CN113697798A - Preparation method of magnetic graphene nano wave absorbing material - Google Patents

Preparation method of magnetic graphene nano wave absorbing material Download PDF

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CN113697798A
CN113697798A CN202110918495.6A CN202110918495A CN113697798A CN 113697798 A CN113697798 A CN 113697798A CN 202110918495 A CN202110918495 A CN 202110918495A CN 113697798 A CN113697798 A CN 113697798A
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graphene
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graphene oxide
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CN113697798B (en
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吴晓宏
石婷
姚远
秦伟
洪杨
刘杨
卢松涛
李杨
康红军
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Harbin Institute of Technology
Chongqing Research Institute of Harbin Institute of Technology
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Abstract

The invention discloses a preparation method of a magnetic graphene nano wave absorbing material, and belongs to the field of wave absorbing materials. The invention aims to solve the problem that strong magnetic dipole moment effect exists among magnetic metal particles, so that agglomeration is easy to occur among the magnetic metal particles. The method comprises the following steps: firstly, dissolving graphene oxide sponge, acidified carbon nano tubes and cobalt nitrate in deionized water, mechanically stirring until the mixture is uniform, then carrying out electrostatic self-assembly reaction under ultrasound to form one-dimensional nano rolls, and quickly freezing; secondly, freeze drying; and thirdly, carrying out heat treatment under the protection of inert gas. The method effectively inhibits the agglomeration of the magnetic nanoparticles, realizes the effective and uniform dispersion of the magnetic particles, improves the impedance matching degree of the material, increases a heterogeneous interface, improves the interface polarization capability of the material, exerts the synergistic advantages of the magnetic material and the graphene material, and effectively improves the electromagnetic wave absorption performance of the composite material.

Description

Preparation method of magnetic graphene nano wave absorbing material
Technical Field
The invention belongs to the field of wave-absorbing materials; in particular to a preparation method of a magnetic graphene nano wave absorbing material.
Background
With the rapid development of modern electronic technology, a great deal of convenience is provided, and a series of serious problems such as serious electromagnetic interference, electromagnetic information leakage, electromagnetic radiation pollution and the like are brought, so that the preparation of the efficient electromagnetic wave absorbing material is one of effective ways for solving the increasingly serious electromagnetic problems in the civil and military fields.
The electromagnetic wave attenuation capability of the wave-absorbing material is related to the dielectric loss, the magnetic loss, the impedance matching characteristic and the like of the material. The traditional magnetic metal material has the advantages of high saturation magnetization, strong magnetic loss capability, low cost and the like, and is regarded as a good wave-absorbing material, but the magnetic metal wave-absorbing material also has many defects, such as poor dispersibility, large density, easy oxidation, easy corrosion, narrow frequency band and the like. More seriously, because the magnetic metal material has higher self conductivity, a serious skin effect can be generated on the surface of the material, the reflection of electromagnetic waves on the surface of the material is increased, and the absorption effect of the electromagnetic waves is reduced. In recent years, graphene materials are widely concerned by researchers due to light weight, corrosion resistance and high stability, but a single graphene material only has dielectric loss to cause poor impedance matching, so that the single graphene material cannot obtain effective wave-absorbing capacity, and further expansion and application of the single graphene material are limited. In view of this, designing and developing a magnetic graphene-based composite wave-absorbing material with high microwave absorption performance and both dielectric loss and magnetic loss is a problem to be solved at present.
At present, a mixture of a graphene-based material and magnetic metal ions is used as a precursor, special structures such as a core shell, an egg shell and a one-dimensional tubular structure are designed, a heterogeneous interface with polarization loss and gaps for scattering electromagnetic waves can be provided, and the wave absorbing performance can be improved. Due to high anisotropy and high aspect ratio, a carrier transmission path is easy to form along the axial direction under a high-frequency electromagnetic field, and the electromagnetic wave energy is further effectively consumed. However, due to the strong dipole moment between the magnetic substances, the aggregation phenomenon is easily generated between the magnetic metal particles of the one-dimensional magnetic graphene-based composite material, the chemical uniformity of the material is poor, the characteristics of the graphene and the magnetic material are not fully exerted, a large number of heterogeneous interfaces cannot be effectively utilized, and the requirements of the modern wave-absorbing material on thinness, lightness, width and strength are not met. Therefore, it is urgently needed to develop a method for preparing a one-dimensional graphene composite material with uniformly dispersed magnetic nanoparticles for efficient electromagnetic wave absorption.
Disclosure of Invention
According to the traditional one-dimensional magnetic graphene composite material, a strong magnetic dipole moment effect exists among magnetic particles, so that the problem of agglomeration among the magnetic particles is easily caused, the chemical uniformity of the material is poor, the characteristics of graphene and the magnetic material are not fully exerted, a large number of heterogeneous interfaces cannot be effectively utilized, and the requirements of modern wave-absorbing materials on thinness, lightness, width and strength are not met.
The invention provides a preparation method of a one-dimensional magnetic graphene nano-roll composite material, which is characterized in that the one-dimensional graphene nano-roll composite material with magnetic particles uniformly distributed among layers of nano-rolls is prepared by adopting a liquid-phase self-assembly-freeze drying-carbothermic method, so that rich heterogeneous interfaces are provided, the interface polarization effect is enhanced, the dielectric loss capability of the material is improved, and the improvement of the electromagnetic wave absorption performance of the composite material is promoted.
In view of the characteristics of excellent dispersion stability, rich active functional groups on the surface and easiness in assembly of Graphene Oxide (GO), the invention aims to realize the controllable preparation of the one-dimensional magnetic graphene nanocolloid wave-absorbing material by adopting an inorganic salt-carbon tube-graphene oxide three method through a liquid-phase self-assembly-freeze drying-carbothermic reduction method. Due to the structural characteristics of the one-dimensional graphene nano coil, in the carbothermic reduction process, inorganic salt is decomposed into magnetic oxide, and the magnetic oxide undergoes carbothermic reduction reaction to further generate magnetic metal. The amorphous carbon of the graphene oxide forms graphitized carbon under the catalytic action of the magnetic metal nanoparticles, so that magnetic particles are encapsulated in the graphitized carbon to form a core-shell structure and are embedded between layers of the one-dimensional nanocolloid, the agglomeration of magnetic substances is effectively inhibited, the effective uniform dispersion of the magnetic particles is realized, the impedance matching degree of the material is improved, a heterogeneous interface is increased, the interface polarization capability of the material is improved, the synergistic advantages of the magnetic material and the graphene material are exerted, and excellent wave-absorbing performance is obtained.
The purpose of the invention is realized by the following technical scheme, and the preparation method of the magnetic graphene nano wave absorbing material is carried out according to the following steps:
dissolving graphene oxide sponge, an acidified carbon nanotube and cobalt nitrate in deionized water, mechanically stirring until the mixture is uniform, performing electrostatic self-assembly reaction under ultrasound to form a one-dimensional nano coil, and quickly freezing;
step two, freeze drying;
and thirdly, carrying out heat treatment under the protection of inert gas to obtain the magnetic graphene nano wave absorbing material.
Further limiting, in the first step, 10-40% of graphene oxide sponge, 80-20% of acidified carbon nanotube and 10-40% of cobalt nitrate are dissolved in deionized water according to weight percentage.
Further, the preparation method of the graphene oxide sponge in the first step is as follows: flake graphite and concentrated sulfuric acid (98%H2SO4) Sodium nitrate (NaNO)3) Potassium permanganate (KMnO)4) And 30% by mass of hydrogen peroxide (H)2O2) Preparing graphene oxide by a liquid phase stripping method (Hummers) as a raw material, centrifugally washing the graphene oxide until the pH value of the solution is 7 after the reaction is finished, and freeze-drying the graphene oxide at-10 ℃ to obtain the graphene oxide sponge.
Further defining, acidifying the carbon nanotubes in step one: adding 120mL of concentrated sulfuric acid and 40mL of concentrated nitric acid into 1g of carbon nano tube, magnetically stirring, condensing and refluxing for 3h at 55 ℃, washing with deionized water until the pH value is about 7 after the reaction is finished, and freeze-drying to obtain the acidified carbon nano tube.
Further defined, the mechanical stirring rate in the first step is 300rpm to 1000 rpm.
Further limit, the ultrasonic frequency in the first step is 20KHz-40 KHz.
Further, the freeze-drying in the second step is to freeze-dry continuously for 48-100 hours at a vacuum degree of 1Pa-10Pa and a temperature of-10 ℃.
Further limiting, the heat treatment in the third step is carried out in a tubular furnace, the temperature is raised to 400-700 ℃ at the speed of 5-20 ℃/min, the constant temperature treatment is carried out for 1-5 h, and the furnace cooling is carried out.
Further, in the third step, the inert gas is nitrogen.
Compared with the prior art, the invention has the beneficial effects that:
the magnetic nano-particles are coated between layers due to the special nano-roll structure, and the surfaces of the magnetic nano-particles are coated with graphitized carbon, so that the agglomeration of the magnetic nano-particles is effectively inhibited, the effective uniform dispersion of the magnetic particles is realized, the impedance matching degree of the material is improved, the heterogeneous interface is increased, the interface polarization capability of the material is improved, and the synergistic advantages of the magnetic material and the graphene material are exerted.
The composite material has a special one-dimensional structure, so that the composite material has the capability of dissipating electromagnetic waves along the axial direction, and carriers migrate directionally in the one-dimensional structure, so that the electromagnetic wave absorption performance of the composite material is effectively improved.
Drawings
Fig. 1 is a TEM image of the magnetic graphene nanoscropping wave-absorbing material prepared in example 1;
FIG. 2 is a three-dimensional reflection loss plot of the magnetic graphene nanoacoustic materials prepared in example 1 over the frequency range of 2.0GHz-18.0 GHz;
FIG. 3 is a three-dimensional reflection loss plot of the magnetic graphene nanoacoustic materials prepared in example 2 in the frequency range of 2.0GHz-18.0 GHz.
Detailed Description
Example 1, the preparation method of the magnetic graphene nano-roll wave-absorbing material in this example is performed according to the following steps:
step one, dissolving 30g of graphene oxide sponge, 40g of acidified carbon nanotube and 30g of cobalt nitrate in 100mL of deionized water, mechanically stirring at the speed of 300rpm until the mixture is uniform, then performing electrostatic self-assembly reaction at the ultrasonic frequency of 20KHz to form a one-dimensional nano roll, and quickly freezing;
step two, freeze drying: continuously freeze-drying for 48 hours at the vacuum degree of 5Pa and the temperature of-10 ℃;
and step three, taking out the freeze-dried material, placing the material in a tubular furnace, carrying out heat treatment, adopting nitrogen as protective gas, heating to 500 ℃ at the speed of 5 ℃/min, carrying out constant temperature treatment for 1h, and cooling along with the furnace to obtain the magnetic graphene nano wave absorbing material.
Step one, the preparation method of the graphene oxide sponge comprises the following steps: flake graphite and concentrated sulfuric acid (98% H)2SO4) Sodium nitrate (NaNO)3) Potassium permanganate (KMnO)4) And 30% by mass of hydrogen peroxide (H)2O2) Preparing graphene oxide by a liquid phase stripping method (Hummers) as a raw material, centrifugally washing the graphene oxide until the pH value of the solution is 7 after the reaction is finished, and freeze-drying the graphene oxide at-10 ℃ to obtain the graphene oxide sponge.
Acidifying the carbon nanotubes in the first step: adding 120mL of concentrated sulfuric acid and 40mL of concentrated nitric acid into 1g of carbon nano tube, magnetically stirring, condensing and refluxing for 3h at 55 ℃, washing with deionized water until the pH value is about 7 after the reaction is finished, and freeze-drying to obtain the acidified carbon nano tube.
The complex dielectric constant and the complex permeability of the magnetic graphene nano wave absorbing material prepared by the method are tested by a vector network analyzer. The wave-absorbing frequency band studied in the invention is 2.0-18.0 GHz. The mass ratio of the sample to the paraffin is 1:9, the sample is immersed into the melted paraffin, the paraffin is absorbed into the sample by utilizing the capillary action, the sample is lightly pressed by a glass rod to ensure that the sample and the paraffin are uniformly mixed, the condition that local paraffin is excessive or insufficient is avoided, and the sample preparation stability is ensured. The mixed sample was pressed with a mold into a coaxial test ring (inner diameter: 3mm, outer diameter: 7mm) having a thickness of 2mm to conduct an electromagnetic wave absorption test.
A TEM image of the magnetic cobalt-based graphene composite material prepared in this embodiment is shown in fig. 1, and it can be clearly understood from a transmission diagram that a one-dimensional nano-roll composite material is successfully prepared, the magnetic nanoparticles encapsulate the layers of the graphene nano-roll, and the carbon shell encapsulating the magnetic nanoparticles is a lattice stripe of graphitized carbon, so that the problem of easy aggregation of the magnetic particles is effectively solved, and the magnetic nanoparticles are uniformly distributed between the layers of the nano-roll. And calculating the reflection loss of the wave-absorbing material by adopting a transmission line method according to the electromagnetic parameters obtained by testing, wherein the unit is dB. When the reflection loss of the material is less than-10 dB, the wave-absorbing material can absorb more than 90% of electromagnetic waves, and when the RL of the material is less than-20 dB, the wave-absorbing material has the wave-absorbing performance equivalent to that of absorbing more than 99% of electromagnetic waves.
The three-dimensional reflection loss graph of the magnetic graphene nano wave absorbing material prepared by the embodiment in the frequency range of 2.0GHz-18.0GHz is shown in fig. 2, and the highest reflection loss energy reaches-63.16 dB according to the electromagnetic parameter result test, so that the magnetic graphene nano wave absorbing material prepared by the method has strong electromagnetic wave absorption performance.
Example 2 and this example are different from example 1 in that the heat treatment temperature in this example is 600 ℃. The other steps and parameters were the same as in example 1. According to the results of electromagnetic parameters, as shown in fig. 3, fig. 3 shows that the highest reflection loss of the cobalt-based magnetic graphene nano roll composite material reaches-64.49 dB, and the cobalt-based magnetic graphene nano roll composite material also shows strong electromagnetic wave absorption performance, so that the structure designed by the invention effectively inhibits the agglomeration phenomenon of magnetic nano particles, the nano particles are uniformly distributed, and the wave absorption performance is improved. Compared with the common magnetic graphene-based wave-absorbing material, the novel one-dimensional magnetic graphene-based composite material has excellent complementarity between dielectric loss and magnetic loss, so that the influence of the wave-absorbing performance of the novel one-dimensional magnetic graphene-based composite material along with the pyrolysis temperature is small. Within a certain temperature range, the electromagnetic wave absorption performance of the composite material can be kept stable, carriers can migrate in a one-dimensional structure along the axial direction, electromagnetic waves are dissipated, magnetic metal agglomeration is effectively inhibited between the graphitized carbon and the nano roll layer, the structure also provides rich heterogeneous interfaces, the interface polarization effect is favorably enhanced, the dielectric loss capacity of the material is improved, and the improvement of the electromagnetic wave absorption performance of the material is greatly promoted.

Claims (10)

1. A preparation method of a magnetic graphene nano wave absorbing material is characterized by comprising the following steps:
dissolving graphene oxide sponge, an acidified carbon nanotube and cobalt nitrate in deionized water, mechanically stirring until the mixture is uniform, performing electrostatic self-assembly reaction under ultrasound to form a one-dimensional nano coil, and quickly freezing;
step two, freeze drying;
and thirdly, carrying out heat treatment under the protection of inert gas to obtain the magnetic graphene nano wave absorbing material.
2. The method according to claim 1, wherein in the first step, 10-40% of graphene oxide sponge, 80-20% of acidified carbon nanotube and 10-40% of cobalt nitrate are dissolved in deionized water by weight percentage.
3. The method according to claim 1, wherein the graphene oxide sponge is prepared as follows: preparing graphene oxide by using crystalline flake graphite, concentrated sulfuric acid, sodium nitrate, potassium permanganate and 30% (mass) hydrogen peroxide as raw materials through a liquid phase stripping method, centrifugally washing until the pH value of the solution is 7 after the reaction is finished, and freeze-drying at-10 ℃ to obtain the graphene oxide sponge.
4. The method of claim 1, wherein the step one of acidifying the carbon nanotubes: adding 120mL of concentrated sulfuric acid and 40mL of concentrated nitric acid into 1g of carbon nano tube, magnetically stirring, condensing and refluxing for 3h at 55 ℃, washing with deionized water until the pH value is about 7 after the reaction is finished, and freeze-drying to obtain the acidified carbon nano tube.
5. The method according to claim 1, wherein the mechanical stirring rate in the first step is 100rpm to 1000 rpm.
6. The method according to claim 1, wherein the ultrasonic frequency in the first step is 10KHz to 40 KHz.
7. The method according to claim 1, wherein the freeze-drying in the second step is carried out under a vacuum of 1Pa to 10Pa at a temperature of-10 ℃ for a period of 48 hours to 100 hours.
8. The preparation method according to claim 1, wherein the heat treatment in step three is carried out in a tube furnace, the temperature is raised to 400-700 ℃ at a rate of 5-20 ℃/min, the temperature is kept constant for 1-5 h, and the furnace cooling is carried out.
9. The method according to claim 1, wherein the heat treatment temperature in the third step is 500 ℃ to 600 ℃.
10. The method according to claim 1, wherein the inert gas in step three is nitrogen.
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