CN111454579A - Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof - Google Patents

Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof Download PDF

Info

Publication number
CN111454579A
CN111454579A CN202010337987.1A CN202010337987A CN111454579A CN 111454579 A CN111454579 A CN 111454579A CN 202010337987 A CN202010337987 A CN 202010337987A CN 111454579 A CN111454579 A CN 111454579A
Authority
CN
China
Prior art keywords
nano
heating
nife
absorbing material
phosphorus
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010337987.1A
Other languages
Chinese (zh)
Inventor
张荣虎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN202010337987.1A priority Critical patent/CN111454579A/en
Publication of CN111454579A publication Critical patent/CN111454579A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/198Graphene oxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
    • C08G83/008Supramolecular polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • C08K3/042Graphene or derivatives, e.g. graphene oxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/02Ingredients treated with inorganic substances
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0083Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/01Magnetic additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The invention relates to the technical field of wave-absorbing materials, and discloses a nano nickel ferrite loaded graphene-based wave-absorbing material which comprises the following formula raw materials and components: phosphorus-doped graphene oxide and nano-porous NiFe2O4And paraffin wax in the weight ratio of 0.2-0.6 to 0.4-0.8 to 1. According to the nano nickel ferrite loaded graphene-based wave-absorbing material, NiFe bimetal MOFs high-temperature thermal cracking is carried out to prepare porous nano NiFe2O4The phosphorus-doped graphene oxide composite material and phosphorus-doped graphene oxide form a composite material, phosphorus doping can improve the conductivity of the graphene oxide, more current carriers can be introduced, the electrical loss capacity of the composite material can be enhanced, structural defects are generated by the phosphorus doping, the interface polarization effect of the material is enhanced, the phosphorus-doped graphene with excellent conductivity and the nano NiFe with excellent magnetic performance are obtained2O4Good impedance matching performance is formed, and the absorbed electromagnetic wave is added into the nano NiFe2O4And a large number of pore structures are continuously reflected, so that the wave absorbing performance of the composite material is enhanced under the synergistic effect.

Description

Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof
Technical Field
The invention relates to the technical field of wave-absorbing materials, in particular to a nano nickel ferrite loaded graphene-based wave-absorbing material and a preparation method thereof.
Background
Electromagnetic waves with electromagnetic radiation characteristics comprise radio waves, microwaves, infrared rays, visible light, ultraviolet rays and the like, precision electronic instruments such as notebook computers, GPS, mobile phones, aircraft navigation systems, medical equipment and the like are interfered by the electromagnetic waves, normal use of the instruments is influenced, the electromagnetic radiation damages human bodies mainly through heat effects, non-heat effects and accumulation effects, and diseases such as immunity reduction, metabolism disorder, memory loss and the like of the human bodies are caused by damage to central nervous systems, organism immune systems, cardiovascular systems and the like of the human bodies after long-term reception of the electromagnetic radiation.
The wave-absorbing material can weaken and absorb the energy of electromagnetic waves projected to the surface, so that the interference of the electromagnetic waves is reduced, the wave-absorbing material can absorb and lose the electromagnetic waves through resistance type loss, dielectric loss, magnetic loss and the like, and the wave-absorbing material mainly comprises carbon series wave-absorbing materials such as graphene, carbon nano tubes, carbon fibers and the like; the iron-based wave-absorbing material comprises barium ferrite, nickel zinc ferrite and the like, wherein the nickel ferrite has good magnetic conductivity and soft magnetism, and can attenuate electromagnetic waves through magnetic loss, but the wave-absorbing material is difficult to achieve impedance matching performance only by the magnetic loss performance of the nickel zinc ferrite, so that the wave-absorbing performance is poor, the graphene has the advantages of high conductivity, large specific surface area, light weight and the like, and the iron-based wave-absorbing material is widely applied to the fields of electromagnetic shielding and electromagnetic wave absorption, can be combined with the graphene, and can improve the impedance matching performance and the wave-absorbing performance of the nickel ferrite material.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a nano nickel ferrite loaded graphene-based wave-absorbing material and a preparation method thereof, and solves the problem that the impedance matching performance and the wave-absorbing performance of a nickel-zinc ferrite material are poor.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a nanometer nickel ferrite loaded graphene-based wave-absorbing material comprises the following formula raw materials and components: phosphorus-doped graphene oxide and nano-porous NiFe2O4And paraffin wax in the weight ratio of 0.2-0.6 to 0.4-0.8 to 1.
Preferably, the preparation method of the nano-porous NiFe2O4 comprises the following steps:
(1) adding a mixed solvent of N, N-dimethylformamide and ethanol into a reaction bottle, adding ligand terephthalic acid and 3, 3-diaminobenzidine, stirring for dissolving, and adding NiCl2And FeCl2Heating the solution in a water bath to 40-60 ℃, uniformly stirring for 20-40min, transferring the solution into a reaction kettle, placing the solution into a reaction kettle heating box, heating to 120-150 ℃, reacting for 4-8h, filtering the solution to remove the solvent, washing the solid product by using distilled water and ethanol, and fully drying to prepare the NiFe bimetallic MOFs.
(2) Putting the NiFe bimetal MOFs into a muffle furnace, heating to 350 ℃ at the heating rate of 2-5 ℃/min, carrying out heat preservation treatment for 30-90min, heating to 520 ℃ at 480 ℃ and calcining for 1-2h to obtain the nano porous NiFe2O 4.
Preferably, the reation kettle heating cabinet includes heating box, heating box below fixedly connected with blast heater, blast heater swing joint have rotary rod, the rotatory fan piece of rotary rod fixedly connected with, the inside fixedly connected with agitating unit of heating box, and agitating unit swing joint has agitator shaft, agitator shaft swing joint have regulator, regulator and fixation clamp swing joint.
Preferably, the terephthalic acid, 3-diaminobenzidine and NiCl are used2And FeCl2The mass ratio of the substances is 16-20:0.5-0.8:1: 2.
Preferably, the preparation method of the nano nickel ferrite loaded graphene-based wave-absorbing material comprises the following steps:
(1) adding distilled water solvent, graphene and sodium hypophosphite into a reaction bottle, placing the reaction bottle in an ultrasonic dispersion instrument, heating the reaction bottle to 40-80 ℃, performing ultrasonic dispersion treatment for 2-4h under 30-50KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the reaction bottle to 150-180 ℃, reacting for 8-15h, cooling the solution to room temperature, filtering to remove the solvent, washing the solid product by using distilled water and ethanol, and fully drying to prepare the phosphorus-doped graphene oxide.
(2) Adding a trichloromethane solvent, phosphorus-doped graphene oxide and nano-porous NiFe into a reaction bottle2O4And paraffin wax, stirring and dissolving, then carrying out ultrasonic dispersion treatment on the solution, pouring the solution into a film forming mould, fully drying and tabletting to prepare a 1mm film, and thus obtaining the nano nickel ferrite loaded graphene-based wave-absorbing material.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the nano nickel ferrite loaded graphene-based wave-absorbing material is prepared by taking terephthalic acid and 3, 3-diaminobenzidine as ligands, preparing NiFe bimetal MOFs through a hot solvent method, and preparing porous nano NiFe through high-temperature thermal cracking2O4And then the paraffin is used as a substrate to form a composite material with the phosphorus-doped graphene oxide, phosphorus doping can improve the conductivity of the graphene oxide, more current carriers can be introduced, the electrical loss capability of the composite material can be enhanced, and the carbon lattice of the graphene is damaged by the phosphorus doping, so that structural defects are generated, the interface polarization effect of the material is enhanced, the phosphorus-doped graphene with excellent conductivity and the nano NiFe with excellent magnetic property are obtained2O4Good impedance matching performance is formed, and the absorbed electromagnetic wave is added into the nano NiFe2O4And a large number of pore structures are continuously reflected, and the excellent wave absorbing performance is shown under the synergistic effect.
Drawings
FIG. 1 is a schematic front view of a heating cabinet;
FIG. 2 is an enlarged schematic view of the stirring device;
1. heating the box body; 2. a blower heater; 3. rotating the rod; 4. rotating the fan blade; 5. a stirring device; 6. a stirring bearing; 7. a stirring rod; 8. a regulator; 9. and (4) fixing clips.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a nanometer nickel ferrite loaded graphene-based wave-absorbing material comprises the following formula raw materials and components: phosphorus-doped graphene oxide and nano-porous NiFe2O4And paraffin wax in the weight ratio of 0.2-0.6 to 0.4-0.8 to 1.
The preparation method of the nano-porous NiFe2O4 comprises the following steps:
(1) adding a mixed solvent of N, N-dimethylformamide and ethanol into a reaction bottle, adding ligand terephthalic acid and 3, 3-diaminobenzidine, stirring for dissolving, and adding NiCl2And FeCl2The weight ratio of the four substances is 16-20:0.5-0.8:1:2, the solution is placed in a water bath kettle to be heated to 40-60 ℃, stirred at a constant speed for 20-40min, the solution is transferred into a reaction kettle, the reaction kettle heating box comprises a heating box body, a blast heater is fixedly connected below the heating box body, the blast heater is movably connected with a rotary rod, the rotary rod is fixedly connected with a rotary fan blade, a stirring device is fixedly connected in the heating box body, the stirring device is movably connected with a stirring bearing, the stirring bearing is movably connected with a stirring rod, the stirring rod is movably connected with a regulator, the regulator is movably connected with a fixing clamp, and placing the solution in a heating box of a reaction kettle, heating the solution to the temperature of 120-150 ℃, reacting for 4-8h, filtering the solution to remove the solvent, washing the solid product by using distilled water and ethanol, and fully drying to prepare the NiFe bimetallic MOFs.
(2) Putting the NiFe bimetal MOFs into a muffle furnace, heating to 350 ℃ at the heating rate of 2-5 ℃/min, carrying out heat preservation treatment for 30-90min, heating to 520 ℃ at 480 ℃, and calcining for 1-2h to obtain the nano porous NiFe2O4
The preparation method of the nano nickel ferrite loaded graphene-based wave-absorbing material comprises the following steps:
(1) adding distilled water solvent, graphene and sodium hypophosphite into a reaction bottle, placing the reaction bottle in an ultrasonic dispersion instrument, heating the reaction bottle to 40-80 ℃, performing ultrasonic dispersion treatment for 2-4h under 30-50KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the reaction bottle to 150-180 ℃, reacting for 8-15h, cooling the solution to room temperature, filtering to remove the solvent, washing the solid product by using distilled water and ethanol, and fully drying to prepare the phosphorus-doped graphene oxide.
(2) Adding a trichloromethane solvent, phosphorus-doped graphene oxide and nano-porous NiFe into a reaction bottle2O4And paraffin wax, stirring and dissolving, then carrying out ultrasonic dispersion treatment on the solution, pouring the solution into a film forming mould, fully drying and tabletting to prepare a 1mm film, and thus obtaining the nano nickel ferrite loaded graphene-based wave-absorbing material.
Example 1
(1) Preparing a NiFe bimetal MOFs component 1: adding a mixed solvent of N, N-dimethylformamide and ethanol into a reaction bottle, adding ligand terephthalic acid and 3, 3-diaminobenzidine, stirring for dissolving, and adding NiCl2And FeCl2The four substances are in a mass ratio of 16:0.5:1:2, the solution is placed in a water bath pot to be heated to 40 ℃, stirred at a constant speed for 20min, and transferred into a reaction kettle, a heating box of the reaction kettle comprises a heating box body, a blast heater is fixedly connected below the heating box body, the blast heater is movably connected with a rotating rod, the rotating rod is fixedly connected with a rotating fan sheet, a stirring device is fixedly connected inside the heating box body, the stirring device is movably connected with a stirring bearing, the stirring bearing is movably connected with a stirring rod, the stirring rod is movably connected with a regulator, the regulator is movably connected with a fixing clamp and is placed in the heating box of the reaction kettle to be heated to 120 ℃, the solution is heated to react for 4h, the solution is filtered to remove the solvent, a solid product is washed by using distilled water and ethanol, and is fully dried.
(2) Preparation of nanoporous NiFe2O4Component 1: putting the NiFe bimetal MOFs component 1 into a muffle furnace, heating to 300 ℃ at the heating rate of 2 ℃/min, carrying out heat preservation treatment for 30min, heating to 480 ℃ and calcining for 1h to obtain the nano porous NiFe2O4And (3) component 1.
(3) Phosphorus-doped graphene oxide component 1: adding distilled water solvent, graphene and sodium hypophosphite into a reaction bottle, placing the reaction bottle in an ultrasonic dispersion instrument, heating the reaction bottle to 40 ℃, performing ultrasonic dispersion treatment for 2 hours under the condition of 30KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the reaction bottle to 150 ℃, reacting for 8 hours, cooling the solution to room temperature, filtering to remove the solvent, washing a solid product by using distilled water and ethanol, and fully drying to prepare the phosphorus-doped graphene oxide component 1.
(4) Preparing a nano nickel ferrite loaded graphene-based wave-absorbing material 1: adding a trichloromethane solvent, a phosphorus-doped graphene oxide component 1 and nano-porous NiFe into a reaction bottle2O4And stirring and dissolving the component 1 and paraffin in a mass ratio of 0.2:0.4:1, performing ultrasonic dispersion treatment on the solution, pouring the solution into a film forming mold, fully drying and tabletting to prepare a 1mm film, and preparing the nano nickel ferrite loaded graphene-based wave-absorbing material 1.
Example 2
(1) Preparing a NiFe bimetal MOFs component 2: adding a mixed solvent of N, N-dimethylformamide and ethanol into a reaction bottle, adding ligand terephthalic acid and 3, 3-diaminobenzidine, stirring for dissolving, and adding NiCl2And FeCl2And the mass ratio of the four substances is 20:0.5:1:2, the solution is placed in a water bath pot to be heated to 60 ℃, the solution is stirred at a constant speed for 20min and transferred into a reaction kettle, a heating box of the reaction kettle comprises a heating box body, a blast heater is fixedly connected below the heating box body, the blast heater is movably connected with a rotating rod, the rotating rod is fixedly connected with a rotating fan sheet, a stirring device is fixedly connected inside the heating box body, the stirring device is movably connected with a stirring bearing, the stirring bearing is movably connected with a stirring rod, the stirring rod is movably connected with a regulator, the regulator is movably connected with a fixing clamp and is placed in the heating box of the reaction kettle to be heated to 150 ℃, the reaction is carried out for 8h, the solution is filtered to remove the solvent, a solid product is washed by using distilled water and ethanol, and is fully dried.
(2) Preparation of nanoporous NiFe2O4And (2) component: placing NiFe bimetal MOFs component 2 in horseIn a muffle furnace, heating up to 300 ℃ at the heating rate of 2 ℃/min, carrying out heat preservation treatment for 90min, heating up to 480 ℃ and calcining for 2h to prepare the nano porous NiFe2O4And (3) component 2.
(3) Phosphorus-doped graphene oxide component 2: adding distilled water solvent, graphene and sodium hypophosphite into a reaction bottle, placing the reaction bottle in an ultrasonic dispersion instrument, heating the reaction bottle to 80 ℃, performing ultrasonic dispersion treatment for 2 hours under the condition of 30KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the reaction bottle to 150 ℃, reacting for 8 hours, cooling the solution to room temperature, filtering to remove the solvent, washing a solid product by using distilled water and ethanol, and fully drying to prepare the phosphorus-doped graphene oxide component 2.
(4) Preparing a nano nickel ferrite loaded graphene-based wave-absorbing material 2: adding a trichloromethane solvent, a phosphorus-doped graphene oxide component 2 and nano-porous NiFe into a reaction bottle2O4And (3) stirring and dissolving the component 2 and paraffin wax in a mass ratio of 0.25:0.75:1, performing ultrasonic dispersion treatment on the solution, pouring the solution into a film forming mold, fully drying and tabletting to prepare a 1mm film, and preparing the nano nickel ferrite loaded graphene-based wave-absorbing material 2.
Example 3
(1) Preparing a NiFe bimetal MOFs component 3: adding a mixed solvent of N, N-dimethylformamide and ethanol into a reaction bottle, adding ligand terephthalic acid and 3, 3-diaminobenzidine, stirring for dissolving, and adding NiCl2And FeCl2The four substances are in a mass ratio of 18:0.65:1:2, the solution is placed in a water bath pot to be heated to 50 ℃, stirred at a constant speed for 30min, and transferred into a reaction kettle, a heating box of the reaction kettle comprises a heating box body, a blast heater is fixedly connected below the heating box body, the blast heater is movably connected with a rotating rod, the rotating rod is fixedly connected with a rotating fan blade, a stirring device is fixedly connected inside the heating box body, the stirring device is movably connected with a stirring bearing, the stirring bearing is movably connected with a stirring rod, the stirring rod is movably connected with a regulator, the regulator is movably connected with a fixing clamp and is placed in the heating box of the reaction kettle to be heated to 130 ℃, the solution is reacted for 6h, the solution is filtered to remove the solvent, the solid product is washed byDrying, and preparing the NiFe bimetal MOFs component 3.
(2) Preparation of nanoporous NiFe2O4And (3) component: putting the NiFe bimetal MOFs component 3 into a muffle furnace, heating to 330 ℃ at the heating rate of 4 ℃/min, carrying out heat preservation treatment for 60min, heating to 500 ℃ again, and calcining for 1.5h to obtain the nano porous NiFe2O4And (3) component.
(3) Phosphorus-doped graphene oxide component 3: adding distilled water solvent, graphene and sodium hypophosphite into a reaction bottle, placing the reaction bottle in an ultrasonic dispersion instrument, heating the reaction bottle to 60 ℃, performing ultrasonic dispersion treatment for 3 hours under 40KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the reaction bottle to 160 ℃, reacting for 12 hours, cooling the solution to room temperature, filtering to remove the solvent, washing a solid product by using distilled water and ethanol, and fully drying to prepare the phosphorus-doped graphene oxide component 3.
(4) Preparing a nano nickel ferrite loaded graphene-based wave-absorbing material 3: adding a trichloromethane solvent, a phosphorus-doped graphene oxide component 3 and nano-porous NiFe into a reaction bottle2O4And (3) stirring and dissolving the component 3 and the paraffin wax in a mass ratio of 0.4:0.6:1, performing ultrasonic dispersion treatment on the solution, pouring the solution into a film forming mold, fully drying and tabletting to prepare a 1mm film, and preparing the nano nickel ferrite loaded graphene-based wave-absorbing material 3.
Example 4
(1) Preparing a NiFe bimetal MOFs component 4: adding a mixed solvent of N, N-dimethylformamide and ethanol into a reaction bottle, adding ligand terephthalic acid and 3, 3-diaminobenzidine, stirring for dissolving, and adding NiCl2And FeCl2The mass ratio of the four substances is 18:0.7:1:2, the solution is placed in a water bath pot to be heated to 40 ℃, stirred at a constant speed for 30min, and transferred into a reaction kettle, a heating box of the reaction kettle comprises a heating box body, a blast heater is fixedly connected below the heating box body, the blast heater is movably connected with a rotating rod, the rotating rod is fixedly connected with a rotating fan blade, a stirring device is fixedly connected inside the heating box body, the stirring device is movably connected with a stirring bearing, the stirring bearing is movably connected with a stirring rod, and the stirring rod is movably connected with an adjusting deviceAnd the device and the regulator are movably connected with the fixed clamp, are placed in a heating box of a reaction kettle, are heated to 150 ℃, react for 8 hours, filter the solution to remove the solvent, wash the solid product by using distilled water and ethanol, and fully dry to prepare the NiFe bimetal MOFs component 4.
(2) Preparation of nanoporous NiFe2O4And (4) component: putting the NiFe bimetal MOFs component 4 into a muffle furnace, heating to 310 ℃ at the heating rate of 4 ℃/min, carrying out heat preservation treatment for 4min, heating to 520 ℃ again, and calcining for 1h to obtain the nano porous NiFe2O4And (4) component.
(3) Phosphorus-doped graphene oxide component 4: adding distilled water solvent, graphene and sodium hypophosphite into a reaction bottle, placing the reaction bottle in an ultrasonic dispersion instrument, heating the reaction bottle to 60 ℃, performing ultrasonic dispersion treatment for 3 hours under 40KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the reaction bottle to 160 ℃, reacting for 10 hours, cooling the solution to room temperature, filtering to remove the solvent, washing a solid product by using distilled water and ethanol, and fully drying to prepare the phosphorus-doped graphene oxide component 4.
(4) Preparing a nano nickel ferrite loaded graphene-based wave-absorbing material 4: adding a trichloromethane solvent, a phosphorus-doped graphene oxide component 4 and nano-porous NiFe into a reaction bottle2O4And stirring and dissolving the component 4 and the paraffin wax according to the mass ratio of 0.5:0.5:1, performing ultrasonic dispersion treatment on the solution, pouring the solution into a film forming mold, fully drying and tabletting to prepare a 1mm film, and preparing the nano nickel ferrite loaded graphene-based wave-absorbing material 4.
Example 5
(1) Preparing a NiFe bimetal MOFs component 5: adding a mixed solvent of N, N-dimethylformamide and ethanol into a reaction bottle, adding ligand terephthalic acid and 3, 3-diaminobenzidine, stirring for dissolving, and adding NiCl2And FeCl2The mass ratio of the four substances is 20:0.8:1:2, the solution is placed in a water bath pot to be heated to 60 ℃, stirred at a constant speed for 40min, and transferred into a reaction kettle, a heating box of the reaction kettle comprises a heating box body, a blast heater is fixedly connected below the heating box body, the blast heater is movably connected with a rotating rod, and the rotating rod is fixedly connected with the rotating rodThe preparation method comprises the steps of fixedly connecting a stirring device with a rotating fan blade and the inside of a heating box body, wherein the stirring device is movably connected with a stirring bearing, the stirring bearing is movably connected with a stirring rod, the stirring rod is movably connected with an adjuster, the adjuster is movably connected with a fixing clamp, placing the stirring rod in the heating box of a reaction kettle, heating the stirring rod to 150 ℃, reacting for 8 hours, filtering a solution to remove a solvent, washing a solid product by using distilled water and ethanol, fully drying, and preparing the NiFe bimetal MOFs component 5.
(2) Preparation of nanoporous NiFe2O4And (5) component: putting the NiFe bimetal MOFs component 5 into a muffle furnace, heating to 350 ℃ at the heating rate of 5 ℃/min, carrying out heat preservation treatment for 90min, heating to 520 ℃ again, and calcining for 2h to obtain the nano porous NiFe2O4And (5) component.
(3) Phosphorus-doped graphene oxide component 5: adding distilled water solvent, graphene and sodium hypophosphite into a reaction bottle, placing the reaction bottle in an ultrasonic dispersion instrument, heating the reaction bottle to 80 ℃, performing ultrasonic dispersion treatment for 4 hours under 50KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the reaction bottle to 180 ℃, reacting for 15 hours, cooling the solution to room temperature, filtering to remove the solvent, washing a solid product by using distilled water and ethanol, and fully drying to prepare the phosphorus-doped graphene oxide component 5.
(4) Preparing a nano nickel ferrite loaded graphene-based wave-absorbing material 5: adding a trichloromethane solvent, a phosphorus-doped graphene oxide component 5 and nano-porous NiFe into a reaction bottle2O4And stirring and dissolving the component 5 and paraffin wax in a mass ratio of 0.6:0.4:1, performing ultrasonic dispersion treatment on the solution, pouring the solution into a film forming mold, fully drying and tabletting to prepare a 2mm film, and preparing the nano nickel ferrite loaded graphene-based wave-absorbing material 5.
The nano nickel ferrite loaded graphene-based wave-absorbing material prepared in the embodiment 1-5 is subjected to electromagnetic parameter and wave-absorbing performance tests by a TTR500 microwave vector network analyzer.
Figure BDA0002467329910000091
Figure BDA0002467329910000101
In summary, the nano nickel ferrite loaded graphene-based wave-absorbing material takes terephthalic acid and 3, 3-diaminobenzidine as ligands, NiFe bimetal MOFs is prepared by a hot solvent method, and porous nano NiFe is prepared by high-temperature thermal cracking2O4And then the paraffin is used as a substrate to form a composite material with the phosphorus-doped graphene oxide, phosphorus doping can improve the conductivity of the graphene oxide, more current carriers can be introduced, the electrical loss capability of the composite material can be enhanced, and the carbon lattice of the graphene is damaged by the phosphorus doping, so that structural defects are generated, the interface polarization effect of the material is enhanced, the phosphorus-doped graphene with excellent conductivity and the nano NiFe with excellent magnetic property are obtained2O4Good impedance matching performance is formed, and the absorbed electromagnetic wave is added into the nano NiFe2O4The wave absorbing material continuously reflects in a large number of pore structures, shows excellent wave absorbing performance under the synergistic effect, has the absorption frequency band of 12.0-16.4GHz, the bandwidth of 4.4GHz and the optimal reflection loss value of-53.1-58.2 dB.

Claims (5)

1. A nanometer nickel ferrite load graphene-based wave-absorbing material comprises the following formula raw materials and components, and is characterized in that: phosphorus-doped graphene oxide and nano-porous NiFe2O4And paraffin wax in the weight ratio of 0.2-0.6 to 0.4-0.8 to 1.
2. The nano-nickel ferrite loaded graphene-based wave-absorbing material according to claim 1, wherein: the preparation method of the nano-porous NiFe2O4 comprises the following steps:
(1) adding ligand terephthalic acid and 3, 3-diaminobenzidine into a mixed solvent of N, N-dimethylformamide and ethanol, and adding NiCl2And FeCl2Heating to 40-60 ℃, stirring for 20-40min, transferring the solution into a reaction kettle, placing the solution into a reaction kettle heating box, heating to 120-Filtering, washing and drying for 8h to prepare NiFe bimetal MOFs;
(2) putting the NiFe bimetal MOFs into a muffle furnace, heating to 350 ℃ at the heating rate of 2-5 ℃/min, carrying out heat preservation treatment for 30-90min, heating to 520 ℃ at 480 ℃ and calcining for 1-2h to obtain the nano porous NiFe2O 4.
3. The nano-nickel ferrite loaded graphene-based wave-absorbing material according to claim 2, wherein: the reation kettle heating cabinet includes heating box, heating box below fixedly connected with blast heater, blast heater swing joint have rotary rod, rotary rod fixedly connected with rotation fan piece, the inside fixedly connected with agitating unit of heating box, and agitating unit swing joint has agitator bearing, agitator bearing swing joint have puddler, puddler swing joint have regulator, regulator and fixation clamp swing joint.
4. The nano-nickel ferrite loaded graphene-based wave-absorbing material according to claim 2, wherein: the terephthalic acid, the 3, 3-diaminobenzidine and the NiCl2And FeCl2The mass ratio of the substances is 16-20:0.5-0.8:1: 2.
5. The nano-nickel ferrite loaded graphene-based wave-absorbing material according to claim 1, wherein: the preparation method of the nano nickel ferrite loaded graphene-based wave-absorbing material comprises the following steps:
(1) adding graphene and sodium hypophosphite into a distilled water solvent, placing the mixture into an ultrasonic dispersion instrument, heating the mixture to 40-80 ℃, performing ultrasonic dispersion treatment for 2-4h under the condition of 30-50KHz, transferring the solution into a reaction kettle, placing the reaction kettle in a heating box of the reaction kettle, heating the solution to 150-180 ℃, reacting for 8-15h, filtering, washing and drying to prepare phosphorus-doped graphene oxide;
(2) adding phosphorus-doped graphene oxide and nano-porous NiFe into trichloromethane solvent2O4And paraffin wax, stirring for dissolving, performing ultrasonic dispersion treatment, pouring the solution into a film forming mould, fully drying and pressingAnd preparing the sheet into a film with the thickness of 1mm, and preparing the nano nickel ferrite loaded graphene-based wave-absorbing material.
CN202010337987.1A 2020-04-26 2020-04-26 Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof Pending CN111454579A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010337987.1A CN111454579A (en) 2020-04-26 2020-04-26 Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010337987.1A CN111454579A (en) 2020-04-26 2020-04-26 Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN111454579A true CN111454579A (en) 2020-07-28

Family

ID=71674684

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010337987.1A Pending CN111454579A (en) 2020-04-26 2020-04-26 Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111454579A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112087939A (en) * 2020-09-10 2020-12-15 中山大学 FeCoNi @ C/carbon nanotube magnetic composite wave-absorbing material and preparation method and application thereof
CN112300402A (en) * 2020-10-30 2021-02-02 西北工业大学 Preparation method of two-dimensional conductive metal organic framework electromagnetic wave absorbent
CN112844320A (en) * 2020-12-26 2021-05-28 中南大学 Carbon material-coated spinel iron oxide in-situ growth MOFs adsorption catalysis complex and preparation method and application thereof
CN113149593A (en) * 2021-05-17 2021-07-23 沈阳理工大学 Magnesium oxysulfate cement-based wave-absorbing material and preparation method thereof
CN113550069A (en) * 2021-08-04 2021-10-26 安徽锦鼎织造有限公司 Preparation process of terahertz hot-air cotton

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103571432A (en) * 2013-11-22 2014-02-12 北京理工大学 Ferrite hollow sphere-graphene composite wave-absorbing material and preparation method thereof
CN103602310A (en) * 2013-09-02 2014-02-26 南京理工大学常熟研究院有限公司 Ferrite composite wave-absorbing material used for wireless radio frequency identification
CN103871755A (en) * 2014-03-05 2014-06-18 南京理工大学 N-doped graphene/nickel ferrite nanometer compound material and preparation thereof
CN104445079A (en) * 2014-11-28 2015-03-25 中国科学院过程工程研究所 Homogeneous-phase multi-element porous oxide material, preparation method and application thereof
CN104817119A (en) * 2015-04-03 2015-08-05 安徽师范大学 Preparation method and applications of transition metallide
CN105199667A (en) * 2015-10-21 2015-12-30 李同乐 Continuous synthesis method of graphene/ferrite nanocomposite
CN105502286A (en) * 2016-01-04 2016-04-20 南京林业大学 Preparation method of porous nano NiFe2O4
CN106957634A (en) * 2017-03-03 2017-07-18 北京科技大学 A kind of preparation method of graphene mesoporous carbon base composite phase-change material
CN208194409U (en) * 2018-03-23 2018-12-07 西北大学 A kind of interior rotation homogeneous reaction device with positioning system
CN109867780A (en) * 2019-03-05 2019-06-11 北京化工大学 It is a kind of to keep the organic polymer of MOFs pattern, preparation method and application

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103602310A (en) * 2013-09-02 2014-02-26 南京理工大学常熟研究院有限公司 Ferrite composite wave-absorbing material used for wireless radio frequency identification
CN103571432A (en) * 2013-11-22 2014-02-12 北京理工大学 Ferrite hollow sphere-graphene composite wave-absorbing material and preparation method thereof
CN103871755A (en) * 2014-03-05 2014-06-18 南京理工大学 N-doped graphene/nickel ferrite nanometer compound material and preparation thereof
CN104445079A (en) * 2014-11-28 2015-03-25 中国科学院过程工程研究所 Homogeneous-phase multi-element porous oxide material, preparation method and application thereof
CN104817119A (en) * 2015-04-03 2015-08-05 安徽师范大学 Preparation method and applications of transition metallide
CN105199667A (en) * 2015-10-21 2015-12-30 李同乐 Continuous synthesis method of graphene/ferrite nanocomposite
CN105502286A (en) * 2016-01-04 2016-04-20 南京林业大学 Preparation method of porous nano NiFe2O4
CN106957634A (en) * 2017-03-03 2017-07-18 北京科技大学 A kind of preparation method of graphene mesoporous carbon base composite phase-change material
CN208194409U (en) * 2018-03-23 2018-12-07 西北大学 A kind of interior rotation homogeneous reaction device with positioning system
CN109867780A (en) * 2019-03-05 2019-06-11 北京化工大学 It is a kind of to keep the organic polymer of MOFs pattern, preparation method and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
中国感光学会编著: "《2016-2017 感光影像学 学科发展报告》", 31 August 2018 *
贺军哲: ""石墨烯/铁酸镍异质结构的制备及电磁特性研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112087939A (en) * 2020-09-10 2020-12-15 中山大学 FeCoNi @ C/carbon nanotube magnetic composite wave-absorbing material and preparation method and application thereof
CN112300402A (en) * 2020-10-30 2021-02-02 西北工业大学 Preparation method of two-dimensional conductive metal organic framework electromagnetic wave absorbent
CN112844320A (en) * 2020-12-26 2021-05-28 中南大学 Carbon material-coated spinel iron oxide in-situ growth MOFs adsorption catalysis complex and preparation method and application thereof
CN112844320B (en) * 2020-12-26 2022-03-18 中南大学 Carbon material-coated spinel iron oxide in-situ growth MOFs adsorption catalysis complex and preparation method and application thereof
CN113149593A (en) * 2021-05-17 2021-07-23 沈阳理工大学 Magnesium oxysulfate cement-based wave-absorbing material and preparation method thereof
CN113550069A (en) * 2021-08-04 2021-10-26 安徽锦鼎织造有限公司 Preparation process of terahertz hot-air cotton

Similar Documents

Publication Publication Date Title
CN111454579A (en) Nano nickel ferrite loaded graphene-based wave-absorbing material and preparation method thereof
Feng et al. Fabrication of NiFe 2 O 4@ carbon fiber coated with phytic acid-doped polyaniline composite and its application as an electromagnetic wave absorber
CN109705808B (en) Cobalt-nickel alloy-porous carbon composite wave-absorbing material with MOF structure and preparation method thereof
CN111154455B (en) Boron-doped mesoporous flower-like ferroferric oxide/carbon composite wave-absorbing material and preparation method thereof
CN112251193A (en) Composite wave-absorbing material based on MXene and metal organic framework and preparation method and application thereof
CN104628372B (en) A kind of niobium nickel co-doped barium ferrite wave-absorbing powder material and preparation method thereof
CN113088252A (en) Iron-cobalt-nickel alloy/carbon/graphene ultrathin wave-absorbing material and preparation method thereof
CN111748233A (en) Low-reflectivity wave-absorbing material and preparation method thereof
CN101481107A (en) Preparation of nickel-zine ferrite (Ni1-xZnxFe2O4) coated carbon nano-tube magnetic nano composite material
CN111509401A (en) Wave-absorbing material of cobalt-doped zinc oxide-polymer-based carbon material and preparation method thereof
CN113248725A (en) Preparation method of electromagnetic wave absorbing material based on MOF derivation and electromagnetic wave absorbing material
CN114853502B (en) Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof
CN110060834A (en) Magnetically soft alloy powder inhales wave plate, preparation method, electronic component and electronic equipment
CN113462357A (en) Wave-absorbing particles and preparation method and application of composite material thereof
CN110669228B (en) CoFe/C composite material and preparation method and application thereof
CN111285671A (en) Low-frequency wave-absorbing material and preparation method thereof
CN111410935A (en) MoS2-Fe3O4-graphene ternary composite wave-absorbing material and preparation method thereof
CN112011235A (en) Cobalt-nickel ferrite-based acrylic resin electromagnetic shielding coating and preparation method thereof
CN111587055A (en) Ni-doped ZnFe2O4-carbon nano fiber-epoxy resin wave-absorbing material and preparation method thereof
CN109796932A (en) A kind of composite wave-suction material and preparation method thereof
CN111647272A (en) High-thermal-conductivity modified silicone rubber composite wave-absorbing material and preparation method thereof
CN115915738A (en) HOF-derived one-dimensional Ni-doped magnetic carbon-based nano composite material and preparation method thereof
CN108483506A (en) A kind of preparation method of barium ferrite@C composite wave-suction materials
CN111423808A (en) Anti-corrosion polyaniline-modified polyurethane electromagnetic shielding coating and preparation method thereof
CN105950111A (en) Preparation method and application of composite wave absorbing material of graphene and zeolite

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200728