CN112375541A - Nitrogen-doped graphene nickel ferrite composite wave-absorbing material and preparation method thereof - Google Patents
Nitrogen-doped graphene nickel ferrite composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped graphene nickel ferrite composite wave-absorbing material and a preparation method thereof. The nano composite material prepared by the invention is composed of a great number of hexagonal nickel ferrite particles with nanometer sizes entangled by two-dimensional folded graphene, has strong electromagnetic wave absorption capacity, wide absorption frequency band and thin matching thickness, and can generate double absorption peaks at low frequency (3-6GHz) and high frequency (12-18 GHz); the nitrogen doping amount of graphene in the composite material can be changed by controlling the addition volume of hydrazine hydrate, meanwhile, the effective attenuation of the composite material to electromagnetic waves in different wave bands can be realized by changing the matching thickness, and the composite material has important application value in the fields of electromagnetic wave absorption and electromagnetic shielding.
Description
Technical Field
The invention relates to the technical field of electromagnetic composite materials, in particular to a nitrogen-doped graphene-nickel ferrite composite wave-absorbing material and a preparation method thereof.
Background
Due to the excessive use of electronic devices, serious problems of electromagnetic radiation pollution, electromagnetic interference and the like are caused, so that the electromagnetic wave absorbing material gradually becomes a research hotspot in the field of functional materials. An electromagnetic wave absorbing material (wave absorbing material for short) is a material that can absorb and attenuate incident electromagnetic waves, and convert electromagnetic energy into heat energy or other forms of energy to dissipate the energy, or make the electromagnetic waves disappear due to interference. The traditional wave-absorbing materials, such as ferrite, metal micropowder, silicon carbide and the like, usually have the defects of narrow absorption band and high density, thereby limiting the application of the materials in practice. The novel wave-absorbing material generally needs to meet the requirements of thin thickness, light weight, wide absorption frequency band, strong absorption capacity (thin, light, wide and strong) and the like.
Reduced Graphene Oxide (RGO), a novel two-dimensional carbon nanomaterial, is generally prepared from natural graphite by a chemical oxidation-reduction process. RGO has good application prospect in the field of wave-absorbing materials due to the characteristics of unique two-dimensional layered structure, good chemical stability, excellent dielectric loss capacity, ultralow density and the like. However, the single RGO has the disadvantages of poor impedance matching, low electromagnetic wave absorption capability, etc., and the application of the RGO material in the field of electromagnetic wave absorption is limited, and it is difficult to meet the requirement of commercial application (the reflection loss value is lower than-10 dB). Nitrogen atoms and defects are introduced into the RGO lattice using a nitrogen-doping agent (hydrazine hydrate), and dipole polarization and defect polarization are generated, thereby enhancing the attenuation ability to electromagnetic waves.
Nickel ferrite (NiFe)2O4) The magnetic metal oxide has excellent performance, and has good chemical stability, thermal stability, ferromagnetism and other properties. The nano material has the characteristics of quantum effect, macroscopic quantum tunnel effect, small-size effect, interface effect and the like, and can absorb electromagnetic waves strongly when the electronic energy level of the nano particles is split. In addition, the nano material has large specific surface area and high surface atomic ratio, and the special structure of high-concentration grain boundary and grain boundary atoms causes the self-generation of atoms and electrons under the electromagnetic radiationThe movement is intensified, so that the electromagnetic energy is converted into heat energy, and the absorption capacity of the electromagnetic wave is enhanced. NiFe2O4After being compounded with RGO, the composite material has dielectric loss and magnetic loss, is favorable for adjusting the impedance matching of the nano composite material and enhancing the attenuation of incident electromagnetic waves.
According to the electromagnetic theory, the material with excellent wave-absorbing performance generally needs to meet two conditions: good impedance matching and strong attenuation loss. Therefore, the hybrid material constructed by compounding the dielectric loss type RGO and the magnetic material (ferrite, magnetic metal, magnetic alloy and the like) is expected to obtain a light, efficient and broadband wave-absorbing material.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the nitrogen-doped graphene-nickel ferrite composite wave-absorbing material and the preparation method thereof, the prepared nano composite wave-absorbing material is composed of a large number of hexagonal nickel ferrite particles with nanometer sizes, and the composite material has the characteristics of strong absorption, low matching thickness, wide frequency band and the like, and is simple in preparation process and environment-friendly.
The nitrogen-doped graphene-nickel ferrite composite wave-absorbing material provided by the invention is composed of nitrogen-doped reduced graphene oxide loaded hexagonal nano-nickel ferrite.
The method for preparing the nitrogen-doped graphene nickel ferrite composite wave-absorbing material comprises the following steps:
s1: respectively adding deionized water and graphene oxide into a container, stirring and then carrying out ultrasonic treatment to obtain a graphene oxide aqueous dispersion;
s2: adding ferric nitrate nonahydrate and nickel nitrate hexahydrate into the dispersion liquid in the S1, stirring for 5-15min to completely dissolve the ferric nitrate nonahydrate and the nickel nitrate hexahydrate to obtain uniform and transparent dispersion liquid, then adding sodium acetate, and stirring for 10-20min to completely dissolve the sodium acetate;
s3: adding polyethylene glycol into the solution of S2, and stirring in a water bath at 45-55 ℃ to dissolve;
s4: adding hydrazine hydrate into the solution of S3, uniformly mixing, adding ammonia water while stirring to adjust the pH of the mixed solution to 11;
s5: adding the mixed solution in the S4 into a reaction kettle for reaction, cooling to room temperature after the reaction is finished, and centrifugally washing until the pH value of the product is neutral;
s6: pre-freezing the product in the S5 for 10-14h, then freeze-drying for 22-26h, and grinding to obtain the nitrogen-doped graphene-nickel ferrite composite wave-absorbing material.
Preferably, the stirring time in the S1 is 8-12min, and the ultrasonic time is 25-35 min.
Preferably, the molar ratio of the ferric nitrate nonahydrate to the nickel nitrate hexahydrate in the S2 is 2: 1-1.05.
Preferably, the mass molar ratio of the graphene oxide to the ferric nitrate nonahydrate is 20-25mg:1 mmol.
Preferably, the mass ratio of the graphene oxide to the deionized water to the sodium acetate to the polyethylene glycol is 1:1200-1400:30-35: 8-12.
Preferably, the reaction conditions in S5 are a temperature of 180 ℃ and a time of 12 h.
The nitrogen-doped graphene nickel ferrite composite wave-absorbing material provided by the invention is applied to electromagnetic wave absorption and electromagnetic shielding.
The wave absorbing action mechanism is as follows: the nitrogen-doped graphene nickel ferrite composite wave-absorbing material (NRGO/hNiFe) prepared by the invention2O4) Oxygen-containing functional groups and structural defects carried by the surface of the RGO can generate dipole polarization under an alternating electromagnetic field, and nitrogen is doped in RGO crystal lattices to introduce the structural defects so as to enhance the attenuation capability of the RGO crystal lattices to electromagnetic waves; the hexagonal nickel ferrite is introduced, so that the impedance matching of the composite material can be regulated and controlled, and the magnetic loss capability of the composite material is enhanced; the two-dimensional folded graphene intertwined hexagonal nickel ferrite nano particles lead to the composite material having rich heterogeneous interfaces and enhance the polarization effect of the interfaces. The attenuation loss of the composite material to electromagnetic waves is enhanced through mechanisms such as interface polarization, dipole polarization, defect polarization and the like and synergistic effects of conductive loss and magnetic loss.
Compared with the prior art, the invention has the beneficial technical effects that:
(1) the invention adopts a hydrothermal method to prepare NRGO/hNiFe in one step2O4The nano composite wave-absorbing material has simple reaction method and easily obtained material,the method has the advantages that no toxic and harmful substance is generated, the method is green and environment-friendly, no inert gas is needed for protection, hydrazine hydrate is used as a nitrogen doping reagent, and the nitrogen doping amount in the graphene is regulated and controlled by changing the adding volume of the hydrazine hydrate.
(2) According to the invention, the pH value of the system is adjusted to 11 by controlling the hydrothermal temperature and time, and the hydrazine hydrate is added, so that the nickel ferrite in the prepared composite material has a unique hexagonal shape.
(3) NRGO/hNiFe prepared by the invention2O4The nano composite material has excellent wave absorbing performance, has the characteristics of strong absorption, wide frequency band, low matching thickness and the like, the minimum reflection loss can reach-54.4 dB under the thickness of 2.2mm, and the effective wave absorbing width is 4.5GHz under the thickness of 1.5 mm; the absorption capacity of the composite material to electromagnetic waves can be regulated and controlled by changing the nitrogen doping amount, the matching thickness and the filling ratio of the graphene.
(4) NRGO/hNiFe prepared by the invention2O4The nano composite material has unique double absorption capacity and can simultaneously absorb electromagnetic waves at low frequency (3-6GHz) and high frequency (12-18 GHz).
Drawings
FIG. 1 is an XRD pattern of the product of examples 1-3;
FIG. 2 is a TEM photograph (scale 100nm) of product S3 from example 3;
FIG. 3 is a TEM photograph (scale 50nm) of product S3 from example 3;
FIG. 4 is an XPS survey of the product S3 from example 3;
FIG. 5 is an XPS C1S spectrum of the product S3 of example 3;
FIG. 6 is an XPS O1S spectrum of the product S3 of example 3;
FIG. 7 is an XPS N1S spectrum of the product S3 from example 3;
FIG. 8 is an XPS Fe 2p spectrum of the product S3 from example 3;
FIG. 9 is an XPS Ni 2p spectrum of product S3 from example 3;
FIG. 10 is a plot of reflection loss versus frequency for the product S1 of example 1 having a fill ratio of 50 wt.%;
FIG. 11 is a plot of reflection loss versus frequency for the product S2 of example 2 having a fill ratio of 50 wt.%;
FIG. 12 is a plot of reflection loss versus frequency for the product S3 of example 3 having a fill ratio of 50 wt.%.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
1. The raw material sources are as follows: graphite oxide, Suzhou carbofeng graphene science and technology limited, Fe (NO)3)3·9H2O，Ni(NO3)2·6H2O, anhydrous sodium acetate, polyethylene glycol (PEG, Mw 6000g · mol)-1) Hydrazine hydrate, ammonia, absolute ethanol were purchased from hadamard, all samples were analytically pure and no further purification treatment was required.
2. The instrument equipment comprises: JA2003N electronic balance, shanghai precision scientific instruments ltd; XD-1800D ultrasonic cleaner, Inc., of the firm International (hong Kong) group.
3. Test method
(1) X-ray diffraction (XRD) test: the crystal structure of the sample is characterized by adopting a LabX XRD-6000 type X-ray diffractometer, wherein the X-ray is Cu-Kalpha ray, the wavelength is 0.154nm, the step length is 0.02 degrees, the light tube current is 36kV, the current is 30mA, the scanning angle is 10-70 degrees, and the scanning speed is 2 degrees/min-1。
(2) Transmission Electron Microscope (TEM) testing: the microstructure of the sample was characterized using a transmission electron microscope model FEI-TF 20. And (3) taking a small amount of sample to be subjected to ultrasonic dispersion in distilled water, dropwise adding the sample to a copper net, drying, sampling and testing.
(3) X-ray photoelectron spectroscopy (XPS) test: uniformly coating a small amount of sample on the surface of the aluminum foil stuck with the conductive adhesive, pressing into a thin sheet, shearing the thin sheet into a sample with a certain shape and size by using scissors, sticking the sample on a sample injection platform, and testing by adopting ESCALAB 250XI model XPS.
(4) And (3) testing microwave absorption performance: the powder product and paraffin are pressed into a coaxial ring sample with the outer diameter of 7.00mm, the inner diameter of 3.04mm and the thickness of about 2mm in a special die according to the mass ratio of 1:1, an AV3629D vector network analyzer is used for testing the electromagnetic parameters of the sample, the wave absorbing performance is obtained through calculation, and the testing frequency is 2-18 GHz.
Example 1
The method for preparing the nitrogen-doped graphene nickel ferrite composite wave-absorbing material comprises the following steps:
s1: respectively adding 120mL of deionized water and 90mg of graphene oxide into a container, stirring for 10min, and then carrying out ultrasonic treatment for 30min to prepare a graphene oxide aqueous dispersion solution with the concentration of 0.75 mg/mL;
s2: to the dispersion described in S1 was added 1.616g (4mmol) of iron nitrate nonahydrate (Fe (NO)3)3·9H2O) and 0.582g (2mmol) of nickel nitrate hexahydrate (Ni (NO)3)2·6H2O), stirring for 10min to completely dissolve to obtain uniform and transparent dispersion, then adding 2.7g of sodium acetate, and stirring for 15min to completely dissolve;
s3: adding 0.75g of polyethylene glycol into the solution of S2, and stirring the mixture at the temperature of 50 ℃ in a water bath to dissolve the polyethylene glycol;
s4: adding 5mL of hydrazine hydrate into the solution of S3, stirring for 10min to obtain a uniform dispersion liquid, uniformly mixing, adding ammonia water while stirring to adjust the pH of the mixed liquid to 11;
s5: adding the mixed solution in the S4 into a reaction kettle, carrying out hydrothermal reaction for 12h at 180 ℃, cooling to room temperature after the reaction is finished, repeatedly centrifuging, and washing with deionized water for multiple times to enable the pH of the product to be neutral;
s6: pre-freezing the product in the S5 for 12h, then freezing and drying for 24h, and grinding to obtain the nitrogen-doped graphene-nickel-iron-oxide composite wave-absorbing material, which is marked as S1.
Example 2
The method for preparing the nitrogen-doped graphene nickel ferrite composite wave-absorbing material comprises the following steps:
s1: respectively adding 120mL of deionized water and 90mg of graphene oxide into a container, stirring for 10min, and then carrying out ultrasonic treatment for 30min to prepare a graphene oxide aqueous dispersion solution with the concentration of 0.75 mg/mL;
s2: to the dispersion described in S1 was added 1.616g (4mmol) of iron nitrate nonahydrate (Fe (NO)3)3·9H2O) and 0.582g (2mmol) of nickel nitrate hexahydrate (Ni (NO)3)2·6H2O), stirring for 10min to completely dissolve,obtaining uniform and transparent dispersion liquid, then adding 2.7g of sodium acetate, and stirring for 15min until the sodium acetate is completely dissolved;
s3: adding 0.75g of polyethylene glycol into the solution of S2, and stirring the mixture at the temperature of 50 ℃ in a water bath to dissolve the polyethylene glycol;
s4: adding 10mL of hydrazine hydrate into the solution of S3, stirring for 10min to obtain a uniform dispersion liquid, uniformly mixing, adding ammonia water while stirring to adjust the pH of the mixed liquid to 11;
s5: adding the mixed solution in the S4 into a reaction kettle, carrying out hydrothermal reaction for 12h at 180 ℃, cooling to room temperature after the reaction is finished, repeatedly centrifuging, and washing with deionized water for multiple times to enable the pH of the product to be neutral;
s6: pre-freezing the product in the S5 for 12h, then freezing and drying for 24h, and grinding to obtain the nitrogen-doped graphene-nickel-iron-oxide composite wave-absorbing material, which is marked as S2.
Example 3
The method for preparing the nitrogen-doped graphene nickel ferrite composite wave-absorbing material comprises the following steps:
s1: respectively adding 120mL of deionized water and 90mg of graphene oxide into a container, stirring for 10min, and then carrying out ultrasonic treatment for 30min to prepare a graphene oxide aqueous dispersion solution with the concentration of 0.75 mg/mL;
s2: to the dispersion described in S1 was added 1.616g (4mmol) of iron nitrate nonahydrate (Fe (NO)3)3·9H2O) and 0.582g (2mmol) of nickel nitrate hexahydrate (Ni (NO)3)2·6H2O), stirring for 10min to completely dissolve to obtain uniform and transparent dispersion, then adding 2.7g of sodium acetate, and stirring for 15min to completely dissolve;
s3: adding 0.75g of polyethylene glycol into the solution of S2, and stirring the mixture at the temperature of 50 ℃ in a water bath to dissolve the polyethylene glycol;
s4: adding 15mL of hydrazine hydrate into the solution of S3, stirring for 10min to obtain a uniform dispersion liquid, uniformly mixing, adding ammonia water while stirring to adjust the pH of the mixed liquid to 11;
s5: adding the mixed solution in the S4 into a reaction kettle, carrying out hydrothermal reaction for 12h at 180 ℃, cooling to room temperature after the reaction is finished, repeatedly centrifuging, and washing with deionized water for multiple times to enable the pH of the product to be neutral;
s6: pre-freezing the product in the S5 for 12h, then freezing and drying for 24h, and grinding to obtain the nitrogen-doped graphene-nickel-iron-oxide composite wave-absorbing material, which is marked as S3.
The samples S1, S2 and S3 prepared in examples 1 to 3 were subjected to performance tests, in which fig. 1 is an XRD pattern of S1, S2 and S3, and 2 θ is 30.3 °, 35.7 °, 43.3 °, 57.3 ° and 63.0 ° with NiFe2O4The corresponding positions of the crystal faces of the standard card (JCPDS 10-0325) (220), (311), (400), (511) and (440) are consistent, and no other characteristic peak is seen in the figure, which indicates that NiFe is prepared under the experimental condition2O4Particles.
FIGS. 2 and 3 are NRGO/hNiFe prepared in example 32O4TEM photograph of the nanocomposite (S3), from which it can be seen that NiFe was prepared2O4The particles have obvious hexagonal morphology, and in addition, the NiFe with hexagonal shape2O4The particles are uniformly supported on the wrinkled graphene sheet layer.
FIGS. 4-8 are NRGO/hNiFe samples prepared in example 32O4XPS spectra of the nanocomposites (S3). Wherein FIG. 3 is NRGO/hNiFe2O4The total spectrum of the nano-composite shows that the sample contains N, C, O, Ni and Fe elements, and the types of the elements are consistent with those of the elements in the prepared nano-composite. Fig. 4 shows the spectrum of C1s, with the peak at 284.8eV corresponding to the C-C/C-C bond, the peak at 286.4eV corresponding to the C-N bond, and the peak at 290.6eV corresponding to the C-O bond. FIG. 5 shows the spectrum of O1s with peaks at 530.8eV, 533eV, 531.7eV, and 530.2eV corresponding to O-C ═ O, C-O, Fe-O-C, and Fe-O bonds, respectively. Fig. 6 shows a spectrum of N1 s, and the types of N can be classified into pyridine nitrogen, pyrrole nitrogen, graphite nitrogen, and nitrogen oxide. FIG. 7 shows a spectrum of Fe 2p, in which peaks at 714.3eV and 711.3eV correspond to Fe 2p3/2And the peak at 724.8eV corresponds to Fe 2p1/2. FIG. 8 shows the spectrum of Ni 2p, in which the peaks at 873.4eV and 855.7eV correspond to Ni 2p1/2And Ni 2p3/2。
Mixing NRGO/hNiFe2O4The nano-composite powder product and paraffin are pressed into the same product with the outer diameter of 7.00mm, the inner diameter of 3.04mm and the thickness of about 2mm in a special die according to the mass ratio of 1:1And (3) testing the electromagnetic parameters of the shaft sample by using an AV3629D vector network analyzer, and calculating to obtain the wave-absorbing performance, wherein the testing frequency is 2-18 GHz. The reflection loss versus frequency curve of sample S1 is shown in FIG. 9, and the maximum absorption intensity reached-33.84 dB at 8.16GHz with a matching thickness of 2.5 mm. The reflection loss of sample S2 as a function of frequency is shown in FIG. 10, and the minimum reflection loss reaches-18.57 dB at 13.44GHz with a matching thickness of 1.5 mm. The reflection loss of sample S3 as a function of frequency is shown in FIG. 11, and when the matching thickness is 2.2mm, the minimum reflection loss value reaches-54.4 dB at 9.2 GHz.
Example 4
The method for preparing the nitrogen-doped graphene nickel ferrite composite wave-absorbing material comprises the following steps:
s1: respectively adding 120mL of deionized water and 100mg of graphene oxide into a container, stirring for 8min, and performing ultrasonic treatment for 25min to obtain a graphene oxide aqueous dispersion;
s2: to the dispersion described in S1 was added 5mmol of iron nitrate nonahydrate (Fe (NO)3)3·9H2O) and 2.5mmol Nickel nitrate hexahydrate (Ni (NO)3)2·6H2O), stirring for 5min to completely dissolve to obtain uniform and transparent dispersion, then adding 3g of sodium acetate, and stirring for 10min to completely dissolve;
s3: adding 0.8g of polyethylene glycol into the solution of S2, and stirring the mixture at the temperature of 45 ℃ in a water bath to dissolve the polyethylene glycol;
s4: adding 5mL of hydrazine hydrate into the solution of S3, stirring for 10min to obtain a uniform dispersion liquid, uniformly mixing, adding ammonia water while stirring to adjust the pH of the mixed liquid to 11;
s5: adding the mixed solution in the S4 into a reaction kettle, carrying out hydrothermal reaction for 12h at 180 ℃, cooling to room temperature after the reaction is finished, repeatedly centrifuging, and washing with deionized water for multiple times to enable the pH of the product to be neutral;
s6: pre-freezing the product in the S5 for 10h, then freezing and drying for 22h, and grinding to obtain the nitrogen-doped graphene nickel ferrite composite wave-absorbing material.
Example 5
The method for preparing the nitrogen-doped graphene nickel ferrite composite wave-absorbing material comprises the following steps:
s1: respectively adding 180mL of deionized water and 100mg of graphene oxide into a container, stirring for 12min, and performing ultrasonic treatment for 35min to obtain a graphene oxide aqueous dispersion;
s2: to the dispersion described in S1 was added 4mmol of iron nitrate nonahydrate (Fe (NO)3)3·9H2O) and 2mmol Nickel nitrate hexahydrate (Ni (NO)3)2·6H2O), stirring for 15min to completely dissolve to obtain uniform and transparent dispersion, then adding 3.5g of sodium acetate, and stirring for 20min to completely dissolve;
s3: adding 1.2g of polyethylene glycol into the solution of S2, and stirring the mixture at the temperature of 55 ℃ in a water bath to dissolve the polyethylene glycol;
s4: adding 15mL of hydrazine hydrate into the solution of S3, stirring for 10min to obtain a uniform dispersion liquid, uniformly mixing, adding ammonia water while stirring to adjust the pH of the mixed liquid to 11;
s5: adding the mixed solution in the S4 into a reaction kettle, carrying out hydrothermal reaction for 12h at 180 ℃, cooling to room temperature after the reaction is finished, repeatedly centrifuging, and washing with deionized water for multiple times to enable the pH of the product to be neutral;
s6: and pre-freezing the product in the S5 for 14h, then freezing and drying for 26h, and grinding to obtain the nitrogen-doped graphene nickel ferrite composite wave-absorbing material.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The nitrogen-doped graphene-nickel ferrite composite wave-absorbing material is characterized by being composed of nitrogen-doped reduced graphene oxide loaded hexagonal nano-nickel ferrite.
2. The method for preparing the nitrogen-doped graphene-nickel-iron-ferrite composite wave-absorbing material according to claim 1, characterized by comprising the following steps:
s1: respectively adding deionized water and graphene oxide into a container, stirring and then carrying out ultrasonic treatment to obtain a graphene oxide aqueous dispersion;
s2: adding ferric nitrate nonahydrate and nickel nitrate hexahydrate into the dispersion liquid in the S1, stirring for 5-15min to completely dissolve the ferric nitrate nonahydrate and the nickel nitrate hexahydrate to obtain uniform and transparent dispersion liquid, then adding sodium acetate, and stirring for 10-20min to completely dissolve the sodium acetate;
s3: adding polyethylene glycol into the solution of S2, and stirring in a water bath at 45-55 ℃ to dissolve;
s4: adding hydrazine hydrate into the solution of S3, uniformly mixing, adding ammonia water while stirring to adjust the pH of the mixed solution to 11;
s5: adding the mixed solution in the S4 into a reaction kettle for reaction, cooling to room temperature after the reaction is finished, and centrifugally washing until the pH value of the product is neutral;
s6: pre-freezing the product in the S5 for 10-14h, then freeze-drying for 22-26h, and grinding to obtain the nitrogen-doped graphene-nickel ferrite composite wave-absorbing material.
3. The method for preparing the nitrogen-doped graphene-nickel-iron-ferrite composite wave-absorbing material according to claim 2, wherein the stirring time in S1 is 8-12min, and the ultrasonic time is 25-35 min.
4. The method for preparing the nitrogen-doped graphene-nickel-ferrite composite wave-absorbing material according to claim 2, wherein the molar ratio of ferric nitrate nonahydrate to nickel nitrate hexahydrate in S2 is 2: 1-1.05.
5. The method for preparing the nitrogen-doped graphene-nickel-iron-ferrite composite wave-absorbing material according to claim 2, wherein the mass molar ratio of the graphene oxide to the ferric nitrate nonahydrate is 20-25mg:1 mmol.
6. The preparation method of the nitrogen-doped graphene-nickel-iron-ferrite composite wave-absorbing material as claimed in claim 2, wherein the mass ratio of the graphene oxide to the deionized water to the sodium acetate to the polyethylene glycol is 1:1200-1400:30-35: 8-12.
7. The method for preparing the nitrogen-doped graphene-nickel-ferrite composite wave-absorbing material according to claim 2, wherein the reaction condition in the S5 is 180 ℃ and 12 h.
8. The nitrogen-doped graphene-nickel-iron-ferrite composite wave-absorbing material as claimed in claim 1 is applied to electromagnetic wave absorption and electromagnetic shielding.
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