CN113993364A - Preparation method and application of nickel hydroxide modified graphene composite broadband wave-absorbing material - Google Patents
Preparation method and application of nickel hydroxide modified graphene composite broadband wave-absorbing material Download PDFInfo
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- 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
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- 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
- H01Q17/007—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems with means for controlling the absorption
Abstract
The invention relates to a nickel hydroxide modified graphene composite broadband wave-absorbing material, a preparation method and application thereof, belonging to the technical field of electromagnetic wave-absorbing materials, wherein the specific synthesis method comprises the following steps: the hydrogen peroxide is utilized to carry out pre-oxidation treatment on the graphene raw material, so that a large number of defects are produced on the surface of the graphene in the step, and conditions are created for loading the nano particles. And then loading nickel hydroxide on the surface of the pretreated graphene under the condition of different addition amounts of alkaline solutions, wherein nickel hydroxide particles under different synthesis conditions have different sizes, and the modification effect of the nickel hydroxide on the graphene can be optimized by regulating and controlling the loading condition, so that the whole absorption capacity of the graphene on electromagnetic waves is enhanced, and the broadband electromagnetic absorption material is obtained.
Description
Technical Field
The invention particularly relates to a preparation method and application of a nickel hydroxide modified graphene composite broadband wave-absorbing material, and belongs to the technical field of electromagnetic wave-absorbing materials.
Background
Graphene is a two-dimensional carbon-based material which is researched vigorously at home and abroad in recent years, and has a very large specific surface area, excellent chemical stability and good conductivity. When the graphene-based wave-absorbing material is applied to an electromagnetic wave-absorbing material, the graphene-based wave-absorbing material has certain electromagnetic absorption performance due to the dielectric loss capacity of graphene. The graphene-based electromagnetic absorption material disclosed in patent CN112165849A of southern opening university in 2020 not only has a wider absorption band, but also can realize the regulation and control of electromagnetic absorption performance by changing the response intensity change of the voltage regulation and control material to electromagnetic signals.
However, when the conductive network structure on the surface of the graphene is applied to the field of wave absorption, the impedance matching capability of the material is seriously influenced, when electromagnetic waves are incident on the surface of the material, the induced electromagnetic field can generate serious bending current on the surface of the graphene, and further incidence of the electromagnetic waves is influenced, so researchers regulate and control the impedance matching characteristic of the graphene by designing a composite material, and further optimize the wave absorption performance of the graphene. In 2021, the chemical research institute of the academy of sciences in Guangdong province discloses a patent CN112788935A, and the electromagnetic parameters of the reduced graphene oxide are regulated and controlled by nano inorganic oxides and nano metals, so that the prepared composite material has excellent electromagnetic absorption performance at high frequency. In 2019, a patent CN109107528A disclosed by the seventh two five research institutes of the china ship re-engineering group company proposes a function of regulating and controlling the performance of graphene by using magnetic nickel metal synthesized by nickel acetate as a nickel source, and through composite component design, the prepared graphene composite material can have the characteristics of small density, large coercive force, high saturation magnetization and large magnetic area.
Disclosure of Invention
Aiming at the problems, the invention utilizes the dielectric property difference between nickel hydroxide and graphene, compounds the two materials by a chemical means, regulates and controls the electromagnetic parameters of the composite material by the modification effect of nickel hydroxide nano particles on the graphene, so that the impedance matching and attenuation capability of the material are balanced, and designs the graphene-based composite material. The material effectively widens the electromagnetic absorption frequency band of graphene by integrating various loss mechanisms, does not adopt toxic organic solvent in the experimental process, can be used as functional stealth coating filler to be coated on the surface of weaponry or electromagnetic protection equipment, reduces the influence of external electromagnetic waves on the equipment body, and has wide application market and wide economic prospect.
The invention aims to provide a preparation method of a nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material; the second purpose is to provide a method for regulating and controlling the electromagnetic parameters of the graphene composite broadband electromagnetic wave absorbing material by controlling the addition amount of the alkaline ammonia water in the reaction; the third purpose is to provide the application of the graphene composite broadband electromagnetic wave absorption material in widening the electromagnetic absorption band of graphene and improving the electromagnetic absorption performance.
In order to achieve the purpose, the invention adopts the following specific scheme:
the preparation method of the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material comprises the steps of taking graphene as a raw material, firstly carrying out oxidation etching on the graphene, manufacturing defects on the surface of the graphene to generate nickel hydroxide load sites, and then compounding nickel hydroxide and the graphene subjected to oxidation etching to uniformly distribute nickel hydroxide nanoparticles on the surface of the graphene to form the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material. The preparation method specifically comprises the following steps:
step one, graphene pretreatment: taking a hydrogen peroxide solution with the mass fraction of 30% as an etching agent, adding 200-300ml of hydrogen peroxide solution into each gram of graphene raw material, preparing 500ml of mixed solution by using distilled water, fully and uniformly dispersing, heating to 60-90 ℃, keeping the temperature for 1-2 hours, separating graphene and the solution, fully cleaning and drying to obtain a graphene precursor;
step two, adding nickel nitrate hexahydrate into the graphene precursor obtained in the step one, maintaining the mass ratio of the nickel nitrate hexahydrate to the graphene precursor at 8-13: 1, and adding distilled water to disperse uniformly to obtain dispersion liquid;
step three, taking ammonia water and distilled water, uniformly mixing, then adding the ammonia water and the distilled water into the dispersion liquid obtained in the step two, and uniformly mixing to obtain a reaction liquid, wherein the amount of the ammonia water is maintained to be 4% -20% of the total volume of the reaction liquid; and heating the reaction solution to 90-120 ℃, maintaining for 4 hours for heat preservation and stirring, and separating and washing a solid-phase product after the reaction is finished to obtain the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material.
And step two, adding distilled water to disperse uniformly, wherein the adding amount of the distilled water is adjusted according to the amount of the material to be dispersed, and the standard is that all reactants can be dispersed in the solvent.
The invention also provides a method for regulating and controlling the electromagnetic parameters of the graphene composite broadband electromagnetic wave absorbing material, wherein the graphene composite broadband electromagnetic wave absorbing material is obtained by loading nickel hydroxide on the surface of graphene pretreated by hydrogen peroxide, and the synthesis method comprises the following steps:
step one, graphene pretreatment: taking a hydrogen peroxide solution with the mass fraction of 30% as an etching agent, adding 200-300ml of hydrogen peroxide solution into each gram of graphene raw material, preparing 500ml of mixed solution by using distilled water, fully and uniformly dispersing, heating to 60-90 ℃, keeping the temperature for 1-2 hours, separating graphene and the solution, fully cleaning and drying to obtain a graphene precursor;
step two, adding nickel nitrate hexahydrate into the graphene precursor obtained in the step one, maintaining the mass ratio of the nickel nitrate hexahydrate to the graphene precursor at 8-13: 1, and adding distilled water to disperse uniformly to obtain dispersion liquid;
step three, taking ammonia water and distilled water, uniformly mixing, then adding the ammonia water and the distilled water into the dispersion liquid obtained in the step two, and uniformly mixing to obtain a reaction liquid, wherein the amount of the ammonia water is maintained to be 4% -20% of the total volume of the reaction liquid; heating the reaction solution to 90-120 ℃, maintaining for 4 hours for heat preservation and stirring, separating and washing a solid-phase product after the reaction is finished, and obtaining the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material;
and the regulation and control means that in the third step, the particle size of the nickel hydroxide particles loaded on the surface of the graphene is realized by adjusting the amount of ammonia water in the reaction liquid.
The invention further provides the preparation method and application of the graphene composite broadband wave-absorbing material prepared by the preparation method in widening the electromagnetic absorption band of graphene and improving the electromagnetic absorption performance.
According to the invention, the nickel hydroxide with the nano-scale is selected as the modified particles, the uniformity of the distribution of the nano-particles on the surface of the graphene is improved through the pre-oxidation etching treatment of the graphene, the growth condition of the nickel hydroxide on the surface of the graphene is controlled through the design of the reaction environment of the nickel hydroxide, the regulation and control effect of the nickel hydroxide on the graphene is optimized to the maximum extent, the effective absorption bandwidth of the graphene-based composite material is increased, and the application potential of the graphene material is widened. Therefore, the composite material designed by modifying the graphene with the nickel hydroxide is a wave-absorbing material with simple process and excellent electromagnetic wave absorption performance, and has great research value and application market.
Has the advantages that:
according to the nickel hydroxide modified graphene composite broadband wave-absorbing material, the graphene raw material is subjected to oxidation pretreatment and nickel hydroxide modification with different particle shapes, when the corresponding matching thickness is less than 2mm, the effective absorption bandwidth can reach 6.0GHz, the material has a wide effective absorption bandwidth and a thin filling thickness, the requirements of the electromagnetic wave-absorbing material on the bandwidth and the thickness can be met, the graphene performance is regulated and controlled by the nickel hydroxide in a polarization enhancing and matching optimizing manner, and the finally synthesized composite material has excellent electromagnetic absorption performance. Meanwhile, the invention does not need to use highly toxic organic solvent, the synthesis temperature can be controlled in a lower temperature range (below 150 ℃), the preparation process is simple, the large-scale production can be realized, and the invention can be used as the functional filler of the electromagnetic absorption coating to realize the application.
In the nickel hydroxide/graphene composite material obtained by the method, nickel hydroxide nanoparticles are uniformly distributed on the surface of graphene, the particle size of nickel hydroxide particles loaded on the surface of the graphene can be controlled by controlling the addition amount of alkaline ammonia water in the reaction, so that the electromagnetic parameters of the graphene composite material are regulated, the matching and loss characteristics are optimized, and the effective absorption bandwidth of the composite material is widened. Through the regulation and control of the ammonia water concentration embodiment, the effective absorption bandwidth of the synthesized nickel hydroxide/graphene composite material can cover 12-18GHz under the condition of low filling ratio of 10wt%, and meanwhile, the matching thickness can be reduced to be less than 2mm, so that excellent electromagnetic wave absorption capacity is shown. According to the invention, hydrogen peroxide is used for carrying out pre-oxidation treatment on the graphene raw material, so that a large number of defects are produced on the surface of the graphene in one step, and conditions are created for loading nanoparticles. And then loading nickel hydroxide on the surface of the pretreated graphene under the condition of different addition amounts of alkaline solutions, wherein nickel hydroxide particles under different synthesis conditions have different sizes, and the modification effect of the nickel hydroxide on the graphene can be optimized by regulating and controlling the loading condition, so that the whole absorption capacity of the graphene on electromagnetic waves is enhanced, and the broadband electromagnetic absorption material is obtained.
Drawings
FIG. 1 is a topographical view of nickel hydroxide/graphene-1;
FIG. 2 is a topographical view of nickel hydroxide/graphene-2;
FIG. 3 is an XRD spectrum of graphene and nickel hydroxide modified graphene samples;
FIG. 4 is a graph of real dielectric part of graphene and nickel hydroxide modified graphene samples;
FIG. 5 is a graph of the imaginary dielectric part of graphene and nickel hydroxide modified graphene samples;
FIG. 6 is a Coler curve map of a nickel hydroxide modified graphene sample;
FIG. 7 is a graphene feedstock performance map;
FIG. 8 is a hydrogen peroxide treated graphene performance map;
FIG. 9 is a nickel hydroxide/graphene-1 performance map;
figure 10 is a nickel hydroxide/graphene-2 performance map.
Detailed Description
The invention is realized by the following technical scheme:
(1) specifically, the invention relates to a nickel hydroxide modified graphene composite broadband wave-absorbing material and a preparation method thereof. Before the graphene and the nickel hydroxide are compounded, a step of hydrogen peroxide oxidation etching treatment is added, under the action of hydrogen peroxide, the original conductive network structure of the graphene can be damaged to a certain degree, but cannot be damaged to the degree of complete breakage, and in the step, an oxidation group can be accessed to the surface of the graphene on the basis of basically maintaining the original structure of the graphene, so that a defect is produced to generate a nickel hydroxide load site, the growth of the nickel hydroxide is more uniform, and the modification effect of the nickel hydroxide on the graphene is exerted to the greatest extent.
(2) The nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material can grow to different shapes under different alkaline conditions, and by taking the concentration of low ammonia water and the concentration of high ammonia water as examples, as shown in fig. 1 and 2, nickel hydroxide can grow to small particles close to a hexagon and be uniformly loaded on the surface of graphene under the condition of low ammonia water addition, and under the condition of high ammonia water addition, the particles of nickel hydroxide become smaller than the particles of the nickel hydroxide in the prior art due to the difference of reaction conditions, and a layer of nickel hydroxide nano particles can be uniformly distributed on the surface of graphene.
(3) According to the nickel hydroxide modified graphene composite broadband electromagnetic wave absorption material, by combining with the analysis of a figure 3-XRD (X-ray diffraction) spectrum, only the graphene subjected to oxidation treatment has a carbon (002) characteristic peak at about 20 degrees, and the nickel hydroxide modified graphene composite material has three corresponding nickel hydroxide characteristic peaks (111), (200) and (220).
(4) The electromagnetic parameters of the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material are greatly changed after being modified by nickel hydroxide, as shown in fig. 4 and 5, the dielectric real part of graphene is reduced after being oxidized by hydrogen peroxide, and the impedance matching of the graphene composite broadband electromagnetic wave absorbing material is proved to be optimized to a certain degree. After nickel hydroxide modification, the electromagnetic parameters of the nickel hydroxide/graphene composite material synthesized according to different alkaline conditions have larger difference, and by combining with the analysis of the micro-morphology of the nickel hydroxide, when the nickel hydroxide particles are larger, the dielectric real part and the dielectric imaginary part of the nickel hydroxide particles are both greatly reduced compared with unmodified graphene samples, and when the nickel hydroxide particles are smaller, the dielectric real part of the nickel hydroxide particles is not greatly changed compared with large particles, but the dielectric imaginary part of the nickel hydroxide particles is greatly improved, so that the loss capacity of the nickel hydroxide/graphene composite material is improved while the excellent impedance matching performance is maintained, and the modification effect of the nickel hydroxide on the graphene can be furthest exerted due to the fact that small particles are distributed on the surface of the graphene more uniformly.
(5) The electromagnetic absorption mechanism of the nickel hydroxide modified graphene composite broadband electromagnetic wave absorption material mainly comes from the interface polarization between graphene and nickel hydroxide, the dipole polarization of nickel hydroxide and the dipole polarization of the surface defects of oxidized graphene, and by combining with the Kerr curve analysis of the material shown in figure 6, a plurality of circular arcs shown in the figure prove the existence of multiple polarization effects in the material, and the effects not only optimize the impedance matching of graphene, but also enhance the loss capacity of the material.
(6) The nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material is improved to a certain extent after graphene is subjected to oxidation pretreatment and then modified by nickel hydroxide. As shown in fig. 6-10, under the condition that the sample filling ratio is 10wt% (the mass ratio of the graphene composite material to the paraffin is 10 to 90, which is the test requirement), the pure graphene sample has poor electromagnetic loss performance through calculation, and the whole sample has no region with the reflection loss value smaller than-10 dB. After the hydrogen peroxide oxidation treatment, a region with a loss value smaller than-10 dB begins to appear in the frequency range of 8-12GHz, which proves that the sample in the frequency range has good electromagnetic absorption capacity, the effective electromagnetic absorption region is further expanded after the nickel hydroxide modification, and for the graphene modified by the large-particle nickel hydroxide, the effective absorption region can cover 14-18GHz under the condition that the thickness of the sample is less than 2mm, and the effective absorption bandwidth reaches 4.0 GHz. And for the graphene modified by the small-particle nickel hydroxide, under the condition that the thickness of a sample is less than 2mm, the effective absorption area can be widened to 12-18GHz, the effective absorption bandwidth reaches 6.0GHz, and the effective absorption performance of broadband is realized.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
The nickel hydroxide modified graphene composite broadband wave-absorbing material and the preparation method thereof comprise the following steps:
And 2, taking 100mg of graphene precursor, respectively adding 1.12g of nickel nitrate hexahydrate and 200ml of distilled water, fully stirring and carrying out ultrasonic separation for 1-2 hours to obtain a precursor mixed solution.
And 3, taking 10ml of ammonia water and 40ml of distilled water, fully and uniformly mixing, slowly pouring the ammonia water and the distilled water into the precursor mixed solution obtained in the step 2, uniformly mixing, maintaining and stirring for 4 hours under the oil bath heating condition at 100 ℃, separating a solid phase and a liquid phase in the solution, fully cleaning and drying to obtain a nickel hydroxide/graphene-1 composite material sample.
Example 2
And 3, taking 20ml of ammonia water and 30ml of distilled water, fully and uniformly mixing, slowly pouring the ammonia water and the distilled water into the precursor mixed solution obtained in the step 2, uniformly mixing, maintaining and stirring for 4 hours under the oil bath heating condition at 100 ℃, separating a solid phase and a liquid phase in the solution, fully cleaning and drying to obtain a nickel hydroxide/graphene-2 composite material sample.
Example 3
And 3, taking 30ml of ammonia water and 20ml of distilled water, fully and uniformly mixing, slowly pouring the ammonia water and the distilled water into the precursor mixed solution obtained in the step 2, uniformly mixing, maintaining and stirring for 4 hours under the oil bath heating condition at 100 ℃, separating a solid phase and a liquid phase in the solution, fully cleaning and drying to obtain a nickel hydroxide/graphene-3 composite material sample.
Example 4
And 3, taking 40ml of ammonia water and 10ml of distilled water, fully and uniformly mixing, slowly pouring the ammonia water and the distilled water into the precursor mixed solution obtained in the step 2, uniformly mixing, maintaining and stirring for 4 hours under the oil bath heating condition at 100 ℃, separating a solid phase and a liquid phase in the solution, fully cleaning and drying to obtain a nickel hydroxide/graphene-4 composite material sample.
Example 5
And 3, slowly pouring 50ml of ammonia water into the precursor mixed solution obtained in the step 2, uniformly mixing, keeping stirring for 4 hours under the oil bath heating condition at 100 ℃, separating a solid phase and a liquid phase in the solution, fully cleaning and drying to obtain a nickel hydroxide/graphene-5 composite material sample.
Test mode and sample performance analysis: the synthesized powder sample was mixed with paraffin wax at a ratio of 10: 90 and pressed into a ring with an inner diameter of 3.04mm and an outer diameter of 7.00mm, an electromagnetic parameter test was performed using a vector network analyzer, and reflection loss performance parameters were obtained by calculation, with the results shown in fig. 7, 8, 9, and 10. The graphene raw material has poor performance under the filling ratio condition, the graphene subjected to hydrogen peroxide etching has effective electromagnetic wave absorption capacity under the condition of 8-12GHz, the effective absorption bandwidth of a sample modified by nickel hydroxide is widened to 6.0GHz, the matching thickness of the sample is reduced to be lower than 2.0mm, and the graphene has excellent electromagnetic absorption performance.
It should be noted that the above-mentioned embodiments illustrate rather than limit the scope of the invention, which is defined by the appended claims. It will be apparent to those skilled in the art that certain insubstantial modifications and adaptations of the present invention can be made without departing from the spirit and scope of the invention.
Claims (5)
1. The preparation method of the nickel hydroxide modified graphene composite broadband electromagnetic wave absorption material is characterized by comprising the following steps of: the graphene composite broadband electromagnetic wave absorbing material is prepared by taking graphene as a raw material, firstly carrying out oxidation etching on the graphene, manufacturing defects on the surface of the graphene to generate nickel hydroxide loading sites, and then compounding nickel hydroxide and the graphene subjected to oxidation etching to uniformly distribute nickel hydroxide nanoparticles on the surface of the graphene to form the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material.
2. The method of claim 1, wherein: the method comprises the following steps:
step one, graphene pretreatment: taking a hydrogen peroxide solution with the mass fraction of 30% as an etching agent, adding 200-300ml of hydrogen peroxide solution into each gram of graphene raw material, preparing 500ml of mixed solution by using distilled water, fully and uniformly dispersing, heating to 60-90 ℃, keeping the temperature for 1-2 hours, separating graphene and the solution, fully cleaning and drying to obtain a graphene precursor;
step two, adding nickel nitrate hexahydrate into the graphene precursor obtained in the step one, maintaining the mass ratio of the nickel nitrate hexahydrate to the graphene precursor at 8-13: 1, and adding distilled water to disperse uniformly to obtain dispersion liquid;
step three, taking ammonia water and distilled water, uniformly mixing, then adding the ammonia water and the distilled water into the dispersion liquid obtained in the step two, and uniformly mixing to obtain a reaction liquid, wherein the amount of the ammonia water is maintained to be 4% -20% of the total volume of the reaction liquid; and heating the reaction solution to 90-120 ℃, maintaining for 4 hours for heat preservation and stirring, and separating and washing a solid-phase product after the reaction is finished to obtain the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material.
3. The method of claim 1, wherein: and step two, adding distilled water to disperse uniformly, wherein the adding amount of the distilled water is adjusted according to the amount of the material to be dispersed, and the standard is that all reactants can be dispersed in the solvent.
4. A method for regulating and controlling electromagnetic parameters of a graphene composite broadband electromagnetic wave absorbing material is characterized by comprising the following steps: the graphene composite broadband electromagnetic wave absorbing material is obtained by loading nickel hydroxide on the surface of graphene pretreated by hydrogen peroxide, and the synthesis method comprises the following steps:
step one, graphene pretreatment: taking a hydrogen peroxide solution with the mass fraction of 30% as an etching agent, adding 200-300ml of hydrogen peroxide solution into each gram of graphene raw material, preparing 500ml of mixed solution by using distilled water, fully and uniformly dispersing, heating to 60-90 ℃, keeping the temperature for 1-2 hours, separating graphene and the solution, fully cleaning and drying to obtain a graphene precursor;
step two, adding nickel nitrate hexahydrate into the graphene precursor obtained in the step one, maintaining the mass ratio of the nickel nitrate hexahydrate to the graphene precursor at 8-13: 1, and adding distilled water to disperse uniformly to obtain dispersion liquid;
step three, taking ammonia water and distilled water, uniformly mixing, then adding the ammonia water and the distilled water into the dispersion liquid obtained in the step two, and uniformly mixing to obtain a reaction liquid, wherein the amount of the ammonia water is maintained to be 4% -20% of the total volume of the reaction liquid; heating the reaction solution to 90-120 ℃, maintaining for 4 hours for heat preservation and stirring, separating and washing a solid-phase product after the reaction is finished, and obtaining the nickel hydroxide modified graphene composite broadband electromagnetic wave absorbing material;
and the regulation and control means that in the third step, the particle size of the nickel hydroxide particles loaded on the surface of the graphene is realized by adjusting the amount of ammonia water in the reaction liquid.
5. The preparation method of claim 1 and the application of the graphene composite broadband wave-absorbing material prepared by the preparation method of claim 1 in widening the electromagnetic absorption band of graphene and improving the electromagnetic absorption performance.
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| CN115161531A (en) * | 2022-07-08 | 2022-10-11 | 西安稀有金属材料研究院有限公司 | High-entropy alloy/graphene composite material with wave absorption performance and preparation method thereof |
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| CN115161531A (en) * | 2022-07-08 | 2022-10-11 | 西安稀有金属材料研究院有限公司 | High-entropy alloy/graphene composite material with wave absorption performance and preparation method thereof |
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