CN111909514A - polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof - Google Patents

polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof Download PDF

Info

Publication number
CN111909514A
CN111909514A CN202010807666.3A CN202010807666A CN111909514A CN 111909514 A CN111909514 A CN 111909514A CN 202010807666 A CN202010807666 A CN 202010807666A CN 111909514 A CN111909514 A CN 111909514A
Authority
CN
China
Prior art keywords
doped zno
polyaniline
nano
absorbing material
wave
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.)
Withdrawn
Application number
CN202010807666.3A
Other languages
Chinese (zh)
Inventor
庞焕林
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 CN202010807666.3A priority Critical patent/CN111909514A/en
Publication of CN111909514A publication Critical patent/CN111909514A/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/22—Expanded, porous or hollow particles
    • C08K7/24—Expanded, porous or hollow particles inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/22—Compounds of iron
    • C09C1/24—Oxides of iron
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01Q—ANTENNAS, i.e. RADIO AERIALS
    • H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
    • H01Q17/004—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems using non-directional dissipative particles, e.g. ferrite powders
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Abstract

The invention relates to the field of wave-absorbing materials and discloses polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material, nano-Fe3O4The hollow microsphere has the characteristics of small density and light weight, can perform multiple scattering on electromagnetic waves to generate scattering and polarization effects, and enhances the electromagnetic wave resistance of the composite materialIn nano-Fe3O4A echinoid nano Co-doped ZnO coating layer is generated on the surface of the hollow microsphere, the echinoid shape of the hollow microsphere is specially needled, the reflectivity of incident electromagnetic waves is favorably adjusted, the impedance matching performance of the material is improved, meanwhile, the Co doping replaces partial Zn crystal lattices, obvious ferromagnetism is shown, a good magnetic loss mechanism is realized, p-toluenesulfonic acid is used as proton doping acid, and the echinoid nano Co-doped ZnO modifies Fe3O4Conductive polymer polyaniline is generated on the surface, and the impedance matching characteristic of the composite material is adjusted, so that the composite wave-absorbing material has excellent wave-absorbing performance of dielectric loss and magnetic loss.

Description

polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof
Technical Field
The invention relates to the field of wave-absorbing materials, in particular to polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and its preparation method.
Background
With the rapid development of electronic information technology, various high-frequency electronic devices are widely used in our daily life, the generated electromagnetic waves and electromagnetic radiation are also larger and larger, electromagnetic radiation pollution becomes another current big social pollution, the human body is exposed to the electromagnetic waves and electromagnetic radiation for a long time, an immune system, a reproductive system, an audio-visual system and the like can be influenced, various diseases are induced, and the strong electromagnetic radiation can cause the normal operation of a navigation system, an electronic precision instrument and the like, so that the development of a novel high-efficiency, light-weight and low-cost electromagnetic shielding and wave absorbing material becomes a research hotspot.
The traditional electromagnetic shielding materials mainly comprise carbon-series wave-absorbing materials such as graphene, carbon fiber and the like, and iron-series wave-absorbing materials such as carbonyl iron, ferrite and the like; the ceramic wave-absorbing material, such as silicon carbide and the like, zinc oxide is a multifunctional semiconductor material, has wide application in the aspects of electrode materials, gas-sensitive elements and the like, has good dielectric loss characteristics, can compound zinc oxide with magnetic materials, such as ferrite and the like, and can obtain the wave-absorbing material with excellent performance.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides high-efficiency polyaniline-Co doped ZnO-Fe3O4The composite wave-absorbing material and the preparation method thereof have excellent wave-absorbing performance.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material: the polyaniline-Co is doped with ZnO-Fe3O4The preparation method of the composite wave-absorbing material comprises the following steps:
(1) adding a glycol solvent, ferric chloride and ammonium bicarbonate into a reaction bottle, uniformly stirring, placing the solution into a hydrothermal reaction device, heating to 180 ℃ for 200 ℃, reacting for 10-15h, centrifugally separating to remove the solvent, washing with distilled water and drying to prepare the nano Fe3O4Hollow microspheres.
(2) Into a reaction flaskAdding distilled water solvent, zinc acetate, cobalt acetate and nano Fe3O4Adding sodium hydroxide into hollow microspheres after uniform ultrasonic dispersion, placing the solution in a hydrothermal reaction device, heating to 120 ℃ for reaction for 10-20h, filtering to remove the solvent, washing with distilled water and ethanol, and drying to obtain urchin-shaped nano Co-doped ZnO modified Fe3O4。
(3) Adding aqueous solution of p-toluenesulfonic acid and echinoid nano Co-doped ZnO modified Fe into a reaction bottle3O4Placing the polyaniline-Co doped ZnO-Fe in an ice water bath after ultrasonic dispersion is uniform, adding aniline and stirring uniformly, slowly dropwise adding an initiator potassium persulfate solution, stirring at a constant speed and reacting for 12-24h, filtering to remove the solvent, washing with a distilled water solvent and ethanol, and drying to obtain the polyaniline-Co doped ZnO-Fe3O4A composite wave-absorbing material.
Preferably, the mass ratio of the ferric chloride to the ammonium bicarbonate in the step (1) is 10: 40-50.
Preferably, the inner wall of the hydrothermal reaction device in the step (1) is fixedly connected with a heating plate, the inner lower part of the hydrothermal reaction device is fixedly connected with a motor, the motor is movably connected with a rotating shaft, a supporting rod is fixedly connected above the rotating shaft, the supporting rod is fixedly connected with a reaction chamber, an expansion spring is fixedly connected inside the reaction chamber, the expansion spring is fixedly connected with a clamping plate, and the clamping plate is movably connected with a hydrothermal reaction kettle.
Preferably, the zinc acetate, the cobalt acetate and the nano Fe in the step (2)3O4The mass ratio of the hollow microspheres to the sodium hydroxide is 100:4-8:9-13: 280-330.
Preferably, the mass fraction of the p-toluenesulfonic acid aqueous solution in the step (3) is 0.5-1%.
Preferably, the urchin-shaped nano Co-doped ZnO modified Fe in the step (3)3O4The mass ratio of the aniline to the potassium persulfate is 6-12:100: 220-240.
(III) advantageous technical effects
Compared with the prior art, the invention has the following experimental principles and beneficial technical effects:
the polyphenyl is prepared byamine-Co doped ZnO-Fe3O4The composite wave-absorbing material is prepared by taking ammonium bicarbonate as a template agent in an ethylene glycol reduction hydrothermal system to obtain nano Fe3O4The hollow microsphere has unique hollow shape, has the characteristics of small density and light weight, can perform multiple scattering on electromagnetic waves to generate scattering and polarization effects, thereby enhancing the absorption and attenuation of the composite material on the electromagnetic waves, and has Fe nanoparticles3O4The sea urchin-shaped nano Co-doped ZnO coating layer is generated on the surface of the hollow microsphere, the sea urchin-shaped nano Co-doped ZnO is formed by stacking Co-doped ZnO nanotubes, the special needling sea urchin-shaped appearance is favorable for adjusting the reflectivity of incident electromagnetic waves, so that the impedance matching performance of the material is improved, meanwhile, the Co-doping replaces partial Zn crystal lattices, obvious ferromagnetism is shown, a good magnetic loss mechanism is realized, p-toluenesulfonic acid is used as proton doping acid, and Fe is modified by the sea urchin-shaped nano Co-doped ZnO3O4Conductive polymer polyaniline is generated on the surface, and the impedance matching characteristic of the composite material is adjusted, so that the composite wave-absorbing material has excellent wave-absorbing performance and impedance matching performance of dielectric loss and magnetic loss, and meets the requirements of thinness, lightness, width and strength of the wave-absorbing material.
Drawings
FIG. 1 is a schematic front view of a hydrothermal reaction apparatus;
FIG. 2 is an enlarged schematic view of the reaction chamber;
figure 3 is a schematic diagram of card adjustment.
1-a hydrothermal reaction device; 2-heating plate; 3, a motor; 4-a rotating shaft; 5-a support rod; 6-a reaction chamber; 7-a telescopic spring; 8-clamping plate; 9-hydrothermal reaction kettle.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material: the preparation method comprises the following steps:
(1) adding ethylene glycol solvent, ferric chloride and ammonium bicarbonate with the mass ratio of 10:40-50 into a reaction bottle, uniformly stirring, placing the solution into a hydrothermal reaction device, wherein the inner wall of the hydrothermal reaction device is fixedly connected with a heaterThe piece, the inside below fixedly connected with motor of hydrothermal reaction unit, motor swing joint has the rotation axis, fixedly connected with bracing piece above the rotation axis, bracing piece fixed connection has the reaction chamber, the inside fixedly connected with expanding spring of reaction chamber, expanding spring fixedly connected with cardboard, cardboard swing joint has the hydrothermal reaction kettle, the heating is to 180 set aside a temperature 200 ℃, the reaction is 10-15h, centrifugal separation removes the solvent, use distilled water washing and drying, the preparation obtains nanometer Fe3O4Hollow microspheres.
(2) Adding distilled water solvent, zinc acetate, cobalt acetate and nano Fe into a reaction bottle3O4Uniformly dispersing hollow microspheres by ultrasonic, adding sodium hydroxide with the mass ratio of 100:4-8:9-13:280-330, placing the solution in a hydrothermal reaction device, heating to 100-120 ℃, reacting for 10-20h, filtering to remove the solvent, washing with distilled water and ethanol, and drying to obtain the urchin-shaped nano Co-doped ZnO modified Fe3O4。
(3) Adding 0.5-1% of p-toluenesulfonic acid aqueous solution and echinoid nano Co-doped ZnO modified Fe into a reaction bottle3O4Ultrasonic dispersing uniformly, placing in ice-water bath, adding aniline, stirring uniformly, slowly dripping initiator potassium persulfate solution, wherein sea urchin-shaped nano Co is doped with ZnO to modify Fe3O4Aniline and potassium persulfate in the mass ratio of 6-12:100:220-240, stirring at constant speed for reaction for 12-24h, filtering to remove the solvent, washing with distilled water solvent and ethanol, and drying to obtain polyaniline-Co doped ZnO-Fe3O4A composite wave-absorbing material.
Example 1
(1) Adding ethylene glycol solvent, ferric chloride and ammonium bicarbonate with the mass ratio of 10:40 into a reaction bottle, uniformly stirring, placing the solution into a hydrothermal reaction device, fixedly connecting a heating sheet on the inner wall of the hydrothermal reaction device, fixedly connecting a motor below the interior of the hydrothermal reaction device, movably connecting the motor with a rotating shaft, fixedly connecting a supporting rod above the rotating shaft, fixedly connecting the supporting rod with a reaction chamber, fixedly connecting an expansion spring inside the reaction chamber, fixedly connecting the expansion spring with a clamping plate, movably connecting the clamping plate with a hydrothermal reaction kettle,heating to 180 ℃, reacting for 10h, centrifugally separating to remove the solvent, washing with distilled water and drying to prepare the nano Fe3O4Hollow microspheres.
(2) Adding distilled water solvent, zinc acetate, cobalt acetate and nano Fe into a reaction bottle3O4Ultrasonically dispersing the hollow microspheres uniformly, adding sodium hydroxide with the mass ratio of 100:4:9:280, placing the solution in a hydrothermal reaction device, heating to 100 ℃, reacting for 10 hours, filtering to remove the solvent, washing with distilled water and ethanol, and drying to obtain urchin-shaped nano Co-doped ZnO modified Fe3O4。
(3) Adding 0.5 mass percent of p-toluenesulfonic acid aqueous solution and echinoid nano Co-doped ZnO modified Fe into a reaction bottle3O4Ultrasonic dispersing uniformly, placing in ice-water bath, adding aniline, stirring uniformly, slowly dripping initiator potassium persulfate solution, wherein sea urchin-shaped nano Co is doped with ZnO to modify Fe3O4The mass ratio of aniline to potassium persulfate is 6:100:220, the mixture is stirred at a constant speed for reaction for 12 hours, the solvent is removed by filtration, and the mixture is washed and dried by using distilled water solvent and ethanol to prepare polyaniline-Co doped ZnO-Fe3O4A composite wave-absorbing material 1.
Example 2
(1) Adding ethylene glycol solvent, ferric chloride and ammonium bicarbonate with the mass ratio of 10:42 into a reaction bottle, uniformly stirring, then placing the solution into a hydrothermal reaction device, wherein the inner wall of the hydrothermal reaction device is fixedly connected with a heating sheet, the lower part inside the hydrothermal reaction device is fixedly connected with a motor, the motor is movably connected with a rotating shaft, the upper part of the rotating shaft is fixedly connected with a supporting rod, the supporting rod is fixedly connected with a reaction chamber, the inside of the reaction chamber is fixedly connected with a telescopic spring, the telescopic spring is fixedly connected with a clamping plate, the clamping plate is movably connected with a hydrothermal reaction kettle, heating is carried out to 180 ℃, reacting for 15 hours, centrifugally separating to remove the solvent, washing with distilled water and3O4hollow microspheres.
(2) Adding distilled water solvent, zinc acetate, cobalt acetate and nano Fe into a reaction bottle3O4Hollow microspheres are added after being uniformly dispersed by ultrasonicSodium hydroxide with the mass ratio of 100:5:10:295, placing the solution in a hydrothermal reaction device, heating to 120 ℃, reacting for 20 hours, filtering to remove the solvent, washing with distilled water and ethanol, and drying to obtain urchin-shaped nano Co-doped ZnO modified Fe3O4。
(3) Adding 0.7 mass percent of p-toluenesulfonic acid aqueous solution and echinoid nano Co-doped ZnO modified Fe into a reaction bottle3O4Ultrasonic dispersing uniformly, placing in ice-water bath, adding aniline, stirring uniformly, slowly dripping initiator potassium persulfate solution, wherein sea urchin-shaped nano Co is doped with ZnO to modify Fe3O4The mass ratio of aniline to potassium persulfate is 8:100:225, the mixture is stirred at a constant speed for reaction for 24 hours, the solvent is removed by filtration, and the polyaniline-Co doped ZnO-Fe is prepared by washing and drying the mixture by using a distilled water solvent and ethanol3O4And (3) composite wave-absorbing material 2.
Example 3
(1) Adding ethylene glycol solvent, ferric chloride and ammonium bicarbonate with the mass ratio of 10:46 into a reaction bottle, uniformly stirring, then placing the solution into a hydrothermal reaction device, wherein the inner wall of the hydrothermal reaction device is fixedly connected with a heating sheet, the lower part inside the hydrothermal reaction device is fixedly connected with a motor, the motor is movably connected with a rotating shaft, the upper part of the rotating shaft is fixedly connected with a supporting rod, the supporting rod is fixedly connected with a reaction chamber, the inside of the reaction chamber is fixedly connected with a telescopic spring, the telescopic spring is fixedly connected with a clamping plate, the clamping plate is movably connected with a hydrothermal reaction kettle, heating is carried out to 190 ℃, reacting for 12 hours, centrifugally separating to remove the solvent, washing with distilled water and3O4hollow microspheres.
(2) Adding distilled water solvent, zinc acetate, cobalt acetate and nano Fe into a reaction bottle3O4Ultrasonically dispersing hollow microspheres uniformly, adding sodium hydroxide with the mass ratio of 100:7:11.5:310, placing the solution in a hydrothermal reaction device, heating to 110 ℃, reacting for 15h, filtering to remove the solvent, washing with distilled water and ethanol, and drying to obtain urchin-shaped nano Co-doped ZnO modified Fe3O4。
(3) Adding mass fraction into a reaction flask0.8% p-toluenesulfonic acid aqueous solution and echinoid nano Co-doped ZnO modified Fe3O4Ultrasonic dispersing uniformly, placing in ice-water bath, adding aniline, stirring uniformly, slowly dripping initiator potassium persulfate solution, wherein sea urchin-shaped nano Co is doped with ZnO to modify Fe3O4The mass ratio of the aniline to the potassium persulfate is 10:100:235, the mixture is stirred at a constant speed for reaction for 18 hours, the solvent is removed by filtration, and the polyaniline-Co doped ZnO-Fe is prepared by washing and drying the mixture by using a distilled water solvent and ethanol3O4And (3) composite wave-absorbing material.
Example 4
(1) Adding ethylene glycol solvent, ferric chloride and ammonium bicarbonate with the mass ratio of 10:50 into a reaction bottle, uniformly stirring, then placing the solution into a hydrothermal reaction device, wherein the inner wall of the hydrothermal reaction device is fixedly connected with a heating sheet, the lower part inside the hydrothermal reaction device is fixedly connected with a motor, the motor is movably connected with a rotating shaft, the upper part of the rotating shaft is fixedly connected with a supporting rod, the supporting rod is fixedly connected with a reaction chamber, the inside of the reaction chamber is fixedly connected with a telescopic spring, the telescopic spring is fixedly connected with a clamping plate, the clamping plate is movably connected with a hydrothermal reaction kettle, heating is carried out to 200 ℃, reacting for 15 hours, centrifugally separating to remove the solvent, washing with distilled water and3O4hollow microspheres.
(2) Adding distilled water solvent, zinc acetate, cobalt acetate and nano Fe into a reaction bottle3O4Adding sodium hydroxide into hollow microspheres after ultrasonic dispersion is carried out uniformly, placing the solution into a hydrothermal reaction device, heating to 120 ℃, reacting for 20 hours, filtering to remove the solvent, washing by using distilled water and ethanol, and drying to prepare the urchin-shaped nano Co-doped ZnO modified Fe3O4。
(3) Adding 1 percent of water solution of p-toluenesulfonic acid and echinoid nano Co-doped ZnO modified Fe into a reaction bottle3O4Ultrasonic dispersing uniformly, placing in ice-water bath, adding aniline, stirring uniformly, slowly dripping initiator potassium persulfate solution, wherein sea urchin-shaped nano Co is doped with ZnO to modify Fe3O4Aniline and potassium persulfate in a mass ratio ofStirring at a constant speed of 12:100:240, reacting for 24 hours, filtering to remove the solvent, washing with a distilled water solvent and ethanol, and drying to prepare polyaniline-Co doped ZnO-Fe3O4And (4) composite wave-absorbing material.
Comparative example 1
(1) Adding ethylene glycol solvent, ferric chloride and ammonium bicarbonate with the mass ratio of 10:35 into a reaction bottle, uniformly stirring, then placing the solution into a hydrothermal reaction device, wherein the inner wall of the hydrothermal reaction device is fixedly connected with a heating sheet, the lower part inside the hydrothermal reaction device is fixedly connected with a motor, the motor is movably connected with a rotating shaft, the upper part of the rotating shaft is fixedly connected with a supporting rod, the supporting rod is fixedly connected with a reaction chamber, the inside of the reaction chamber is fixedly connected with an expansion spring, the expansion spring is fixedly connected with a clamping plate, the clamping plate is movably connected with a hydrothermal reaction kettle, heating is carried out to 180 ℃, reacting for 15 hours, centrifugally separating to remove the solvent, washing with distilled water and3O4hollow microspheres.
(2) Adding distilled water solvent, zinc acetate, cobalt acetate and nano Fe into a reaction bottle3O4Ultrasonically dispersing the hollow microspheres uniformly, adding sodium hydroxide according to the mass ratio of 100:2:7:260, placing the solution in a hydrothermal reaction device, heating to 120 ℃, reacting for 20 hours, filtering to remove the solvent, washing with distilled water and ethanol, and drying to obtain urchin-shaped nano Co-doped ZnO modified Fe3O4。
(3) Adding 1 percent of water solution of p-toluenesulfonic acid and echinoid nano Co-doped ZnO modified Fe into a reaction bottle3O4Ultrasonic dispersing uniformly, placing in ice-water bath, adding aniline, stirring uniformly, slowly dripping initiator potassium persulfate solution, wherein sea urchin-shaped nano Co is doped with ZnO to modify Fe3O4The mass ratio of aniline to potassium persulfate is 4:100:210, the mixture is stirred at a constant speed for reaction for 24 hours, the solvent is removed by filtration, and the mixture is washed and dried by using distilled water solvent and ethanol to prepare polyaniline-Co doped ZnO-Fe3O4Comparison 1 of composite wave-absorbing material.
The polyaniline-Co in the examples and the comparative examples are doped with ZnO-Fe3O4Composite wave absorbing materialThe material and paraffin are uniformly mixed, the mass ratio of the composite wave-absorbing material to the paraffin is 4:6, the mixture is pressed into a ring-shaped sheet with the thickness of 1.5mm, and the wave-absorbing performance of the composite material is tested by using an SVA1032X vector network analyzer, wherein the test standard is GB/T32596-.
Figure BDA0002629733940000081

Claims (6)

1. polyaniline-Co doped ZnO-Fe3O4The composite wave-absorbing material is characterized in that: the polyaniline-Co is doped with ZnO-Fe3O4The preparation method of the composite wave-absorbing material comprises the following steps:
(1) adding ferric chloride and ammonium bicarbonate into ethylene glycol solvent, placing the solution in a hydrothermal reaction device, heating to 180 ℃ and 200 ℃, reacting for 10-15h, centrifugally separating, washing and drying to prepare the nano Fe3O4Hollow microspheres;
(2) adding zinc acetate, cobalt acetate and nano Fe into distilled water solvent3O4Adding sodium hydroxide into hollow microspheres after ultrasonic dispersion is uniform, placing the solution in a hydrothermal reaction device, heating to 120 ℃ for reaction for 10-20h, filtering, washing and drying to prepare urchin-shaped nano Co-doped ZnO modified Fe3O4；
(3) Adding echinoid nano Co doped ZnO modified Fe into water solution of p-toluenesulfonic acid3O4Placing the polyaniline-Co doped ZnO-Fe in ice water bath after ultrasonic dispersion, adding aniline, stirring uniformly, slowly dropwise adding an initiator potassium persulfate solution, reacting for 12-24h, filtering, washing and drying to obtain the polyaniline-Co doped ZnO-Fe3O4A composite wave-absorbing material.
2. The polyaniline-Co doped ZnO-Fe as claimed in claim 13O4The composite wave-absorbing material is characterized in that: the mass ratio of the ferric chloride to the ammonium bicarbonate in the step (1) is 10: 40-50.
3. The polyaniline-Co doped ZnO-Fe as claimed in claim 13O4The composite wave-absorbing material is characterized in that: the hydrothermal reaction device in step (1) inner wall fixedly connected with heating plate, hydrothermal reaction device inside below fixedly connected with motor, motor swing joint has the rotation axis, rotation axis top fixedly connected with bracing piece, bracing piece fixed connection have the reaction chamber, the inside fixedly connected with expanding spring of reaction chamber, expanding spring fixedly connected with cardboard, cardboard swing joint has hydrothermal reaction kettle.
4. The polyaniline-Co doped ZnO-Fe as claimed in claim 13O4The composite wave-absorbing material is characterized in that: zinc acetate, cobalt acetate and nano Fe in the step (2)3O4The mass ratio of the hollow microspheres to the sodium hydroxide is 100:4-8:9-13: 280-330.
5. The polyaniline-Co doped ZnO-Fe as claimed in claim 13O4The composite wave-absorbing material is characterized in that: the mass fraction of the p-toluenesulfonic acid aqueous solution in the step (3) is 0.5-1%.
6. The polyaniline-Co doped ZnO-Fe as claimed in claim 13O4The composite wave-absorbing material is characterized in that: in the step (3), urchin-shaped nano Co-doped ZnO modified Fe3O4The mass ratio of the aniline to the potassium persulfate is 6-12:100: 220-240.
CN202010807666.3A 2020-08-12 2020-08-12 polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof Withdrawn CN111909514A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010807666.3A CN111909514A (en) 2020-08-12 2020-08-12 polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010807666.3A CN111909514A (en) 2020-08-12 2020-08-12 polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof

Publications (1)

Publication Number Publication Date
CN111909514A true CN111909514A (en) 2020-11-10

Family

ID=73284380

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010807666.3A Withdrawn CN111909514A (en) 2020-08-12 2020-08-12 polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111909514A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113278255A (en) * 2021-05-19 2021-08-20 湖南飞鸿达新材料有限公司 High-frequency-band heat-conduction wave-absorbing insulating pad with heat conductivity and wave absorption

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113278255A (en) * 2021-05-19 2021-08-20 湖南飞鸿达新材料有限公司 High-frequency-band heat-conduction wave-absorbing insulating pad with heat conductivity and wave absorption
CN113278255B (en) * 2021-05-19 2022-03-25 湖南飞鸿达新材料有限公司 High-frequency-band heat-conduction wave-absorbing insulating pad with heat conductivity and wave absorption

Similar Documents

Publication Publication Date Title
CN107399735A (en) A kind of preparation method and applications of graphene composite aerogel absorbing material
CN108251054B (en) Composite wave-absorbing material and preparation method thereof
CN108190876B (en) A kind of graphene composite absorber and preparation method thereof
CN111154455B (en) Boron-doped mesoporous flower-like ferroferric oxide/carbon composite wave-absorbing material and preparation method thereof
CN105728743A (en) Preparation method of composite wave absorbing material
CN113248725A (en) Preparation method of electromagnetic wave absorbing material based on MOF derivation and electromagnetic wave absorbing material
CN111748233A (en) Low-reflectivity wave-absorbing material and preparation method thereof
CN106519516B (en) A kind of dielectric composite material and preparation method thereof based on paraffin cladding barium titanate nano particle
CN106883818B (en) Hud typed carbon ball/carbon nano tube composite wave-absorbing material and preparation method
CN109666451A (en) A method of absorbing material is prepared using biomass carbon source
CN111909514A (en) polyaniline-Co doped ZnO-Fe3O4Composite wave-absorbing material and preparation method thereof
CN108530100B (en) Carbon-based wave absorption film and preparation method thereof
CN111410935A (en) MoS2-Fe3O4-graphene ternary composite wave-absorbing material and preparation method thereof
CN111349299A (en) High-thermal-conductivity graphene-SiC-NiO modified acrylic resin electromagnetic shielding material and preparation method thereof
CN106854453A (en) A kind of preparation method of lamellar composite absorbing material
CN106675516B (en) A kind of transition metal chalcogenide-carbonyl iron dust composite microwave absorbent and preparation method thereof
CN111235695B (en) Preparation method of porous carbon fiber electromagnetic wave absorbing agent
CN111393845B (en) Chiral polypyrrole/Fe 3 O 4 Preparation method and application of graphene composite material
CN111205819B (en) Carbon nanotube-aluminum nitride wave absorbing agent and preparation method thereof, carbon nanotube-aluminum nitride composite wave absorbing material and application thereof
CN111491501A (en) Electromagnetic shielding material with conductive polymer coated with nickel ferrite and preparation method thereof
CN105542156B (en) A kind of preparation method of conductive polyaniline nanometer composite microwave absorbing material
CN116200120A (en) Composite wave-absorbing sizing material and preparation method thereof
CN113423255B (en) Core-shell structure Ti 4 O 7 Magnetic metal composite absorbent and preparation method thereof
CN108997685A (en) CCTO/PVDF composite material and preparation method
CN109180070B (en) Flexible hybrid carbon nano wave-absorbing paper and preparation method thereof

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
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20201110