CN108034408B - Preparation method of graphene-based composite wave-absorbing material - Google Patents
Preparation method of graphene-based composite wave-absorbing material Download PDFInfo
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- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 8
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- 238000000034 method Methods 0.000 claims abstract description 8
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 6
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- 239000000178 monomer Substances 0.000 claims abstract description 4
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 239000012153 distilled water Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 14
- FWQOXFQRLISKCM-UHFFFAOYSA-N [Co].[Nd] Chemical compound [Co].[Nd] FWQOXFQRLISKCM-UHFFFAOYSA-N 0.000 claims description 11
- 239000006185 dispersion Substances 0.000 claims description 9
- 239000011240 wet gel Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
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- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 4
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 3
- 229910003205 Nd(NO3)3·6H2O Inorganic materials 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
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- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
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- 238000001338 self-assembly Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
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- 238000011065 in-situ storage Methods 0.000 abstract 1
- 239000003999 initiator Substances 0.000 abstract 1
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- 238000006116 polymerization reaction Methods 0.000 abstract 1
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- 239000004094 surface-active agent Substances 0.000 abstract 1
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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Abstract
The invention relates to a preparation method of a graphene-based composite wave-absorbing material, which comprises the steps of firstly, preparing graphene oxide by using a modified Hummers method with natural graphite powder as a raw material and concentrated sulfuric acid and permanganate as oxidants, then selecting nitrates of strontium, neodymium, cobalt and iron as raw materials and citric acid as a complexing agent, preparing neodymium-cobalt-doped strontium ferrite by using a sol-gel-self-propagating method, then preparing a graphene/neodymium-cobalt-doped strontium ferrite composite material by using dimethylformamide as a solvent, cetyl trimethyl ammonium bromide as a surfactant and hydrazine hydrate as a reducing agent and adopting a self-assembly method; and finally, uniformly mixing the graphene-neodymium cobalt doped strontium ferrite composite material and an aniline monomer, and obtaining the ternary nano composite material by using ammonium persulfate as an initiator through an in-situ polymerization method. The material has the advantages of low preparation cost, simple process, low density, strong wave-absorbing capability and wide frequency band, and has important application value in the aspects of microwave absorption and electromagnetic wave shielding.
Description
Technical Field
The invention relates to a preparation method of a wave-absorbing material, in particular to a preparation method of a graphene-based composite wave-absorbing material, and belongs to the technical field of wave-absorbing materials.
Background
In the 21 st century of rapid development of science and technology, various electronic products come out one after another and rapidly enter the families of ordinary people, which brings great convenience to life, but worry about that people also suffer from various degrees of damage from electromagnetic waves while enjoying the benefits. The electromagnetic wave is easy to cause pathological changes of human bodies when being in an electromagnetic wave environment for a long time, and meanwhile, the electromagnetic wave can interfere the normal work of various electronic equipment and communication instruments and even cause the electronic equipment and the communication instruments to break down. Electromagnetic interference is the fourth environmental pollution source following the industrial three wastes, so how to effectively prevent and eliminate electromagnetic interference has become the focus of the scientific and technological community.
Graphene, a cellular two-dimensional material, has been successfully ascending in the front of the leaderboard of common wave-absorbing materials by virtue of its characteristics of light weight, large specific surface area, good flexibility, good conductivity, large dielectric loss, and the like. Meanwhile, a large number of chemical bonds can be exposed on the surface of the oxidized graphene, and polarization relaxation can be generated easily under the action of an electromagnetic field, so that the purpose of attenuating electromagnetic waves is achieved, and the application of the graphene in the field of wave absorption is wider. However, the new wave-absorbing materials need to meet the requirements of "thin, light, wide, and strong". Electrical losses arise mainly from electron polarization, atomic polarization, intrinsic electric dipole orientation polarization, and interfacial polarization. The magnetic loss mainly includes eddy current loss, hysteresis loss and residual loss. Graphene has large dielectric loss and a small amount of magnetic loss, single graphene interface impedance matching is poor, in addition, the loss mechanism is less, and the wave absorbing effect is not strong. However, since graphene has a large specific surface area, graphene can be compounded with a magnetic loss type wave-absorbing material to form complementary advantages, and on one hand, the compounding of the electric loss wave-absorbing material and the magnetic loss wave-absorbing material can exert electromagnetic losses in two forms to obtain better electromagnetic wave absorption performance; on the other hand, the composite material with the light graphene material is also beneficial to reducing the weight of the wave-absorbing material.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a graphene-based composite wave-absorbing material, which is simple, easy to operate and low in cost, and the prepared wave-absorbing material is high in dielectric loss and magnetic loss, stable in electromagnetic property, wide in wave-absorbing frequency band and good in wave-absorbing property.
In order to achieve the purpose, the graphene and the neodymium-cobalt-doped strontium ferrite are compounded to improve the impedance matching, in addition, a conductive polymer is added into a compound system to serve as a coating layer, the interface combination of magnetic particles and the graphene is enhanced, meanwhile, the conductive polymer has high dielectric loss, and the wave-absorbing performance of the material in a high-frequency band can be enhanced after ternary compounding.
The specific scheme is as follows:
a graphene-based composite wave-absorbing material is of a sandwich structure, a middle layer is graphene/neodymium-cobalt doped strontium ferrite, and the outermost layer is polyaniline.
The preparation method of the graphene-based composite wave-absorbing material comprises the following steps:
(1) preparing graphene oxide: weighing 3-4 g of graphite powder, 2.5-3.5 g of persulfate and 2-4 g P2O5Sequentially adding the mixture into 15-18 ml of concentrated sulfuric acid, stirring for 6-8 hours at 80-85 ℃, adding distilled water to dilute the reaction system to a pH value of 4-5 after the reaction system is cooled to room temperature, standing for 20-24 hours, filtering, washing with water until the filtrate is neutral, and drying the obtained product to a constant weight at room temperature to obtain pre-oxidized graphite; adding pre-oxidized graphite into 120-150 mL of concentrated sulfuric acid, uniformly stirring, slowly adding 15-18 g of strong oxidant in an ice water bath, uniformly stirring, slowly heating to 35-40 ℃, continuously reacting for 2-4h, slowly adding 250-300 mL of distilled water into a system, then reacting for 2-3 h, controlling the temperature of the system to be not more than 50 ℃, adding 300-350 mL of distilled water again, stirring until the system is uniform, then dropwise adding 10-40 mL of hydrogen peroxide with the concentration of 30%, converting the solution into bright brown, washing with a hydrochloric acid solution after centrifugal separation, finally dialyzing for 7-8 d with distilled water, and freeze-drying the obtained upper-layer dispersion to obtain graphene oxide;
(2) preparation of SNCF (neodymium cobalt doped strontium ferrite): according to the chemical formula Sr of neodymium cobalt doped strontium ferrite0.85Nd0.15Co0.15Fe11.85O19Weighing Sr (NO) according to the stoichiometric ratio in3)2，Fe(NO3)3·9H2O，Nd(NO3)3·6H2O，Co(NO3)2·4H2Dissolving O in distilled water, stirring uniformly to obtain a clear solution, slowly dropwise adding a citric acid solution, stirring uniformly, adjusting the pH value to 7 to obtain a sol, evaporating the sol in a 75-85 ℃ water bath, stirring to obtain a wet gel, drying the wet gel, igniting the wet gel in air to obtain a fluffy precursor, grinding and calcining to obtain SNCF;
(3) preparing a graphene/neodymium cobalt doped strontium ferrite composite material: respectively dissolving graphene oxide and neodymium-cobalt-doped strontium ferrite in DMF (dimethyl formamide) to obtain a graphene oxide solution and a neodymium-cobalt-doped strontium ferrite suspension, adding Cetyl Trimethyl Ammonium Bromide (CTAB) into the graphene oxide solution, dispersing uniformly, slowly dripping the mixture into the neodymium-cobalt-doped strontium ferrite suspension, mixing uniformly, adding hydrazine hydrate into a reaction system, stirring in a water bath at 95 ℃ for 12-14 h, carrying out suction filtration, washing with water and alcohol until the filtrate is neutral, and finally carrying out vacuum drying to obtain a graphene/neodymium-cobalt-doped strontium ferrite composite material;
(4) preparing the graphene-based composite wave-absorbing material: dissolving a graphene/neodymium-cobalt doped strontium ferrite composite material and 1-2 ml of aniline monomer in 30-50 ml of hydrochloric acid solution, wherein the molar ratio of the graphene/neodymium-cobalt doped strontium ferrite composite material to aniline is 1:2.5, and uniformly dispersing to obtain a dispersion liquid; dissolving 2.5-3.5 g of ammonium persulfate in 20-30 ml of hydrochloric acid solution to obtain a transparent solution, slowly dripping the transparent solution into the dispersion, stirring in an ice water bath for 12-15 hours, and sequentially carrying out suction filtration, water washing, alcohol washing and vacuum drying to obtain the graphene-based composite wave-absorbing material.
Further, in the step (1), the persulfate is potassium persulfate or sodium persulfate.
Further, in the step (1), the strong oxidant is potassium permanganate or potassium dichromate.
Further, in the step (1), the volume concentration of the hydrochloric acid solution is 10%.
Further, in the step (2), citric acid is added according to the molar ratio of the citric acid to the metal ions being 1: 1.
Further, in the step (2), the drying temperature is 120 ℃, and the time is 10-12 hours.
Further, in the step (2), the calcining temperature is 900 ℃ and the time is 2-4 h.
Further, in the step (3), the molar ratio of graphene oxide to neodymium-cobalt-doped strontium ferrite is 6:100, the molar ratio of hexadecyl trimethyl ammonium bromide to graphene oxide is 0.8:100, and the molar ratio of hydrazine hydrate to graphene oxide is 0.7: 1.
Further, in the step (3), the temperature of vacuum drying is 60 ℃, and the time is 10-12 h.
Further, in the step (4), the concentration of the hydrochloric acid solution is 1.0 mol/L.
Has the advantages that: the method is simple, easy to operate and low in cost, and the prepared wave-absorbing material is high in dielectric loss and magnetic loss, stable in electromagnetic property, wide in wave-absorbing frequency band and good in wave-absorbing property, and has a good application prospect in the field of electromagnetic wave shielding and electromagnetic wave absorption.
Drawings
Fig. 1 is an XRD pattern of the graphene-based composite wave-absorbing material prepared in example 1;
fig. 2 is a wave-absorbing performance diagram of the graphene-based composite wave-absorbing material prepared in example 1.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments.
Example 1
(1) Preparing graphene oxide: 3g of graphite powder, 2.5g of sodium persulfate and 2.5g of 2.5g P were weighed out2O5Sequentially adding the mixture into 15ml of concentrated sulfuric acid, stirring for 6 hours at 80 ℃, adding distilled water to dilute the mixture until the pH value is 4 after a reaction system is cooled to room temperature, standing for 20 hours, filtering, washing with water until the filtrate is neutral, and drying the obtained product to constant weight at room temperature to obtain pre-oxidized graphite; adding pre-oxidized graphite into 120mL of concentrated sulfuric acid, uniformly stirring, slowly adding 15g of strong oxidant potassium permanganate in an ice water bath, uniformly stirring, slowly heating to 35 ℃, continuing to react for 2h, slowly adding 250mL of distilled water into the system, reacting for 2h, controlling the temperature of the system to be not more than 50 ℃, adding 350mL of distilled water again, stirring until the system is uniform, dropwise adding 10mL of hydrogen peroxide with the concentration of 30%,the solution is changed into bright brown, after centrifugal separation, the solution is washed by 1L of hydrochloric acid solution with the volume concentration of 10%, finally, the solution is dialyzed for 7d by distilled water to remove residual metal ions and acid, and the obtained upper-layer dispersion liquid is frozen and dried to obtain graphene oxide GO;
(2) preparation of SNCF (neodymium cobalt doped strontium ferrite): weighing Sr (NO) according to the stoichiometric ratio of neodymium cobalt doped strontium ferrite3)2，Fe(NO3)3·9H2O，Nd(NO3)3·6H2O，Co(NO3)2·4H2Dissolving O in distilled water, uniformly stirring to obtain a clear solution, weighing citric acid as a complexing agent according to the molar ratio of metal ions to citric acid of 1:1, dissolving the citric acid in the distilled water to obtain a citric acid solution, slowly dripping the citric acid solution into the clear solution, uniformly stirring, adjusting the pH value of 7 to obtain a sol, evaporating the sol in a water bath at 80 ℃, stirring to obtain a wet gel, drying the wet gel at 120 ℃ for 12 hours, then igniting the wet gel in the air to obtain a fluffy precursor, grinding, calcining, and calcining at 900 ℃ for 3 hours to obtain SNCF;
(3) preparing a graphene/neodymium cobalt doped strontium ferrite composite material: weighing GO and neodymium cobalt doped strontium ferrite according to m (GO) (m (SNCF)) 6:100, respectively adding the GO and the neodymium cobalt doped strontium ferrite into dimethylformamide to obtain a graphene oxide solution and a neodymium cobalt doped strontium ferrite suspension, adding Cetyl Trimethyl Ammonium Bromide (CTAB) (m (CTAB)) 0.8:100 into the graphene oxide solution, performing ultrasonic treatment for 2h, slowly dripping the GO solution into the neodymium cobalt doped strontium ferrite suspension, stirring for 1h to mix uniformly, and mixing according to m (hydrazine hydrate): m (go) ═ 0.7:1, adding hydrazine hydrate into the reaction system, stirring in a water bath at 95 ℃ for 12 hours, then carrying out suction filtration, washing with water and alcohol until the filtrate is neutral, and carrying out vacuum drying at 60 ℃ for 12 hours to obtain the graphene/neodymium-cobalt doped strontium ferrite composite material.
(4) Preparing the graphene-based composite wave-absorbing material: dissolving a graphene/neodymium-cobalt doped strontium ferrite composite material and 1ml of aniline monomer in 30ml of hydrochloric acid solution, wherein the molar ratio of the graphene/neodymium-cobalt doped strontium ferrite composite material to aniline is 1:2.5, and uniformly dispersing to obtain a dispersion liquid; 2.5g of persulfuric acid was takenAmmonium was dissolved in 20ml of 1 mol. L-1And (3) obtaining a transparent solution, slowly dripping the transparent solution into the dispersion, stirring in an ice water bath for 12 hours, and sequentially carrying out suction filtration, water washing, alcohol washing and vacuum drying at 60 ℃ for 12 hours to obtain the graphene-based composite wave-absorbing material.
The phase structure analysis of the graphene-based composite wave-absorbing material prepared in example 1 is performed by using an X-ray diffractometer, and an XRD pattern is shown in fig. 1, in fig. 1: (a) representing SNCF, (b) representing RGO/SNCF nanocomposite, (c) representing RGO/SNCF/PANI nanocomposite, (d) representing GO, (e) representing PANI, and from FIG. 1 we can see that characteristic diffraction peaks appear at 30.1, 32.2, 34.1, 37.0, 40.3, 42.3, 55.20, 56.83 and 63.31, which is comparable to standard SrFe12O19The characteristic peaks of the ferrite are basically consistent, which shows that when the doping amount of the neodymium cobalt is 0.15, the prepared SNCF ferrite is still in a magnetoplumbite type, the neodymium cobalt well enters the crystal lattice of the strontium ferrite, and other impurity phases are not generated. FIGS. 1(b) and (c) show XRD patterns corresponding to RGO/SNCF and RGO/SNCF/PANI, respectively, from which the characteristic peak of SNCF is clearly seen, and not the characteristic peak of GO at around 10 deg. shown in FIG. 1(a), which indicates that GO is reduced to RGO by the action of hydrazine hydrate as a reducing agent, and SNCF is dispersed on RGO sheets by self-assembly. Notably, no significant characteristic peaks of PANI were observed in the XRD patterns of RGO/SNC/PANI, probably due to the lower PANI content in the system.
The electromagnetic parameters and the wave-absorbing performance of the sample are analyzed by using vector network analysis, the result is shown in fig. 2, fig. 2 is a wave-absorbing performance diagram of the graphene-based composite wave-absorbing material prepared in example 1, and is a reflectivity loss curve of the RGO/SNCF/PANI nano composite material with the RGO content of 6% under different thicknesses, and it can be found from fig. 2 that the minimum reflection loss value is-42.4 dB when the thickness is 2mm, the corresponding peak frequency is 14.56GHz, the effective absorption frequency bands are respectively 5.7GHz, and excellent wave-absorbing performance is shown.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (7)
1. A preparation method of a graphene-based composite wave-absorbing material is characterized by comprising the following steps:
(1) preparing graphene oxide: weighing 3-4 g of graphite powder, 2.5-3.5 g of persulfate and 2-4 g P2O5Sequentially adding the mixture into 15-18 ml of concentrated sulfuric acid, stirring for 6-8 h at 80-85 ℃, adding distilled water to dilute the reaction system to a pH value of 4-5 after the reaction system is cooled to room temperature, standing for 20-24 h, filtering, washing with water until the filtrate is neutral, and drying the obtained product to a constant weight at room temperature to obtain pre-oxidized graphite; adding pre-oxidized graphite into 120-150 mL of concentrated sulfuric acid, uniformly stirring, slowly adding 15-18 g of strong oxidant in an ice water bath, uniformly stirring, slowly heating to 35-40 ℃, continuously reacting for 2-4h, slowly adding 250-300 mL of distilled water into a system, then reacting for 2-3 h, controlling the temperature of the system to be not more than 50 ℃, adding 300-350 mL of distilled water again, stirring until the system is uniform, then dropwise adding 10-40 mL of hydrogen peroxide with the concentration of 30%, converting the solution into bright brown, washing with a hydrochloric acid solution after centrifugal separation, finally dialyzing for 7-8 d with distilled water, and freeze-drying the obtained upper-layer dispersion to obtain graphene oxide;
(2) preparing SNCF: according to the chemical formula Sr of neodymium cobalt doped strontium ferrite0.85Nd0.15Co0.15Fe11.85O19Weighing Sr (NO) according to the stoichiometric ratio in3)2，Fe(NO3)3·9H2O，Nd(NO3)3·6H2O，Co(NO3)2·4H2Dissolving O in distilled water, stirring uniformly to obtain a clear solution, slowly dropwise adding a citric acid solution, stirring uniformly, adjusting the pH value to 7 to obtain a sol, evaporating the sol in a 75-85 ℃ water bath, stirring to obtain a wet gel, drying the wet gel, igniting the wet gel in air to obtain a fluffy precursor, grinding and calcining to obtain SNCF;
(3) preparing a graphene/neodymium cobalt doped strontium ferrite composite material: respectively dissolving graphene oxide and neodymium-cobalt-doped strontium ferrite in DMF (dimethyl formamide) to obtain a graphene oxide solution and a neodymium-cobalt-doped strontium ferrite suspension, adding hexadecyl trimethyl ammonium bromide into the graphene oxide solution, dispersing uniformly, slowly dripping the mixture into the neodymium-cobalt-doped strontium ferrite suspension, mixing uniformly, adding hydrazine hydrate into a reaction system, stirring in a water bath at 95 ℃ for 12-14 h, carrying out suction filtration, washing with water and alcohol until the filtrate is neutral, and finally carrying out vacuum drying to obtain a graphene/neodymium-cobalt-doped strontium ferrite composite material;
(4) preparing the graphene-based composite wave-absorbing material: dissolving a graphene/neodymium-cobalt doped strontium ferrite composite material and 1-2 ml of aniline monomer in 30-50 ml of hydrochloric acid solution, wherein the molar ratio of the graphene/neodymium-cobalt doped strontium ferrite composite material to aniline is 1:2.5, and uniformly dispersing to obtain a dispersion liquid; dissolving 2.5-3.5 g of ammonium persulfate in 20-30 ml of hydrochloric acid solution to obtain a transparent solution, slowly dripping the transparent solution into the dispersion, stirring in an ice water bath for 12-15 hours, and sequentially carrying out suction filtration, water washing, alcohol washing and vacuum drying to obtain the graphene-based composite wave-absorbing material;
in the step (2), the molar ratio of citric acid to metal ions is 1: 1;
in the step (2), the calcining temperature is 900 ℃ and the time is 2-4 h;
in the step (3), the molar ratio of graphene oxide to neodymium-cobalt-doped strontium ferrite is 6:100, the molar ratio of hexadecyl trimethyl ammonium bromide to graphene oxide is 0.8:100, and the molar ratio of hydrazine hydrate to graphene oxide is 0.7: 1.
2. The preparation method of the graphene-based composite wave-absorbing material according to claim 1, wherein in the step (1), the persulfate is potassium persulfate or sodium persulfate.
3. The method for preparing the graphene-based composite wave-absorbing material according to claim 1, wherein in the step (1), the strong oxidant is potassium permanganate or potassium dichromate.
4. The preparation method of the graphene-based composite wave-absorbing material of claim 1, wherein in the step (1), the volume concentration of the hydrochloric acid solution is 10%.
5. The preparation method of the graphene-based composite wave-absorbing material according to claim 1, wherein in the step (2), the drying temperature is 120 ℃ and the time is 10-12 h.
6. The preparation method of the graphene-based composite wave-absorbing material according to claim 1, wherein in the step (3), the temperature of vacuum drying is 60 ℃ and the time is 10-12 h.
7. The method for preparing the graphene-based composite wave-absorbing material according to any one of claims 1 to 6, wherein in the step (4), the concentration of the hydrochloric acid solution is 1.0 mol/L.
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