CN112226203A - Hollow microsphere core-shell structure wave-absorbing material and preparation method and application thereof - Google Patents
Hollow microsphere core-shell structure wave-absorbing material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a hollow microsphere core-shell structure wave-absorbing material, and a preparation method and application thereof. Including Fe3O4Hollow microsphere, ZnO coating Fe3O4Outer surface of hollow microspheres, Fe3O4The hollow microspheres are a hollow porous structure. With FeCl3·6H2Preparing Fe by taking O, polyvinylpyrrolidone (PVP), urea and glycol as raw materials and adopting a hydrothermal method3O4Hollow microspheres; with Zn (Ac)2·2H2O and absolute ethyl alcohol are mixed and react in an alkaline environment to obtain ZnO coated Fe3O4The hollow core-shell microsphere wave-absorbing material. Has better wave-absorbing performance and certain loss to the electromagnetic wave of each wave band.
Description
Technical Field
The invention belongs to the technical field of electromagnetic wave absorbing materials, and particularly relates to a hollow microsphere core-shell structure wave absorbing material, and a preparation method and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
In the information age, electromagnetic pollution caused by electromagnetic waves having electromagnetic radiation characteristics such as radio waves, microwaves, infrared rays, ultraviolet rays, and the like, has become one of the most serious pollution problems in the world at present. Excessive electromagnetic radiation can cause abnormal operation of communication systems and precision instruments, and can also have adverse effects on the immune system of the human body. Therefore, it is a research focus to develop a new electromagnetic shielding material with high efficiency, light weight and low density to reduce the electromagnetic radiation pollution.
The electromagnetic shielding material attenuates and consumes electromagnetic waves through the reflection, absorption and guide effects on electromagnetic energy flow and through modes of resistance type loss, dielectric type loss, magnetic loss and the like, electromagnetic energy transmission between a shielded area and the outside is blocked, and therefore the electromagnetic radiation problem is effectively solved. At present, the electromagnetic shielding materials are mainly divided into carbon series wave-absorbing materials, iron series wave-absorbing materials, ceramic series wave-absorbing materials and the like. Wherein, Fe3O4Better magnetic property can attenuate electromagnetic waves through magnetic loss, but better impedance matching and efficient microwave attenuation are difficult to achieve simultaneously only by means of a single loss mechanism of a single material, and Fe3O4Materials are difficult to completely attenuate and dissipate electromagnetic waves due to poor impedance matching.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a hollow microsphere core-shell structure wave-absorbing material, and a preparation method and application thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows:
in a first aspect, the hollow microsphere core-shell structure wave-absorbing material comprises Fe3O4Hollow microsphere, ZnO coating Fe3O4Hollow micro-meterOuter surface of the ball, Fe3O4The hollow microspheres are a hollow porous structure.
Fe3O4The hollow microsphere is a hollow porous structure, and the hollow porous structure has a good electromagnetic wave absorption effect. Electromagnetic waves are absorbed mainly by dielectric type losses and magnetic losses. After the electromagnetic shielding material is prepared, the electromagnetic shielding material has good wave absorbing performance and has certain loss on electromagnetic waves of various wave bands.
According to the special core-shell structure, zinc oxide is a dielectric material, ferroferric oxide is a magnetic material, interface polarization is generated on a joint surface between the two materials, and the hollow structure of the ferroferric oxide hollow sphere is added, so that the incident electromagnetic wave can be reflected and lost for multiple times at the interface and in the cavity to achieve the purpose of reducing the electromagnetic wave.
In some embodiments of the invention, Fe3O4The particle size of the hollow microspheres is 300-600 nm.
In some embodiments of the invention, the particle size of the hollow microsphere core-shell structure wave-absorbing material is 400-700 nm.
The hollow microsphere core-shell structure wave-absorbing material has better wave-absorbing performance under the combined action of the range of particle size and the hollow structure. In a certain particle size range, the method is favorable for the effect of interface polarization on wave absorption.
In a second aspect, the preparation method of the hollow microsphere core-shell structure wave-absorbing material comprises the following specific steps:
with FeCl3·6H2Preparing Fe by taking O, polyvinylpyrrolidone (PVP), urea and glycol as raw materials and adopting a hydrothermal method3O4Hollow microspheres;
the obtained Fe3O4Hollow microspheres with Zn (Ac)2·2H2O and absolute ethyl alcohol are mixed and react in an alkaline environment to obtain ZnO coated Fe3O4The hollow core-shell microsphere wave-absorbing material.
Preparation of Fe3O4The reduction reaction is generated in the process of hollow microspheres, namely, trivalent iron is partially reduced into divalent iron by ethylene glycol, and the divalent iron is generated by urea hydrolysisIn alkaline environment, obtaining hollow ferroferric oxide by hydrothermal method.
The obtained ferroferric oxide is of a hollow porous structure, in the reaction raw materials, urea is decomposed at high temperature to generate bubbles, so that nano particles can generate a hollow state, and ferric iron in ferric trichloride is partially reduced, so that the product contains the ferroferric oxide.
In some embodiments of the invention, FeCl3·6H2O, PVP, the proportion of urea and glycol is as follows: 0.8-1.5g, 1.5-2.5g, 3-5g, 4-5 mL; preferably 1.1g:2g:4g:4.5 mL.
In some embodiments of the invention, the temperature of the hydrothermal reaction is 180-; preferably, the temperature of the hydrothermal reaction is 200 ℃ and the time of the hydrothermal reaction is 30 h. Fe obtained when the hydrothermal reaction time is 30h3O4The hollow core-shell microsphere wave-absorbing material has better wave-absorbing performance.
The duration of the hydrothermal reaction influences the Fe obtained3O4The hollow microspheres have wave-absorbing property. Too long or too short hydrothermal reaction time is not favorable for increasing Fe3O4The hollow microspheres have wave-absorbing property. The wall thickness of the ferroferric oxide is increased due to the prolonging of the hydrothermal time, the cavity is reduced, and the reflection loss of electromagnetic waves is reduced.
In some embodiments of the invention, Fe3O4Hollow microspheres with Zn (Ac)2·2H2The proportion of O and absolute ethyl alcohol is 0.8-1.2g:6-7g:80-120 mL; preferably 1g:6.8g:100 mL.
In some embodiments of the invention, Fe3O4Hollow microspheres with Zn (Ac)2·2H2The temperature of the O reaction is 50-70 ℃, and the reaction time is 3-5 h; preferably, the reaction temperature is 60 ℃ and the reaction time is 4 h.
Fe3O4The hollow microsphere is prepared by firstly adding ferric ions, then reducing and oxidizing to obtain ferroferric oxide, and if the ferrous ions are directly added and oxidized again, the obtained product contains ferric oxide. The method for preparing ferroferric oxide by firstly adding ferric ions, then reducing and oxidizingThe method can greatly reduce the content of ferric oxide.
Ethylene glycol and urea with FeCl3·6H2O and polyvinylpyrrolidone are added in an amount which is helpful for obtaining the magnetic ferroferric oxide material.
In some embodiments of the invention, the alkaline environment is maintained by adding sodium hydroxide in absolute ethanol, Fe3O4The ratio of the hollow microspheres to the anhydrous ethanol solution of sodium hydroxide is 1g:240-260 mL; preferably 1g:250 mL.
Further, the mass concentration of the anhydrous ethanol solution of the sodium hydroxide is 0.005-0.015 g/mL; preferably 0.01 g/mL.
In a third aspect, the hollow microsphere core-shell structure wave-absorbing material is applied to the field of electromagnetic shielding materials.
In a fourth aspect, the electromagnetic shielding material comprises the hollow microsphere core-shell structure wave-absorbing material and paraffin.
Preferably, the mass fraction of the hollow microsphere core-shell structure wave-absorbing material in the electromagnetic shielding material is 50-70%; preferably 65 to 75%; more preferably 70%.
The wave-absorbing performance is influenced by the adding quality of the hollow microsphere core-shell structure wave-absorbing material in the battery shielding material, and the wave-absorbing performance can be better exerted within a certain adding amount range.
In a fifth aspect, a method for preparing the electromagnetic shielding material comprises:
firstly, melting paraffin, then mixing the hollow microsphere core-shell structure wave-absorbing material with the paraffin, and cooling.
One or more technical schemes of the invention have the following beneficial effects:
preparation of Fe by hydrothermal method and sol-gel method respectively3O4Hollow microspheres of (2) and ZnO-coated Fe3O4The hollow microsphere core-shell structure material. The preparation method has simple flow, easy operation and lower cost. The hollow core-shell microspheres of zinc oxide coated ferroferric oxide prepared by the method have uniform size, and the size can be effectively regulated and controlled through test parameters. Not only asThe uniformly dispersed zinc oxide coated ferroferric oxide hollow core-shell microspheres can improve impedance matching and increase dielectric loss on the premise of keeping the original magnetic loss performance of the material, so that the integral wave-absorbing performance of the ferroferric oxide magnetic material is optimized.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the invention and not to limit the invention.
FIG. 1a Fe prepared in example 13O4SEM image of the hollow microspheres of (a);
FIG. 1b is an SEM image of example 1 after ZnO cladding;
FIG. 2a shows Fe prepared in example 13O4TEM images of the hollow microspheres of (a);
FIG. 2b is a TEM image of the ZnO prepared in example 1 after coating;
FIG. 3 is ZnO coated Fe prepared in example 13O4The XRD pattern of the hollow microsphere core-shell structure wave-absorbing material;
FIG. 4a is a graph showing real and imaginary parts of dielectric constants of the electromagnetic shielding materials of example 4 and comparative example 1, ε' represents the real part, and ε "represents the imaginary part;
FIG. 4b is a graph showing the real and imaginary parts of the magnetic permeability of the electromagnetic shielding materials of example 4 and comparative example 1, where μ' denotes the real part and μ "denotes the imaginary part;
FIG. 4c shows real and imaginary parts of dielectric constants of the electromagnetic shielding materials of example 5 and comparative example 2, ε' represents the real part, and ε "represents the imaginary part;
FIG. 4d shows the real and imaginary parts of the magnetic permeability of the electromagnetic shielding materials of example 5 and comparative example 2, where μ' denotes the real part and μ "denotes the imaginary part;
FIG. 5a is a graph showing reflection loss of the electromagnetic shielding material according to example 4;
FIG. 5b is a graph showing reflection loss of the electromagnetic shielding material according to example 5;
fig. 5c is a graph showing reflection loss of the electromagnetic shielding material of comparative example 1;
FIG. 5d is a graph showing reflection loss of the electromagnetic shielding material of comparative example 2;
FIG. 6a is a graph showing reflection loss of the electromagnetic shielding material according to example 6;
FIG. 6b is a graph showing reflection loss of the electromagnetic shielding material according to example 7;
fig. 6c is a graph showing reflection loss of the electromagnetic shielding material of comparative example 3;
fig. 6d is a reflection loss graph of the electromagnetic shielding material of comparative example 4.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise. The invention will be further illustrated by the following examples
Example 1
(1) 45mL of ethylene glycol was weighed, and 1.1g of FeCl was added thereto3·6H2Placing the mixed solution on a magnetic stirrer, stirring the mixed solution until the mixed solution is transparent, and then carrying out ultrasonic homogenization on the mixed solution; transferring the obtained solution to a reaction kettle with a polytetrafluoroethylene lining, placing the reaction kettle in an electric heating blast box, heating to 200 ℃, keeping the temperature for 30 hours, and naturally cooling to room temperature to obtain Fe3O4The hollow microspheres of (1).
(2) 0.68g of Zn (Ac) was added under ultrasonic agitation2·2H2O and 0.1g of Fe prepared in step (1)3O4Adding the hollow microspheres into 100mL of absolute ethyl alcohol; then 25mL of an alcoholic solution containing 0.25g NaOH was added dropwise in a water bath at 60 ℃. Mechanical stirring after the completion of the dropwise additionAnd 4h, separating the obtained product from the solvent by using a magnet, washing the product with absolute ethyl alcohol and deionized water for multiple times, and drying the product. To obtain ZnO coated Fe3O4The hollow microsphere core-shell structure material.
FIG. 1a shows Fe obtained in step (1) of example 13O4As shown in FIG. 1a, the surface morphology of the hollow microspheres of (1) was complete when the amount of urea was 4g and the hydrothermal time was 30 hours. As shown in FIG. 2a, when the amount of urea was 4g and the hydrothermal time was 30 hours, the thickness of the hollow spherical shell layer was 100 to 150 nm.
It can be seen from FIGS. 2a and 2b that Fe produced in step (1)3O4Is a hollow structure.
FIG. 3 shows ZnO-coated Fe obtained in example 13O4The XRD pattern of the hollow microsphere core-shell structure material.
Example 2:
compared with the example 1, the heating time in the step (1) is 36h, and other conditions are not changed. To obtain Fe3O4The hollow microspheres of (1).
The operation of step (2) was the same as in example 1 to obtain ZnO-coated Fe3O4The hollow microsphere core-shell structure material.
Example 3:
the amount of urea in step (1) was changed to 6g compared to example 1, and the other conditions were not changed. To obtain Fe3O4The hollow microspheres of (1). Step (2) is the same as in example 1.
Example 4
Paraffin was melted, and the ZnO of example 1 was coated with Fe3O4The hollow microsphere core-shell structure material is mixed with molten paraffin to obtain the electromagnetic shielding material, wherein ZnO coats Fe3O4The mass ratio of the hollow microsphere core-shell structure material is 50%.
Example 5
Paraffin was melted, and the ZnO of example 1 was coated with Fe3O4The hollow microsphere core-shell structure material is mixed with molten paraffin to obtain the electromagnetic shielding material, wherein ZnO coats Fe3O4The mass ratio of the hollow microsphere core-shell structure material is70％。
Comparative example 1
Melting of paraffin, Fe prepared in example 13O4The hollow microsphere material is mixed with paraffin to obtain the electromagnetic shielding material, ZnO is coated with Fe3O4The mass ratio of the hollow microsphere core-shell structure material is 50%.
Comparative example 2
Melting of paraffin, Fe prepared in example 13O4The hollow microsphere material is mixed with paraffin to obtain the electromagnetic shielding material, ZnO is coated with Fe3O4The mass ratio of the hollow microsphere core-shell structure material is 70%.
Example 6
The paraffin wax was melted, and the ZnO prepared in example 2 was coated with Fe3O4The hollow microsphere core-shell structure material is mixed with paraffin to obtain the electromagnetic shielding material, wherein ZnO coats Fe3O4The mass ratio of the hollow microsphere core-shell structure material is 50%.
Example 7
The paraffin wax was melted, and the ZnO prepared in example 2 was coated with Fe3O4The hollow microsphere core-shell structure material is mixed with paraffin to obtain the electromagnetic shielding material, wherein ZnO coats Fe3O4The mass ratio of the hollow microsphere core-shell structure material is 70%.
Comparative example 3
Melting of paraffin, Fe prepared in example 23O4The hollow microsphere material is mixed with paraffin to obtain the electromagnetic shielding material, ZnO is coated with Fe3O4The mass ratio of the hollow microsphere core-shell structure material is 50%.
Comparative example 4
Melting of paraffin, Fe prepared in example 23O4The hollow microsphere material is mixed with paraffin to obtain the electromagnetic shielding material, ZnO is coated with Fe3O4The mass ratio of the hollow microsphere core-shell structure material is 70%.
Comparative example 5
In comparison to example 1, the starting material of step (1)FeCl3·6H2Changing O to FeCl2·6H2And O, removing the raw material ethylene glycol. The resulting product is partially magnetic, biased to reddish brown, rather than black, so the resulting product is a mixture of ferric oxide and ferroferric oxide.
Fig. 4a, 4b, 4c, 4d show the real part of the dielectric constant of the electromagnetic shielding material of example 1, which corresponds to the elastic energy storage part, i.e., the part that can be discharged after an input of an electric signal, compared to the real part of the dielectric constant of the electromagnetic shielding material of comparative example 1, as can be seen from fig. 4 a. Therefore, the electromagnetic shielding material of embodiment 4 has a good wave-absorbing property.
As can be seen from fig. 4b and 4d, the magnetic properties of the material after coating are not significantly affected.
It can be seen from fig. 4c that the electromagnetic shielding material of example 5 has better wave-absorbing property compared to the real part of the dielectric constant of the electromagnetic shielding material of comparative example 2. And ZnO coated Fe can be obtained3O4The hollow microsphere core-shell structure material has better wave-absorbing performance with the mass ratio of 70 percent.
As can be seen from fig. 5a, 5b, 5c, 5d, the uncoated material has a strong reflection loss at some thicknesses but a too small reflection loss at the remaining wavelength bands and thicknesses. And after coating, the material has certain loss to electromagnetic waves of all wave bands. Where the absorption band of fig. 5b is the broadest, the absorption band of fig. 5b is larger than the absorption band of fig. 5 a. The absorption bands of fig. 5c and 5d are narrower.
As can be seen from fig. 6a, 6b, 6c, 6d, the uncoated material has a strong reflection loss at some thickness but a too small reflection loss at the remaining wavelength bands and thicknesses. And after coating, the material has certain loss to electromagnetic waves of all wave bands. And example 2 preparation of ZnO coated Fe3O4Compared with ZnO coated Fe in example 1, the hollow microsphere core-shell structure material3O4The hollow microsphere core-shell structure material has weaker wave-absorbing performance.
Example 3 the resulting ZnO coated Fe compared to example 13O4Hollow microsphere core-shell structureThe wave absorbing performance of the structural material is weaker.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A hollow microsphere core-shell structure wave-absorbing material is characterized in that: including Fe3O4Hollow microsphere, ZnO coating Fe3O4Outer surface of hollow microspheres, Fe3O4The hollow microspheres are a hollow porous structure.
2. The hollow microsphere core-shell structure wave-absorbing material of claim 1, which is characterized in that: fe3O4The particle size of the hollow microspheres is 300-600 nm.
3. The hollow microsphere core-shell structure wave-absorbing material of claim 1, which is characterized in that: the particle size of the hollow microsphere core-shell structure wave-absorbing material is 400-700 nm.
4. The preparation method of the hollow microsphere core-shell structure wave-absorbing material of any one of claims 1 to 3, which is characterized by comprising the following steps: the method comprises the following specific steps:
with FeCl3·6H2Preparing Fe by taking O, polyvinylpyrrolidone, urea and ethylene glycol as raw materials and adopting a hydrothermal method3O4Hollow microspheres;
the obtained Fe3O4Hollow microspheres with Zn (Ac)2·2H2O and absolute ethyl alcohol are mixed and react in an alkaline environment to obtain ZnO coated Fe3O4The hollow core-shell microsphere wave-absorbing material;
preferably, the alkaline environment is maintained by adding an absolute ethanol solution of sodium hydroxide;
further preferably, the mass concentration of the anhydrous ethanol solution of sodium hydroxide is 0.005-0.015 g/mL; preferably 0.01 g/mL.
5. The preparation method of the hollow microsphere core-shell structure wave-absorbing material of claim 4, which is characterized by comprising the following steps: FeCl3·6H2O, PVP, the proportion of urea and glycol is as follows: 0.8-1.5g, 1.5-2.5g, 3-5g, 4-5 mL; preferably 1.1g:2g:4g:4.5 mL.
6. The preparation method of the hollow microsphere core-shell structure wave-absorbing material of claim 4, which is characterized by comprising the following steps: the temperature of the hydrothermal reaction is 180 ℃ and 220 ℃, and the time of the hydrothermal reaction is 24-36 h; preferably, the temperature of the hydrothermal reaction is 200 ℃, and the time of the hydrothermal reaction is 30 h;
or, Fe3O4Hollow microspheres with Zn (Ac)2·2H2The proportion of O and absolute ethyl alcohol is 0.8-1.2g:6-7g:80-120 mL; preferably 1g:6.8g:100 mL.
7. The preparation method of the hollow microsphere core-shell structure wave-absorbing material of claim 4, which is characterized by comprising the following steps: fe3O4Hollow microspheres with Zn (Ac)2·2H2The temperature of the O reaction is 50-70 ℃, and the reaction time is 3-5 h; preferably, the reaction temperature is 60 ℃ and the reaction time is 4 h.
8. The hollow microsphere core-shell structure wave-absorbing material of any one of claims 1 to 3, which is applied to the field of electromagnetic shielding materials.
9. An electromagnetic shielding material, characterized in that: the wave-absorbing material comprises the hollow microsphere core-shell structure wave-absorbing material and paraffin;
preferably, the mass fraction of the hollow microsphere core-shell structure wave-absorbing material in the electromagnetic shielding material is 50-70%; preferably 65 to 75%; more preferably 70%.
10. The method for preparing an electromagnetic shielding material of claim 9, wherein: the method comprises the following steps: firstly, melting paraffin, then mixing the hollow microsphere core-shell structure wave-absorbing material with the paraffin, and cooling.
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