters (complex dielectric constant and complex permeability) of the FeCo @ MXene core-shell structure composite wave-absorbing material prepared in the example 1 of the invention are tested by using an Agilent vector network analyzer with the model number of N5230A, and the test result is shown in FIG. 3. The FeCo @ MXene core-shell structure composite wave-absorbing material has a high real part of complex dielectric constant within a frequency band of 2-18 GHzε') And imaginary part (ε") The value shows that the material has remarkable dielectric polarization loss characteristics; in addition, the existence of shell magnetic FeCo enables the composite material to obtain higher real part of complex magnetic permeability ()μ') And imaginary part (μ") The magnetic material has strong magnetic loss capability.
According to the transmission line theory, based on tested electromagnetic parameters, the wave absorbing performance of FeCo @ MXene core-shell structure composite wave absorbing material with different thicknesses is obtained, as shown in FIG. 4, it can be seen that as the thickness of the material increases, the absorption peak value moves to low frequency; when the thickness of the material is 1.6mm, the bandwidth better than-10 dB (90% absorption) reaches 8.8 GHz.
Example 2
The embodiment comprises the following steps:
(1) weighing 6gTi3AlC2Pouring MAX phase powder into a 500 mL polytetrafluoroethylene beaker containing 40% hydrofluoric acid solution, and magnetically stirring at a rotating speed of 300 r/min under the ultrasonic assistance of 60W to react for 12 h; after the reaction is finished, standing the mixed solution for 2 hours, removing supernatant, washing the black precipitate for 4 times by using deionized water, filtering, and drying for 2 hours at the temperature of 60 ℃ in vacuum to obtain lamellar MXene powder;
(2) 4.5g of CoSO were weighed out separately4•6H2O and 5.5g FeSO4·7H2O, and dissolved in a glass flask containing 150 mL of ethanol solvent, and the step of adding(1) Uniformly stirring and dispersing the obtained lamellar MXene powder for 3 hours at the rotating speed of 250 r/min by magnetic force to form a mixed solution; slowly adding 20mL of 80% hydrazine hydrate solution and NaOH compound into the mixed solution, adjusting the pH value to 13, and continuously magnetically stirring and dispersing at the rotating speed of 500 r/min for 1 h to obtain reaction liquid; and transferring the reaction liquid into a 200mL reaction kettle containing a polytetrafluoroethylene lining, sealing, placing the reaction liquid into an air-blast drying oven, reacting for 3h at the temperature of 180 ℃ to enable the generated magnetic FeCo nanoparticles to be coated on the surface of the lamellar MXene, finally washing black precipitates obtained by the reaction with deionized water, and drying for 2h at the temperature of 50 ℃ in vacuum to obtain the FeCo @ MXene core-shell structure composite wave-absorbing material.
Example 3
The embodiment comprises the following steps:
(1) weighing 8gTi3SiC2Pouring MAX phase powder into a 500 mL polytetrafluoroethylene beaker containing 40% hydrofluoric acid solution, and magnetically stirring and reacting at a rotating speed of 400 r/min for 18 h under the ultrasonic assistance of 80W; and after the reaction is finished, standing the mixed solution for 3 hours, removing a supernatant, washing the black precipitate for 5 times by using deionized water, filtering, and drying at 60 ℃ in vacuum for 3 hours to obtain MXene powder.
(2) 11.2g of Co (NO) were weighed out separately3)2•6H2O and 10.8g FeSO4·7H2Dissolving O in a glass flask filled with 150 mL of glycol solvent, adding the lamellar MXene powder obtained in the step (1), and magnetically stirring at the rotating speed of 400 r/min to uniformly disperse the mixed solution for 2 hours; slowly adding 25mL of 80% hydrazine hydrate solution and NaOH compound into the mixed solution, adjusting the pH value to 12, and continuously magnetically stirring and dispersing at the rotating speed of 400 r/min for 2h to obtain reaction liquid; transferring the reaction solution into a 200mL reaction kettle containing a polytetrafluoroethylene lining, sealing, and placing the reaction solution into an air-blast drying oven to react for 6h at the temperature of 120 ℃ so that the generated magnetic FeCo nanoparticles are coated on the surface of the lamellar MXene. And finally, washing the black precipitate obtained by the reaction with deionized water, and drying for 2h at the temperature of 60 ℃ in vacuum to obtain the FeCo @ MXene core-shell structure composite wave-absorbing material.
Claims (11)
1. The FeCo @ MXene core-shell structure composite wave-absorbing material is characterized in that the FeCo @ MXene core-shell structure composite wave-absorbing material is lamellar MXene with magnetic FeCo nano particles coated on the surface; the mass ratio of the magnetic FeCo nanoparticles to the lamellar MXene is 1: 2-4; the preparation method of the FeCo @ MXene core-shell structure composite wave-absorbing material comprises the following steps: uniformly dispersing bivalent iron salt, bivalent cobalt salt and lamellar MXene powder into an alcohol solvent to form a mixed solution, then sequentially adding a reducing agent and inorganic base, adjusting the pH value to 11-13, stirring and dispersing to form a reaction solution, transferring the reaction solution to a closed container, heating to 120-180 ℃, reacting for 3-6 hours, cooling to room temperature after the reaction is finished, washing, and drying to obtain the FeCo MXene core-shell structure composite wave-absorbing material.
2. The preparation method of the FeCo @ MXene core-shell structure composite wave-absorbing material of claim 1, comprising the following steps: uniformly dispersing bivalent iron salt, bivalent cobalt salt and lamellar MXene powder into an alcohol solvent to form a mixed solution, then sequentially adding a reducing agent and inorganic base, adjusting the pH value to 11-13, stirring and dispersing to form a reaction solution, transferring the reaction solution to a closed container, heating to 120-180 ℃, reacting for 3-6 hours, cooling to room temperature after the reaction is finished, washing, and drying to obtain the FeCo MXene core-shell structure composite wave-absorbing material.
3. The preparation method according to claim 2, wherein the ferrous salt is selected from one or more of ferrous nitrate, ferrous chloride and ferrous sulfate and their hydrates; or the divalent cobalt salt is selected from one or more of cobalt nitrate, cobalt chloride, cobalt sulfate and hydrates of the cobalt nitrate, the cobalt chloride and the cobalt sulfate.
4. The method according to claim 2, wherein the reducing agent is hydrazine hydrate.
5. The method according to claim 4, wherein the hydrazine hydrate is mixed with Fe in the mixed solution2+The mass ratio of (A) to (B) is 2-3:1。
6. the preparation method of claim 2, wherein the mass ratio of the flaky layered MXene powder to the divalent cobalt salt reduced to elemental cobalt is 2-3: 1.
7. The method according to claim 2, wherein the mixed solution contains Fe2+And Co2+The mass ratio of the Co to the Co is 0.8-1.2: 12+The amount concentration of the substance(s) is 0.01 to 0.1 mol/L.
8. The method according to claim 7, wherein the Co is contained in the mixed solution2+The amount concentration of the substance(s) is 0.02-0.04 mol/L.
9. The production method according to claim 2, wherein the base is an inorganic base; or the alcohol organic solvent is one or two of ethanol and glycol; alternatively, the reaction temperature is 160 ℃; alternatively, the reaction time is 4 h.
10. The method for preparing the layered MXene powder of any one of claims 2 to 9, wherein the layered MXene powder is prepared by: adding the MAX phase powder of the transition metal carbide into hydrofluoric acid solution, stirring and reacting for 12-24h under the ultrasonic assistance effect, standing after the reaction is finished, removing supernatant, washing and precipitating, filtering, and drying to obtain lamellar MXene powder.
11. The method of claim 10, wherein the transition metal carbide MAX phase powder has a particle size of 200 mesh, which is Ti3SiC2Or Ti3AlC2(ii) a The mass percent of the hydrofluoric acid solution is 40%.
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| CN111574958B (en) * | 2020-05-19 | 2023-03-21 | 东华大学 | Carbide MXene/SiO of core-edge structure 2 Nano-plate-shaped ultrathin microwave absorbing material |
| CN112251193A (en) * | 2020-09-25 | 2021-01-22 | 同济大学 | Composite wave-absorbing material based on MXene and metal organic framework and preparation method and application thereof |
| CN113161762A (en) * | 2021-04-15 | 2021-07-23 | 浙江理工大学 | Core-shell structure metal/sericin-based carbon nano composite wave-absorbing material and preparation method thereof |
| CN113316379B (en) * | 2021-05-26 | 2022-09-02 | 湖南工程学院 | Nano composite structure wave absorber material, preparation method and application |
| CN114478148B (en) * | 2022-01-10 | 2022-07-19 | 北京理工大学 | Blasting multi-mechanism coupling type energetic electromagnetic damage cloud cluster and preparation method and application thereof |
| CN115924984B (en) * | 2022-08-31 | 2023-11-17 | 青岛大学 | Preparation method of iron ion doped CoS2/MXene heterostructure composite material |
| CN115612388A (en) * | 2022-11-07 | 2023-01-17 | 江南大学 | FeCo @ MXene-NH 2 Preparation method of nanoparticle-doped waterborne polyurethane electromagnetic shielding coating |
| CN116769326B (en) * | 2023-05-30 | 2024-03-29 | 南昌大学 | MXene-based wave-absorbing material, preparation method and application |
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