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CN110283570A - A kind of FeCo@MXene core-shell structure composite wave-suction material and preparation method thereof - Google Patents

A kind of FeCo@MXene core-shell structure composite wave-suction material and preparation method thereof Download PDF

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Publication number
CN110283570A
CN110283570A CN201910644641.3A CN201910644641A CN110283570A CN 110283570 A CN110283570 A CN 110283570A CN 201910644641 A CN201910644641 A CN 201910644641A CN 110283570 A CN110283570 A CN 110283570A
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mxene
feco
core
shell structure
preparation
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CN110283570B (en
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贺君
颜铄清
邓永和
陈桥
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Hunan Institute of Engineering
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Abstract

A kind of FeCo MXene core-shell structure composite wave-suction material and preparation method thereof, the material are the core-shell structures formed by magnetic Fe Co nano particle cladding sheet MXene, and the mass ratio of the FeCo nano particle and MXene are 1:2 ~ 4;Wherein, MXene has sheet microstructure, and surface is rich in functional group, and FeCo can be made to be coated on the surface MXene, forms the microcosmic core-shell structure of dielectric-magnetism two-phase hetero-junctions, has significant dielectric polarization loss characteristics;Simultaneously, the FeCo for being coated on the surface MXene not only has high-frequency natural resonance effects and strong magnetic loss mechanism, and balance the difference between the multiple dielectric and magnetic of composite material and Complex Permeability Spectrum, conducive to the matching with space impedance, therefore, the material shows wideband strong electromagnetic wave absorption characteristic, and reflectivity results show its bandwidth better than -10dB up to 8.8GHz.

Description

A kind of FeCo@MXene core-shell structure composite wave-suction material and preparation method thereof
Technical field
The invention belongs to field of functional materials, and in particular to a kind of FeCo@MXene core-shell structure composite wave-suction material and its Preparation method.
Background technique
In military field, as the radar exploration technique develops by leaps and bounds, radar stealth technology is increasingly subject to pay close attention to, and adopts It is the effective way for realizing radar invisible with absorbing material;In civil field, the development of wireless communication technique and corresponding product It is universal, while offering convenience to people's daily life, serious electromagnetic pollution and electromagnetic interference problem are also produced, suction is used Wave material is the effective means for solving electromagnetic interference and electromagnetic pollution.Numerous studies have shown that high-performance wave-absorbing material should be same When there is dielectric loss, conductance loss and the multiple electromagnetic wave attenuation mechanism such as magnetic loss.
MXene is big because having small two-dimensional layer microstructure, density, large specific surface area and conductivity, be a kind of performance compared with Good dielectric type absorbing material.But for single MXene phase material without magnetic loss mechanism, absorbing property is limited.CN 106750277 A discloses a kind of MXene- polyaniline compound wave-absorbing material and preparation method thereof;107660114 A of CN discloses a kind of two sulphur Change molybdenum/MXene lamellar composite absorbing material preparation method;107645065 A of CN discloses a kind of onion carbon/MXene layers The preparation method of shape Wave suction composite material.Above by the way that MXene and other absorbing materials is compound, improve to a certain extent The absorbing property of MXene.But compound polyaniline, molybdenum disulfide and onion carbon is still dielectric type absorbing material, can not be made MXene introduces magnetic loss mechanism, therefore, improves the limitation of MXene absorbing property.
Summary of the invention
Technical problem solved by the invention is: overcome the deficiencies in the prior art, and the present invention provides a kind of FeCo@MXene Core-shell structure composite wave-suction material and preparation method thereof, which has multiple electromagnetic wave attenuation mechanism, to incoming electromagnetic wave table Reveal the strong absorption characteristic of wideband.
The technical solution used to solve the technical problems of the present invention is that: a kind of FeCo@MXene core-shell structure composite wave-absorbing material Material, is the sheet MXene of surface coated magnetic FeCo nano particle.
Preferably, the mass ratio of above-mentioned magnetic Fe Co nano particle and sheet MXene are 1:2 ~ 4.
The preparation method of FeCo@MXene core-shell structure composite wave-suction material of the present invention, comprising the following steps: by ferrous iron Salt and divalent cobalt and sheet MXene powder are dispersed in alcohols solvent and form mixed liquor, then sequentially add reduction Agent and inorganic base adjust pH value to 11 ~ 13, are dispersed with stirring to form reaction solution, the reaction solution is transferred to closed container, heat up It is cooled to room temperature after the reaction was completed to 120-180 DEG C of reaction 3-6h, washs, be dried to obtain the FeCo@MXene core-shell structure Composite wave-suction material.
Preferably, in hydrate of the divalent iron salt selected from ferrous nitrate, frerrous chloride and ferrous sulfate and three It is one or more.
Preferably, the divalent cobalt is selected from one of cobalt nitrate, cobalt chloride and cobaltous sulfate and the hydrate of three Or it is a variety of.
Preferably, the reducing agent is hydrazine hydrate.More preferably, the hydrazine hydrate and Fe in the mixed liquor2+Object The amount ratio of matter is 2 ~ 3:1.
Preferably, the mass ratio that the sheet MXene powder and the divalent cobalt are reduced to simple substance cobalt is 1 ~ 2: 1。
Preferably, in the mixed liquor, Fe2+And Co2+The mass ratio of the material be 0.8 ~ 1.2:1, the Co2+Substance Amount concentration is 0.01 ~ 0.1mol/L, the Co2+Substance withdrawl syndrome be 0.02 ~ 0.04 mol/L.
Preferably, the alcohol organic solvent is one or two kinds of in ethyl alcohol and ethylene glycol.
Preferably, the alkali is inorganic base.
Preferably, the reaction temperature is 160 DEG C, and more preferably, the reaction time is 4h.
Preferably, the sheet MXene powder the preparation method is as follows: transition metal carbide MAX phase powder is added Enter in hydrofluoric acid solution, 12 are stirred to react under ultrasonic wave added effect ~ for 24 hours, it after the reaction was completed, stands, removes supernatant, washing is heavy It forms sediment, filtering is dried to obtain sheet MXene powder.
Preferably, the transition metal carbide MAX phase powder diameter is 200 mesh, is Ti3SiC2Or Ti3AlC2
Preferably, the mass percent of the hydrofluoric acid solution is 40%.
The beneficial effects of the present invention are:
(1) in FeCo@MXene core-shell structure composite wave-suction material provided by the invention, MXene has sheet microstructure, Its surface is rich in functional group, and FeCo can be made to be coated on the surface MXene, forms the microcosmic nucleocapsid knot of dielectric-magnetism two-phase hetero-junctions Structure, and then have significant dielectric polarization loss characteristics;In addition, the FeCo for being coated on the surface MXene is not only total with high-frequency natural Effect of shaking and magnetic loss mechanism, and the difference between the multiple dielectric and magnetic of composite material and Complex Permeability Spectrum is balanced, it is conducive to With the matching of space impedance, therefore, FeCo@MXene Core-shell structure material shows wideband strong electromagnetic wave absorption characteristic, reflectivity The result shows that its bandwidth better than -10dB reaches 8.8GHz;
(2) preparation method provided by the invention, process conditions are mild, and production cost is low, are conducive to industrialized production.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the sheet MXene in the embodiment of the present invention 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of FeCo@MXene core-shell structure composite wave-suction material prepared by the embodiment of the present invention 1;
Fig. 3 is that 1 gained FeCo@MXene core-shell structure composite wave-suction material of the embodiment of the present invention is joined in the electromagnetism of 2 ~ 18GHz frequency range Number figure;
Fig. 4 is the FeCo@MXene core-shell structure composite wave-suction material of 1 gained different-thickness of the embodiment of the present invention in 2 ~ 18GHz frequency The absorbing property figure of section.
Specific embodiment
The present invention is further detailed with attached drawing with reference to embodiments.
Embodiment 1
The present embodiment the following steps are included:
(1) 5gTi is weighed3SiC2 MAX phase powder pours into the 500 mL polytetrafluoros for filling that mass fraction is 40% hydrofluoric acid solution In ethylene beaker, and 24 h are reacted with 300 r/min revolving speed magnetic agitations under the ultrasonic wave added effect that power is 40 W;To anti- After answering, supernatant is removed after above-mentioned mixed liquor is stood 2h, then makes to be washed with deionized black precipitate 3 times, then It filters and obtains MXene powder after 80 DEG C of 2 h of drying of vacuum, test powders microscopic appearance is as shown in Figure 1, it is seen then that system of the present invention The uniform sheet microstructure of pattern is presented in standby MXene.
(2) 2.3g CoCl is weighed respectively2•6H2O and 2.8g FeSO4·7H2O, and be dissolved in equipped with 150 mL ethylene glycol In the glass flask of solvent;The sheet MXene powder that step (1) obtains is added, and equal with 300 r/min revolving speed magnetic agitations Even dispersion 2h forms mixed liquor;It is slowly added to the hydrazine hydrate solution and NaOH compound of 10mL concentration 80% into mixed liquor, adjusts Its pH value continues to obtain reaction solution with 400 r/min revolving speed magnetic agitations dispersion, 1 h to 11;Reaction solution is transferred to containing polytetrafluoro It in the 200mL reaction kettle of ethylene liner and seals, and is put into air dry oven the magnetic for making to generate with 160 DEG C of 4 h of thermotonus Property FeCo nano particle is coated on the surface of sheet MXene;Finally reaction gained black precipitate is made to be washed with deionized water It washs, after 80 DEG C of 1 h of drying of vacuum, obtains the FeCo@MXene core-shell structure composite wave-suction material, the microscopic appearance of test As shown in Figure 2.Pass through comparison diagram 1 and Fig. 2, it is seen then that nanometer Fe Co particle is successfully synthesized and is uniformly coated on sheet The surface MXene, being formed using FeCo particle is shell and using MXene as the nucleocapsid microstructure of core.
The FeCo@of the preparation of present example 1 is tested using the vector network analyzer of Agilent model N5230A MXene core-shell structure composite wave-suction material electromagnetic parameter (complex dielectric permittivity and complex permeability), test results are shown in figure 3.It can Know, FeCo@MXene core-shell structure composite wave-suction material have in 2 ~ 18GHz frequency range high complex dielectric permittivity real part (ε') and it is empty Portion (ε") value, show that it has significant dielectric polarization loss characteristic;In addition, the presence of shell magnetic Fe Co makes composite material Obtain higher complex permeability real part (μ') and imaginary part (μ") value, have strong magnetic loss ability.
According to transmission line theory, it is multiple to obtain different-thickness FeCo@MXene core-shell structure for the electromagnetic parameter based on test The absorbing property of absorbing material is closed, as shown in Figure 4, it is seen then that as material thickness increases, absorption peak is mobile toward low frequency;Work as material Material with a thickness of 1.6mm when, better than -10dB(90% absorb) bandwidth reach 8.8GHz.
Embodiment 2
The present embodiment the following steps are included:
(1) 6gTi is weighed3AlC2MAX phase powder pours into the 500 mL polytetrafluoroethylene (PTFE) for filling that concentration is 40% hydrofluoric acid solution In beaker, and 12 h are reacted with 300 r/min revolving speed magnetic agitations under the ultrasonic wave added effect that power is 60 W;Wait react knot Shu Hou removes supernatant after above-mentioned mixed liquor is stood 2h, then makes to be washed with deionized black precipitate 4 times, refilter And sheet MXene powder is obtained after 60 DEG C of 2 h of drying of vacuum;
(2) 4.5g CoSO is weighed respectively4•6H2O and 5.5g FeSO4·7H2O, and be dissolved in equipped with 150 mL alcohol solvents In glass flask, the sheet MXene powder that step (1) obtains is added, and evenly dispersed with 250 r/min revolving speed magnetic agitations 3h forms mixed liquor;It is slowly added to the hydrazine hydrate solution and NaOH compound of 20mL concentration 80% into mixed solution, adjusts its pH To 13, continue to obtain reaction solution with 500 r/min revolving speed magnetic agitations dispersion, 1 h;Reaction solution is transferred to containing in polytetrafluoroethylene (PTFE) It in the 200mL reaction kettle of lining and seals, and is put into air dry oven the magnetic Fe Co for making to generate with 180 DEG C of 3 h of thermotonus Nano particle is coated on the surface of sheet MXene, finally makes to be washed with deionized by reaction gained black precipitate, vacuum After 50 DEG C of 2 h of drying, the FeCo@MXene core-shell structure composite wave-suction material is obtained.
Embodiment 3
The present embodiment the following steps are included:
(1) 8gTi is weighed3SiC2MAX phase powder pours into the 500 mL polytetrafluoroethylene (PTFE) for filling that concentration is 40% hydrofluoric acid solution In beaker, and 18 h are reacted with 400 r/min revolving speed magnetic agitations under the ultrasonic wave added effect that power is 80 W;Wait react knot Shu Hou removes supernatant after above-mentioned mixed liquor is stood 3h, then makes to be washed with deionized black precipitate 5 times, refilter And MXene powder is obtained after 60 DEG C of 3 h of drying of vacuum.
(2) 11.2g Co (NO is weighed respectively3)2•6H2O and 10.8g FeSO4·7H2O, and be dissolved in equipped with 150 mL second In the glass flask of diol solvent, the sheet MXene powder that step (1) obtains is added, and stir with 400 r/min revolving speed magnetic force Mix the mixed liquor of evenly dispersed 2h;The hydrazine hydrate solution and NaOH compound of 25mL concentration 80% are slowly added into mixed solution, Its pH to 12 is adjusted, continues to obtain reaction solution with 400 r/min revolving speed magnetic agitations dispersion, 2 h;Reaction solution is transferred to containing poly- four It in the 200mL reaction kettle of vinyl fluoride liner and seals, and is put into air dry oven with 120 DEG C of 6 h of thermotonus, make generation Magnetic Fe Co nano particle is coated on the surface of sheet MXene.Reaction gained black precipitate is finally used into deionized water It washs, after 60 DEG C of 2 h of drying of vacuum, obtains the FeCo@MXene core-shell structure composite wave-suction material.

Claims (10)

1. a kind of FeCo@MXene core-shell structure composite wave-suction material, which is characterized in that the FeCo@MXene core-shell structure is multiple Close the sheet MXene that absorbing material is surface coated magnetic FeCo nano particle.
2. FeCo@MXene core-shell structure composite wave-suction material according to claim 1, which is characterized in that the magnetism The mass ratio of FeCo nano particle and sheet MXene are 1:2 ~ 4.
3. the preparation method of FeCo@MXene core-shell structure composite wave-suction material as claimed in claim 1 or 2, comprising the following steps: By divalent iron salt, divalent cobalt and sheet MXene powder it is evenly dispersed with alcohols solvent in form mixed liquor, then successively plus Enter reducing agent and inorganic base, adjusts pH value to 11 ~ 13, be dispersed with stirring to form reaction solution, the reaction solution is transferred to closed appearance Device is warming up to 120-180 DEG C of reaction 3-6h and is cooled to room temperature after the reaction was completed, washing, dry the FeCo@MXene core Shell structure composite wave-suction material.
4. preparation method according to claim 3, which is characterized in that the divalent iron salt is selected from ferrous nitrate, protochloride One of iron and ferrous sulfate and the hydrate of three are a variety of;Preferably, the divalent cobalt is selected from cobalt nitrate, chlorination One of cobalt and cobaltous sulfate and the hydrate of three are a variety of.
5. preparation method according to claim 3 or 4, which is characterized in that the reducing agent is hydrazine hydrate;It is more highly preferred to , Fe in the hydrazine hydrate and the mixed liquor2+The mass ratio of the material be 2 ~ 3:1.
6. according to the described in any item preparation methods of claim 3-5, which is characterized in that the sheet MXene powder and institute Stating divalent cobalt and being reduced to the mass ratio of simple substance cobalt is 2 ~ 3:1.
7. according to the described in any item preparation methods of claim 3-6, which is characterized in that in the mixed liquor, Fe2+And Co2+'s The mass ratio of the material is 0.8 ~ 1.2:1, the Co2+Substance withdrawl syndrome be 0.01 ~ 0.1mol/L, more preferably, the Co2 +Substance withdrawl syndrome be 0.02 ~ 0.04mol/L.
8. according to the described in any item preparation methods of claim 3-7, which is characterized in that the alkali is inorganic base;Preferably, institute It is one or two kinds of in ethyl alcohol and ethylene glycol for stating alcohol organic solvent;More preferably, the reaction temperature is 160 DEG C;More Preferably, the reaction time is 4h.
9. according to the described in any item preparation methods of claim 3-8, which is characterized in that the system of the sheet MXene powder Preparation Method is as follows: transition metal carbide MAX phase powder being added in hydrofluoric acid solution, is stirred to react under ultrasonic wave added effect 12-24h is stood after the reaction was completed, removes supernatant, washing precipitating, and filtering is dried to obtain sheet MXene powder.
10. preparation method described in -9 according to claim 1, which is characterized in that the transition metal carbide MAX phase powder grain Diameter is 200 mesh, is Ti3SiC2Or Ti3AlC2;The mass percent of the hydrofluoric acid solution is 40%.
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Cited By (10)

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CN111574958A (en) * 2020-05-19 2020-08-25 东华大学 Carbide MXene/SiO of core-edge structure2Nano-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
CN113316379A (en) * 2021-05-26 2021-08-27 湖南工程学院 Nano composite structure wave absorber material, preparation method and application
CN114478148A (en) * 2022-01-10 2022-05-13 北京理工大学 Explosive multi-mechanism coupling type energetic electromagnetic damage cloud cluster and preparation method and application thereof
CN114552231A (en) * 2022-01-24 2022-05-27 华南理工大学 Ferrite-manganese oxide-MXene composite wave-absorbing particle and preparation method and application thereof
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
CN115924984A (en) * 2022-08-31 2023-04-07 青岛大学 Preparation method of iron ion doped CoS2/MXene heterostructure composite material
CN117603654A (en) * 2023-11-28 2024-02-27 中国人民解放军陆军工程大学 Two-dimensional FeCoNi@MoS 2 Nano-structure electromagnetic wave absorbing material and preparation method thereof
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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CN108633242A (en) * 2018-04-11 2018-10-09 西安工程大学 A kind of titanium carbon/nickle composite powder radio-radar absorber and preparation method
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CN107418511A (en) * 2017-05-25 2017-12-01 大连理工大学 The preparation method of FeCo/ redox graphene composite wave-suction materials
CN108633242A (en) * 2018-04-11 2018-10-09 西安工程大学 A kind of titanium carbon/nickle composite powder radio-radar absorber and preparation method
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Cited By (13)

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Publication number Priority date Publication date Assignee Title
CN111574958A (en) * 2020-05-19 2020-08-25 东华大学 Carbide MXene/SiO of core-edge structure2Nano-plate-shaped ultrathin microwave absorbing material
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
CN113316379A (en) * 2021-05-26 2021-08-27 湖南工程学院 Nano composite structure wave absorber material, preparation method and application
CN114478148A (en) * 2022-01-10 2022-05-13 北京理工大学 Explosive multi-mechanism coupling type energetic electromagnetic damage cloud cluster and preparation method and application thereof
CN114552231A (en) * 2022-01-24 2022-05-27 华南理工大学 Ferrite-manganese oxide-MXene composite wave-absorbing particle and preparation method and application thereof
CN115924984A (en) * 2022-08-31 2023-04-07 青岛大学 Preparation method of iron ion doped CoS2/MXene heterostructure composite material
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
CN117603654A (en) * 2023-11-28 2024-02-27 中国人民解放军陆军工程大学 Two-dimensional FeCoNi@MoS 2 Nano-structure electromagnetic wave absorbing material and preparation method thereof

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