CN111410935A - MoS2-Fe3O4-graphene ternary composite wave-absorbing material and preparation method thereof - Google Patents
MoS2-Fe3O4-graphene ternary composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of wave-absorbing materials and discloses a MoS2‑Fe3O4The graphene ternary composite wave-absorbing material comprises the following formula raw materials and components: aminated graphene aerogel, ferric chloride, urea, surfactant and nano MoS2Hollow microspheres. The MoS2‑Fe3O4The-graphene ternary composite wave-absorbing material is an aminated graphene aerogel covalently grafted by tetraethylenepentamine, has a three-dimensional network structure and a large specific surface area, and a large number of amino and imino groups are opposite to Fe3+Has strong adsorption effect, and the generated three-dimensional porous Fe in the shape of nanometer flowers3O4Uniformly growing in the matrix surface and lamellar structure of graphene aerogel, nano MoS2Hollow microsphere and three-dimensional porous Fe in nanometer flower shape3O4The modified graphene is compounded, has a three-dimensional conductive network, an interface polarization effect and good magnetic property, and endows the composite material with good electricityThe resistance loss and the magnetic loss performance enhance the impedance matching performance of the composite material under the synergistic action.
Description
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a MoS2-Fe3O4-graphene ternary composite wave-absorbing material and a preparation method thereof.
Background
Electromagnetic waves are electromagnetic energy with electromagnetic radiation characteristics, including radio waves, microwaves, infrared rays, visible light, ultraviolet rays and the like, with the development of industry, electromagnetic pollution is ubiquitous around people, mainly electromagnetic radiation can affect normal working operations of mobile phone network signals, aircraft navigation systems, medical equipment and the like, such as free radiation, non-free radiation with thermal effect, non-free radiation without thermal effect and base station electromagnetic wave which are not free radiation waves, and human bodies are damaged to immune systems, cardiovascular systems, reproductive systems and the like of human bodies through thermal effect, non-thermal effect, accumulation effect and the like after being contacted with electromagnetic radiation for a long time, so that diseases such as immune system reduction, metabolism disorder and the like are caused, and therefore, development of materials with electromagnetic shielding, absorption and attenuation electromagnetic waves becomes a research hotspot.
The existing wave-absorbing materials mainly comprise carbon-series wave-absorbing materials such as graphene, carbon nanotubes and the like; ceramic-based wave-absorbing materials such as silicon carbide and the like; iron-based wave-absorbing material such as ferrite, etc., wherein the nano Fe3O4Good magnetism, less pollution, low price and easy obtaining, can absorb and lose electromagnetic waves through magnetic loss, is a wave-absorbing material widely applied, but only depends on Fe3O4The magnetic loss of the impedance ligand is difficult to reach, and the electromagnetic wave can not be lost under a wide frequency band.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a MoS2-Fe3O4-graphene ternary composite wave-absorbing material and preparation method thereof, solving problem of Fe3O4The impedance matching performance of the wave-absorbing material is poor.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: MoS2-Fe3O4The graphene ternary composite wave-absorbing material comprises the following raw materials and components: aminated graphene aerogel, ferric chloride, urea, surfactant and nano MoS2The hollow microspheres comprise aminated graphene aerogel, ferric chloride, urea and a surfactant in a mass ratio of 6-15:100:200-400: 180-300.
Preferably, the surfactant is tetrabutylammonium bromide.
Preferably, the preparation method of the aminated graphene aerogel is as follows:
(1) adding a graphene oxide aqueous solution with the mass fraction of 2-4% into a reaction bottle, adding tetraethylenepentamine after uniform ultrasonic dispersion, pouring the solution into a micro reaction kettle, placing the micro reaction kettle into a reaction kettle heating box, heating to 160-180 ℃, reacting for 10-15h, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, freeze-drying and grinding into fine powder to prepare the aminated graphene aerogel.
Preferably, the mass ratio of the graphene oxide to the triethylene tetramine is 1: 1.5-2.5.
Preferably, the reation kettle heating cabinet includes the inside both sides fixedly connected with rotary device of box, box inside below fixedly connected with heating device, box, and the inside swing joint of rotary device has swivel bearing, swivel bearing and rotary rod swing joint, and rotary rod fixed connection reation kettle case, the inside miniature reation kettle that is provided with of reation kettle incasement.
Preferably, the nano MoS2The preparation method of the hollow microsphere comprises the following steps:
(1) adding a mixed solvent of distilled water and ethanol into a reaction bottle, wherein the volume ratio of the distilled water to the ethanol is 8-12:1, adding manganese sulfate and ammonium bicarbonate with the mass ratio of 1:5-6, placing the mixture into a constant-temperature water bath kettle, heating the mixture to 40-60 ℃, reacting for 8-12h, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, and fully drying to obtain the nano MnCO3And (3) microspheres.
(2) Adding distilled water solvent and nano MnCO into a reaction bottle3Adding sodium molybdate and L-cysteine after uniform ultrasonic dispersion of microspheres, pouring the solution into a micro reaction kettle after uniform stirring, placing the solution into a reaction kettle heating box, heating to 200-2Hollow microspheres.
Preferably, the nano MnCO3The mass ratio of the microspheres to the sodium molybdate to the L-cysteine is 0.5-0.8:1: 3-4.
Preferably, the MoS2-Fe3O4The preparation method of the-graphene ternary composite wave-absorbing material comprises the following steps:
aminated graphene aerogel, ferric chloride, urea, surfactant and nano MoS2The hollow microspheres are prepared by the following steps of,
(1) adding an ethylene glycol solvent, aminated graphene aerogel and ferric chloride into a reaction bottle, after uniform ultrasonic dispersion, placing the reaction bottle in an oil bath, heating to 35-55 ℃, uniformly stirring for 4-10h, adding urea and a surfactant tetrabutylammonium bromide, heating to 190-3O4Modifying graphene.
(2) Adding distilled water solvent and three-dimensional porous Fe into a reaction bottle3O4Modified graphene and nano MoS2After the hollow microspheres are uniformly dispersed by ultrasonic, pouring the solution into a micro reaction kettle, placing the micro reaction kettle in a reaction kettle heating box, heating to 120 ℃, reacting for 2-5h, filtering the solution to remove the solvent, and drying to obtain the MoS2-Fe3O4-graphene ternary composite wave-absorbing material.
Preferably, the three-dimensional porous Fe3O4Modified graphene and nano MoS2The mass ratio of the hollow microspheres is 2.5-4: 1.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the MoS2-Fe3O4The graphene ternary composite wave-absorbing material is prepared by performing nucleophilic substitution reaction and amidation reaction on epoxy groups and carboxyl groups in a nucleophilic reagent tetraethylenepentamine and graphene oxide, and simultaneously performing strong pi-pi stacking action between graphene oxide lamella layers to prepare the tetraene pentamine covalent grafted aminated graphene aerogel, wherein the graphene aerogel has a three-dimensional network structure and large specific surface area, and a large number of amino groups and imino groups are uniformly dispersed in a matrix of the graphene aerogel in a tetraethylenepentamine molecular chain manner3+Has strong adsorption effect, and the generated product is adsorbed under the action of a surfactant tetrabutylammonium bromideThree-dimensional porous Fe of nanometer flower form3O4Uniformly grows on the surface of a matrix and in a lamellar structure of the graphene aerogel, and effectively reduces the amount of nano Fe3O4The phenomenon of agglomeration.
The MoS2-Fe3O4-graphene ternary composite wave-absorbing material prepared from nano MnCO3The microspheres are used as templates, and the nano MoS is prepared by a liquid phase deposition method and hydrochloric acid etching2Hollow microspheres and then nano flower-shaped three-dimensional porous Fe with large specific surface3O4Compounding modified graphene to obtain MoS2-Fe3O4The three-dimensional conductive network and the interface polarization effect are formed among the graphene ternary composite wave-absorbing material, the composite material is endowed with good resistance loss and magnetic loss performance through good magnetic performance, and meanwhile, the nano MoS2And three-dimensional porous Fe3O4The pore structure can continuously reflect electromagnetic waves, enhances the impedance matching performance of the composite material under the synergistic effect, and shows excellent wave-absorbing effect.
Drawings
FIG. 1 is a schematic front view of a case;
fig. 2 is an enlarged schematic view of the rotary bearing.
1. A box body; 2. a heating device; 3. a rotating device; 4. a rotating bearing; 5. rotating the rod; 6. a reaction kettle box; 7. a miniature reaction kettle.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: MoS2-Fe3O4The graphene ternary composite wave-absorbing material comprises the following raw materials and components: aminated graphene aerogel, ferric chloride, urea, surfactant tetrabutylammonium bromide and nano MoS2The hollow microspheres comprise aminated graphene aerogel, ferric chloride, urea and a surfactant in a mass ratio of 6-15:100:200-400: 180-300.
The preparation method of the aminated graphene aerogel comprises the following steps:
(1) adding a graphene oxide aqueous solution with the mass fraction of 2-4% into a reaction bottle, adding tetraethylenepentamine after the graphene oxide aqueous solution is uniformly dispersed by ultrasonic, wherein the mass ratio of the graphene oxide aqueous solution to the tetraethylenepentamine is 1:1.5-2.5, pouring the solution into a micro reaction kettle, placing the solution into a reaction kettle heating box, wherein the reaction kettle heating box comprises a box body, a heating device is fixedly connected below the inner part of the box body, rotating devices are fixedly connected on two sides of the inner part of the box body, a rotating bearing is movably connected inside the rotating device and is movably connected with a rotating rod, the rotating rod is fixedly connected with the reaction kettle box, a micro reaction kettle is arranged inside the reaction kettle box, heating is carried out to the temperature of 160-180 ℃, reacting for 10-15h, filtering the solution to remove a solvent, washing a solid product by using distilled water and ethanol, carrying out.
Nano MoS2The preparation method of the hollow microsphere comprises the following steps:
(1) adding a mixed solvent of distilled water and ethanol into a reaction bottle, wherein the volume ratio of the distilled water to the ethanol is 8-12:1, adding manganese sulfate and ammonium bicarbonate with the mass ratio of 1:5-6, placing the mixture into a constant-temperature water bath kettle, heating the mixture to 40-60 ℃, reacting for 8-12h, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, and fully drying to obtain the nano MnCO3And (3) microspheres.
(2) Adding distilled water solvent and nano MnCO into a reaction bottle3Uniformly dispersing microspheres by ultrasonic, adding sodium molybdate and L-cysteine in a mass ratio of 0.5-0.8:1:3-4, uniformly stirring, pouring the solution into a micro reaction kettle, placing the micro reaction kettle in a reaction kettle heating box, heating to 200-2Hollow microspheres.
MoS2-Fe3O4The preparation method of the-graphene ternary composite wave-absorbing material comprises the following steps:
(1) adding ethylene glycol solvent, aminated graphene aerogel and ferric chloride into a reaction bottle, placing the reaction bottle into an oil bath pot after ultrasonic dispersion is uniform, heating to 35-55 ℃, stirring at constant speed for 4-10h, and adding urea and ferric chlorideHeating the surfactant tetrabutylammonium bromide to the temperature of 190-3O4Modifying graphene.
(2) Adding distilled water solvent and three-dimensional porous Fe into a reaction bottle3O4Modified graphene and nano MoS2The mass ratio of the hollow microspheres to the water is 2.5-4:1, after the ultrasonic dispersion is uniform, the solution is poured into a micro reaction kettle and placed in a heating box of the reaction kettle, the reaction is carried out for 2-5h after the solution is heated to 120 ℃ plus 100 ℃, the solvent is removed by filtration and the solution is dried, and the MoS is prepared2-Fe3O4-graphene ternary composite wave-absorbing material.
Example 1
(1) Aminated graphene aerogel component 1: adding a graphene oxide aqueous solution with the mass fraction of 2% into a reaction bottle, adding tetraethylenepentamine after uniform ultrasonic dispersion, wherein the mass ratio of the graphene oxide aqueous solution to the tetraethylenepentamine is 1:1.5, pouring the solution into a micro-reaction kettle, placing the solution into a reaction kettle heating box, wherein the reaction kettle heating box comprises a box body, a heating device is fixedly connected below the inner part of the box body, rotating devices are fixedly connected on two sides of the inner part of the box body, a rotating bearing is movably connected inside the rotating devices, the rotating bearing is movably connected with a rotating rod, the rotating rod is fixedly connected with the reaction kettle box, the micro-reaction kettle is arranged inside the reaction kettle, heating is carried out to 160 ℃, reacting for 10 hours, filtering the solution to remove a solvent, washing a solid product by using distilled water and ethanol, carrying out freeze drying and grinding to obtain the.
(2) Preparation of three-dimensional porous Fe3O4Modifying the graphene component 1, adding an ethylene glycol solvent, an aminated graphene aerogel component 1 and ferric chloride into a reaction bottle, placing the reaction bottle into an oil bath pot after ultrasonic dispersion is uniform, heating to 35 ℃, stirring at a constant speed for 4 hours, adding urea and a surfactant tetrabutylammonium bromide, wherein the aminated graphene aerogel and the chlorine are uniformly mixedHeating iron oxide, urea and surfactant tetrabutylammonium bromide to 190 ℃ in a mass ratio of 6:100:200:180, uniformly stirring and reacting for 1h, cooling the solution to room temperature, filtering to remove the solvent, washing the solid product with distilled water and ethanol, drying, placing the solid product in an atmosphere furnace, introducing nitrogen, heating to 480 ℃ at a heating rate of 2 ℃/min, keeping the temperature and calcining for 2h to prepare the three-dimensional porous Fe in the shape of nano flower3O4Modifying the graphene component 1.
(3) Preparation of Nano MoS2Hollow microsphere component 1: adding a mixed solvent of distilled water and ethanol into a reaction bottle, wherein the volume ratio of the distilled water to the ethanol is 8:1, adding manganese sulfate and ammonium bicarbonate with the mass ratio of 1:5, placing the mixture into a constant-temperature water bath kettle, heating the mixture to 40 ℃, reacting for 8 hours, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, fully drying, and obtaining the nano MnCO3Placing the microspheres in a distilled water solvent, adding sodium molybdate and L-cysteine according to the mass ratio of 0.5:1:3 after uniformly dispersing by ultrasonic, pouring the solution into a micro-reaction kettle after uniformly stirring, placing the micro-reaction kettle in a reaction kettle heating box, heating to 200 ℃, reacting for 20 hours, cooling the solution to room temperature, filtering, washing, placing a solid product in a hydrochloric acid solution with the mass fraction of 3%, uniformly stirring for 10 hours, filtering, washing and fully drying the solution to prepare the nano MoS2Hollow microsphere component 1.
(4) Preparation of MoS2-Fe3O4-graphene ternary composite wave-absorbing material 1: adding distilled water solvent and three-dimensional porous Fe into a reaction bottle3O4Modified graphene component 1 and nano MoS2The mass ratio of the hollow microsphere component 1 to the hollow microsphere component 1 is 2.5:1, after the ultrasonic dispersion is uniform, the solution is poured into a micro reaction kettle and placed in a heating box of the reaction kettle, the temperature is increased to 100 ℃, the reaction is carried out for 2 hours, the solution is filtered to remove the solvent and dried, and the MoS is prepared2-Fe3O4-graphene ternary composite wave-absorbing material 1.
Example 2
(1) Aminated graphene aerogel component 2: adding a graphene oxide aqueous solution with the mass fraction of 2.5% into a reaction bottle, adding tetraethylenepentamine after uniform ultrasonic dispersion, wherein the mass ratio of the graphene oxide aqueous solution to the tetraethylenepentamine is 1:1.7, pouring the solution into a micro-reaction kettle, placing the solution into a reaction kettle heating box, wherein the reaction kettle heating box comprises a box body, a heating device is fixedly connected below the inner part of the box body, rotating devices are fixedly connected to two sides of the inner part of the box body, a rotating bearing is movably connected inside the rotating devices, the rotating bearing is movably connected with a rotating rod, the rotating rod is fixedly connected with the reaction kettle box, a micro-reaction kettle is arranged inside the reaction kettle box, heating is carried out to 180 ℃, reacting for 10 hours, filtering the solution to remove a solvent, washing a solid product by using distilled water and ethanol, carrying out freeze drying and grinding to obtain the.
(2) Preparation of three-dimensional porous Fe3O4Adding a glycol solvent, an aminated graphene aerogel component 2 and ferric chloride into a reaction bottle, ultrasonically dispersing uniformly, placing the reaction bottle in an oil bath, heating to 40 ℃, stirring at a constant speed for 8 hours, adding urea and a surfactant tetrabutylammonium bromide, wherein the mass ratio of the aminated graphene aerogel, the ferric chloride, the urea and the surfactant tetrabutylammonium bromide is 8:100:250:210, heating to 220 ℃, stirring at a constant speed for reaction for 1 hour, cooling the solution to room temperature, filtering to remove the solvent, washing and drying a solid product by using distilled water and ethanol, placing the solid product in an atmosphere furnace, introducing nitrogen, heating at a heating rate of 3 ℃/min, heating to 480 ℃, preserving heat and calcining for 4 hours, thus obtaining the three-dimensional porous Fe in the shape of a nanometer flower3O4Modifying the graphene component 2.
(3) Preparation of Nano MoS2Hollow microsphere component 2: adding a mixed solvent of distilled water and ethanol into a reaction bottle, wherein the volume ratio of the distilled water to the ethanol is 8:1, adding manganese sulfate and ammonium bicarbonate with the mass ratio of 1:5.2, placing the mixture into a constant-temperature water bath kettle, heating the mixture to 50 ℃, reacting for 12 hours, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, fully drying, and obtaining the nano MnCO3Placing the microspheres in a distilled water solvent, adding sodium molybdate and L-cysteine with the mass ratio of 0.6:1:3.2 after uniformly dispersing by ultrasonic, pouring the solution into a micro reaction kettle after uniformly stirring, placing the micro reaction kettle in a reaction kettle heating box, heating to 230 ℃, reacting for 24 hours,cooling the solution to room temperature, filtering, washing, placing the solid product in a hydrochloric acid solution with the mass fraction of 4%, uniformly stirring for 20 hours, filtering, washing and fully drying the solution to prepare the nano MoS2Hollow microsphere component 2.
(4) Preparation of MoS2-Fe3O4-graphene ternary composite wave-absorbing material 2: adding distilled water solvent and three-dimensional porous Fe into a reaction bottle3O4Modified graphene component 2 and nano MoS2The mass ratio of the hollow microsphere component 1 to the hollow microsphere component 1 is 3:1, after the ultrasonic dispersion is uniform, the solution is poured into a micro reaction kettle and placed in a heating box of the reaction kettle, the heating is carried out to 120 ℃, the reaction is carried out for 4 hours, the solution is filtered to remove the solvent and dried, and the MoS is prepared2-Fe3O4-graphene ternary composite wave-absorbing material 2.
Example 3
(1) Aminated graphene aerogel component 3: adding 3% graphene oxide aqueous solution into a reaction bottle, adding tetraethylenepentamine after uniform ultrasonic dispersion, wherein the mass ratio of the graphene oxide aqueous solution to the tetraethylenepentamine is 1:2, pouring the solution into a micro reaction kettle, placing the solution into a reaction kettle heating box, wherein the reaction kettle heating box comprises a box body, a heating device is fixedly connected to the lower part of the inner part of the box body, rotating devices are fixedly connected to two sides of the inner part of the box body, a rotating bearing is movably connected to the inner part of each rotating device, the rotating bearing is movably connected with a rotating rod, the rotating rod is fixedly connected with the reaction kettle box, the micro reaction kettle is arranged in the reaction kettle box, heating is carried out to 170 ℃, reacting is carried out for 12 hours, filtering the solution to remove a solvent, washing a solid product by using distilled water and ethanol, carrying out freeze drying and grinding.
(2) Preparation of three-dimensional porous Fe3O4Modifying the graphene component 3, adding an ethylene glycol solvent, an aminated graphene aerogel component 3 and ferric chloride into a reaction bottle, placing the reaction bottle into an oil bath pot after ultrasonic dispersion is uniform, heating to 45 ℃, stirring at a constant speed for 7 hours, and then adding urea and a surfactant tetrabutylammonium bromide, wherein the mass ratio of the aminated graphene aerogel, the ferric chloride, the urea and the surfactant tetrabutylammonium bromide is 10:100:300220, heating to 210 ℃, stirring at a constant speed for reaction for 2 hours, cooling the solution to room temperature, filtering to remove the solvent, washing the solid product with distilled water and ethanol, drying, placing the solid product in an atmosphere furnace, introducing nitrogen, heating to 500 ℃ at the heating rate of 4 ℃/min, keeping the temperature and calcining for 3 hours to prepare the three-dimensional porous Fe in the shape of nano flowers3O4Modifying the graphene component 3.
(3) Preparation of Nano MoS2Hollow microsphere component 3: adding a mixed solvent of distilled water and ethanol into a reaction bottle, wherein the volume ratio of the distilled water to the ethanol is 10:1, adding manganese sulfate and ammonium bicarbonate with the mass ratio of 1:5.5, placing the mixture into a constant-temperature water bath kettle, heating the mixture to 50 ℃, reacting for 10 hours, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, fully drying, and obtaining the nano MnCO3Placing the microspheres in a distilled water solvent, adding sodium molybdate and L-cysteine after uniformly dispersing by ultrasonic, wherein the mass ratio of the sodium molybdate to the L-cysteine is 0.65:1:3.5, stirring uniformly, pouring the solution into a micro-reaction kettle, placing the micro-reaction kettle in a reaction kettle heating box, heating to 210 ℃, reacting for 25h, cooling the solution to room temperature, filtering, washing, placing the solid product in a hydrochloric acid solution with the mass fraction of 4%, stirring at a constant speed for 15h, filtering, washing and fully drying the solution to prepare the nano MoS2Hollow microsphere component 3.
(4) Preparation of MoS2-Fe3O4-graphene ternary composite wave-absorbing material 3: adding distilled water solvent and three-dimensional porous Fe into a reaction bottle3O4Modified graphene component 3 and nano MoS2The mass ratio of the hollow microsphere component 3 to the hollow microsphere component 3 is 3.2:1, after the ultrasonic dispersion is uniform, the solution is poured into a micro reaction kettle and placed in a heating box of the reaction kettle, the temperature is increased to 110 ℃, the reaction is carried out for 3 hours, the solution is filtered to remove the solvent and dried, and the MoS is prepared2-Fe3O4-a graphene ternary composite wave-absorbing material 3.
Example 4
(1) Aminated graphene aerogel component 4: adding a 4% graphene oxide aqueous solution into a reaction bottle, adding tetraethylenepentamine after uniform ultrasonic dispersion, wherein the mass ratio of the graphene oxide aqueous solution to the tetraethylenepentamine is 1:2.2, pouring the solution into a micro reaction kettle, placing the solution into a reaction kettle heating box, wherein the reaction kettle heating box comprises a box body, a heating device is fixedly connected below the inner part of the box body, rotating devices are fixedly connected on two sides of the inner part of the box body, a rotating bearing is movably connected inside the rotating devices, the rotating bearing is movably connected with a rotating rod, the rotating rod is fixedly connected with the reaction kettle box, the micro reaction kettle is arranged inside the reaction kettle box, heating is carried out to 180 ℃, reacting is carried out for 15 hours, filtering the solution to remove a solvent, washing a solid product by using distilled water and ethanol, carrying out freeze drying and grinding to obtain an aminated graphene aerogel.
(2) Preparation of three-dimensional porous Fe3O4Modifying a graphene component 4, adding an ethylene glycol solvent, an aminated graphene aerogel component 4 and ferric chloride into a reaction bottle, ultrasonically dispersing uniformly, placing the reaction bottle into an oil bath pot, heating to 45 ℃, stirring at a constant speed for 6 hours, adding urea and a surfactant tetrabutylammonium bromide, wherein the mass ratio of the aminated graphene aerogel, the ferric chloride, the urea and the surfactant tetrabutylammonium bromide is 13:100:350:270, heating to 220 ℃, stirring at a constant speed for reaction for 2 hours, cooling the solution to room temperature, filtering to remove the solvent, washing and drying a solid product by using distilled water and ethanol, placing the solid product into an atmosphere furnace, introducing nitrogen, heating at a heating rate of 5 ℃/min, heating to 480 ℃, preserving heat and calcining for 3 hours, thus obtaining the three-dimensional porous Fe in the shape of a nanometer flower3O4A modified graphene component 4.
(3) Preparation of Nano MoS2Hollow microsphere component 4: adding a mixed solvent of distilled water and ethanol into a reaction bottle, wherein the volume ratio of the distilled water to the ethanol is 11:1, adding manganese sulfate and ammonium bicarbonate with the mass ratio of 1:5.7, placing the mixture into a constant-temperature water bath kettle, heating the mixture to 60 ℃, reacting for 10 hours, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, fully drying, and obtaining the nano MnCO3Placing the microspheres in a distilled water solvent, adding sodium molybdate and L-cysteine according to the mass ratio of 0.7:1:3.8 after uniformly dispersing by ultrasonic, pouring the solution into a micro-reaction kettle after uniformly stirring, placing the micro-reaction kettle in a reaction kettle heating box, heating to 230 ℃, reacting for 22 hours, cooling the solution to room temperature, filtering, washing, placing the solid product in a mass positionStirring at constant speed for 18h in 5% hydrochloric acid solution, filtering, washing and fully drying the solution to obtain the nano MoS2A hollow microsphere component 4.
(4) Preparation of MoS2-Fe3O4-graphene ternary composite wave-absorbing material 4: adding distilled water solvent and three-dimensional porous Fe into a reaction bottle3O4Modified graphene component 4 and nano MoS2The mass ratio of the hollow microsphere component 4 to the hollow microsphere component 3.6:1, pouring the solution into a micro reaction kettle after uniform ultrasonic dispersion, placing the micro reaction kettle into a reaction kettle heating box, heating to 120 ℃, reacting for 5 hours, filtering the solution to remove the solvent, and drying to prepare the MoS2-Fe3O4-a graphene ternary composite wave-absorbing material 4.
Example 5
(1) Aminated graphene aerogel component 5: adding a 4% graphene oxide aqueous solution into a reaction bottle, adding tetraethylenepentamine after uniform ultrasonic dispersion, wherein the mass ratio of the graphene oxide aqueous solution to the tetraethylenepentamine is 1:2.5, pouring the solution into a micro reaction kettle, placing the solution into a reaction kettle heating box, wherein the reaction kettle heating box comprises a box body, a heating device is fixedly connected below the inner part of the box body, rotating devices are fixedly connected on two sides of the inner part of the box body, a rotating bearing is movably connected inside the rotating devices, the rotating bearing is movably connected with a rotating rod, the rotating rod is fixedly connected with the reaction kettle box, the micro reaction kettle is arranged inside the reaction kettle box, heating is carried out to 180 ℃, reacting is carried out for 15 hours, filtering the solution to remove a solvent, washing a solid product by using distilled water and ethanol, carrying out freeze drying and grinding to obtain the aminated graphene aerogel.
(2) Preparation of three-dimensional porous Fe3O4Modifying graphene component 5, adding a glycol solvent, an aminated graphene aerogel component 5 and ferric chloride into a reaction bottle, placing the reaction bottle into an oil bath pot after ultrasonic dispersion is uniform, heating to 55 ℃, stirring at a constant speed for 10 hours, adding urea and a surfactant tetrabutylammonium bromide, wherein the mass ratio of the aminated graphene aerogel, the ferric chloride, the urea and the surfactant tetrabutylammonium bromide is 15:100:400:300, heating to 220 ℃, stirring at a constant speed for reaction for 3 hours, cooling the solution to the temperature of 15:100:400:300, and stirring at a constant speed for reactionFiltering to remove the solvent at room temperature, washing the solid product with distilled water and ethanol, drying, placing the solid product in an atmosphere furnace, introducing nitrogen, heating to 520 ℃ at a heating rate of 5 ℃/min, and calcining for 4h to obtain the three-dimensional porous Fe in the shape of nanoflower3O4Modifying the graphene component 5.
(3) Preparation of Nano MoS2Hollow microsphere component 5: adding a mixed solvent of distilled water and ethanol into a reaction bottle, wherein the volume ratio of the distilled water to the ethanol is 12:1, adding manganese sulfate and ammonium bicarbonate with the mass ratio of 1:6, placing the mixture into a constant-temperature water bath kettle, heating the mixture to 60 ℃, reacting for 12 hours, filtering the solution to remove the solvent, washing a solid product by using distilled water and ethanol, fully drying, and obtaining the nano MnCO3Placing the microspheres in a distilled water solvent, adding sodium molybdate and L-cysteine with the mass ratio of 0.8:1:4 after uniformly dispersing by ultrasonic, pouring the solution into a micro-reaction kettle after uniformly stirring, placing the micro-reaction kettle in a reaction kettle heating box, heating to 230 ℃, reacting for 30 hours, cooling the solution to room temperature, filtering, washing, placing the solid product in a hydrochloric acid solution with the mass fraction of 5%, uniformly stirring for 20 hours, filtering, washing and fully drying the solution to prepare the nano MoS2A hollow microsphere component 5.
(4) Preparation of MoS2-Fe3O4-graphene ternary composite wave-absorbing material 5: adding distilled water solvent and three-dimensional porous Fe into a reaction bottle3O4Modified graphene component 5 and nano MoS2The mass ratio of the hollow microsphere component 5 to the hollow microsphere component 5 is 4:1, after the ultrasonic dispersion is uniform, the solution is poured into a micro reaction kettle and placed in a heating box of the reaction kettle, the heating is carried out to 120 ℃, the reaction is carried out for 5 hours, the solution is filtered to remove the solvent and dried, and the MoS is prepared2-Fe3O4-a graphene ternary composite wave-absorbing material 5.
Respectively mixing MoS2-Fe3O4Uniformly mixing the graphene ternary composite wave-absorbing material 1-5 with paraffin to prepare a sheet with the thickness of 2mm, and testing the wave-absorbing performance by using an ZVA40 vector network analyzer.
In summary, the MoS2-Fe3O4The graphene ternary composite wave-absorbing material is prepared by performing nucleophilic substitution reaction and amidation reaction on epoxy groups and carboxyl groups in a nucleophilic reagent tetraethylenepentamine and graphene oxide, and simultaneously performing strong pi-pi stacking action between graphene oxide lamella layers to prepare the tetraene pentamine covalent grafted aminated graphene aerogel, wherein the graphene aerogel has a three-dimensional network structure and large specific surface area, and a large number of amino groups and imino groups are uniformly dispersed in a matrix of the graphene aerogel in a tetraethylenepentamine molecular chain manner3+Has strong adsorption effect, and under the action of surfactant tetrabutylammonium bromide, the produced three-dimensional porous Fe in nanometer flower shape3O4Uniformly grows on the surface of a matrix and in a lamellar structure of the graphene aerogel, and effectively reduces the amount of nano Fe3O4The phenomenon of agglomeration.
With nano MnCO3The microspheres are used as templates, and the nano MoS is prepared by a liquid phase deposition method and hydrochloric acid etching2Hollow microspheres and then nano flower-shaped three-dimensional porous Fe with large specific surface3O4Compounding modified graphene to obtain MoS2-Fe3O4The three-dimensional conductive network and the interface polarization effect are formed among the graphene ternary composite wave-absorbing material, the composite material is endowed with good resistance loss and magnetic loss performance through good magnetic performance, and meanwhile, the nano MoS2And three-dimensional porous Fe3O4The pore structure can continuously reflect electromagnetic waves, the impedance matching performance of the composite material is enhanced under the synergistic effect, the excellent wave absorbing effect is shown, and the maximum reflection loss can reach-41.65 to-49.68 db in the absorption frequency of 7.2 to 8.3 GHz.
Claims (9)
1. MoS2-Fe3O4The graphene ternary composite wave-absorbing material comprises the following raw materials and components, and is characterized in that: aminated graphene aerogel, ferric chloride, urea, watchSurfactant and nano MoS2The hollow microspheres comprise aminated graphene aerogel, ferric chloride, urea and a surfactant in a mass ratio of 6-15:100:200-400: 180-300.
2. A MoS according to claim 12-Fe3O4-graphene ternary composite wave-absorbing material, characterized in that: the surfactant is tetrabutylammonium bromide.
3. A MoS according to claim 12-Fe3O4-graphene ternary composite wave-absorbing material, characterized in that: the preparation method of the aminated graphene aerogel comprises the following steps:
(1) adding tetraethylenepentamine into graphene oxide aqueous solution with the mass fraction of 2-4% and uniform ultrasonic dispersion, pouring the solution into a micro reaction kettle, placing the micro reaction kettle into a reaction kettle heating box, heating to 160-.
4. A MoS according to claim 32-Fe3O4-graphene ternary composite wave-absorbing material, characterized in that: the mass ratio of the graphene oxide to the triethylene tetramine is 1: 1.5-2.5.
5. A MoS according to claim 32-Fe3O4-graphene ternary composite wave-absorbing material, characterized in that: the reation kettle heating cabinet includes the inside both sides fixedly connected with rotary device of box, box inside below fixedly connected with heating device, box, and the inside swing joint of rotary device has swivel bearing, swivel bearing and rotary rod swing joint, and rotary rod fixed connection reation kettle case, the inside miniature reation kettle that is provided with of reation kettle incasement portion.
6. A MoS according to claim 12-Fe3O4-graphene ternary composite wave-absorbing material, whichIs characterized in that: the nano MoS2The preparation method of the hollow microsphere comprises the following steps:
(1) adding manganese sulfate and ammonium bicarbonate into a mixed solvent of distilled water and ethanol with a volume ratio of 8-12:1, heating to 40-60 ℃ with a mass ratio of 1:5-6, reacting for 8-12h, filtering, washing and drying to obtain the nano MnCO3Microspheres;
(2) adding nano MnCO into distilled water solvent3Uniformly dispersing microspheres by ultrasonic, adding sodium molybdate and L-cysteine, pouring the solution into a micro reaction kettle, placing the solution into a reaction kettle heating box, heating to the temperature of 200-2Hollow microspheres.
7. A MoS according to claim 62-Fe3O4-graphene ternary composite wave-absorbing material, characterized in that: the nano MnCO3The mass ratio of the microspheres to the sodium molybdate to the L-cysteine is 0.5-0.8:1: 3-4.
8. A MoS according to claim 12-Fe3O4-graphene ternary composite wave-absorbing material, characterized in that: the MoS2-Fe3O4The preparation method of the-graphene ternary composite wave-absorbing material comprises the following steps:
(1) adding aminated graphene aerogel and ferric chloride into an ethylene glycol solvent, performing ultrasonic dispersion uniformly, heating to 35-55 ℃, stirring for 4-10h, adding urea and a surfactant tetrabutylammonium bromide, heating to 190-3O4Modifying graphene;
(2) adding three-dimensional porous Fe into distilled water solvent3O4Modified graphene and nano MoS2Dispersing hollow microsphere in ultrasonic wave, and mixing the solutionPouring into a micro reaction kettle, placing in a reaction kettle heating box, heating to 120 ℃, reacting for 2-5h, filtering and drying to obtain MoS2-Fe3O4-graphene ternary composite wave-absorbing material.
9. A MoS according to claim 12-Fe3O4-graphene ternary composite wave-absorbing material, characterized in that: the three-dimensional porous Fe3O4Modified graphene and nano MoS2The mass ratio of the hollow microspheres is 2.5-4: 1.
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| CN112063365A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
| CN112939083A (en) * | 2021-02-07 | 2021-06-11 | 哈尔滨工业大学（威海） | Molybdenum disulfide/ferroferric oxide/graphene nanosheet composite wave absorber and preparation method thereof |
| CN113725423A (en) * | 2021-09-17 | 2021-11-30 | 陕西科技大学 | MnCO3/MoS2Heterojunction composite material and preparation method and application thereof |
| CN116514170A (en) * | 2022-01-21 | 2023-08-01 | 湘潭大学 | Hollow flower ball structure molybdenum disulfide and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112063365A (en) * | 2020-09-04 | 2020-12-11 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
| CN112063365B (en) * | 2020-09-04 | 2021-06-01 | 山东大学 | Molybdenum disulfide nitrogen composite porous carbon material and preparation method and application thereof |
| CN112939083A (en) * | 2021-02-07 | 2021-06-11 | 哈尔滨工业大学（威海） | Molybdenum disulfide/ferroferric oxide/graphene nanosheet composite wave absorber and preparation method thereof |
| CN113725423A (en) * | 2021-09-17 | 2021-11-30 | 陕西科技大学 | MnCO3/MoS2Heterojunction composite material and preparation method and application thereof |
| CN116514170A (en) * | 2022-01-21 | 2023-08-01 | 湘潭大学 | Hollow flower ball structure molybdenum disulfide and application thereof |
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