CN113277501A - Nitrogen-doped reduced graphene oxide aerogel and application thereof in preparation of microwave absorbing material - Google Patents
Nitrogen-doped reduced graphene oxide aerogel and application thereof in preparation of microwave absorbing material Download PDFInfo
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- CN113277501A CN113277501A CN202110519430.4A CN202110519430A CN113277501A CN 113277501 A CN113277501 A CN 113277501A CN 202110519430 A CN202110519430 A CN 202110519430A CN 113277501 A CN113277501 A CN 113277501A
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Abstract
The invention discloses nitrogen-doped reduced graphene oxide aerogel and application thereof in preparation of microwave absorbing materials. The preparation method of the nitrogen-doped reduced graphene oxide aerogel comprises the following steps: ultrasonically and uniformly mixing the graphene oxide dispersion liquid, urea and ethylene glycol, and then transferring the mixture into a hydrothermal reaction kettle for hydrothermal reduction reaction to obtain nitrogen-doped reduced graphene oxide hydrogel; and (3) placing the hydrogel in an ethanol water solution to remove surface impurities, and finally performing a freeze drying process to obtain the nitrogen-doped reduced graphene oxide aerogel with the ultralight three-dimensional porous structure. And uniformly mixing the nitrogen-doped reduced graphene oxide aerogel with paraffin, compacting, measuring and analyzing the microwave absorption performance of the nitrogen-doped reduced graphene oxide aerogel. The preparation method is short in preparation period and simple, the used reagent is non-toxic and harmless, and the prepared aerogel shows excellent dielectric property and microwave absorption property and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of microwave absorbing materials, and particularly relates to nitrogen-doped reduced graphene oxide aerogel and application thereof in preparation of microwave absorbing materials.
Background
At present, with the wide application of electromagnetic technology in various fields such as communication, medicine, scientific research, military and the like, while providing convenience for human life and promoting the development of human society, the normal life of people is greatly influenced by the caused electromagnetic pollution, and electromagnetic pollution such as electromagnetic radiation, electromagnetic interference and the like becomes a new pollution besides noise pollution, air pollution and water pollution. Therefore, how to reduce electromagnetic pollution while making full use of electromagnetic technology has recently become a hot research topic.
The microwave absorbing material can attenuate and absorb electromagnetic waves incident into the material, and is an important measure for attenuating the electromagnetic waves and solving the problem of electromagnetic pollution. With the rapid development of various technologies, the demand for efficient microwave absorbing materials is increasing, and the design of electromagnetic wave absorbing materials is also demanding. The high-efficiency microwave absorbing material has the characteristics of thin matching thickness, wide absorbing frequency band, light weight and the like besides high loss capacity. In the military field, the wave-absorbing material is widely used in stealth technology, absorbs electromagnetic waves incident to the surface of equipment, and reduces the detectability of targets. In the civil field, as an electromagnetic protection material, the wave-absorbing material can reduce the harm of electromagnetic radiation to human bodies and the interference to precise instruments and equipment. Therefore, the wave-absorbing material has wide application prospect in both military field and civil field. As a research hotspot at home and abroad, continuous scholars are invested in the research of microwave absorbing materials, and various novel microwave absorbing materials emerge endlessly.
The attenuation mechanism of the microwave absorption material can be divided into two types of dielectric loss and magnetic loss mainly according to the material characteristics, and the dielectric loss is generally divided into two types of conductance loss and polarization loss; magnetic losses mainly include natural resonance, exchange resonance, and eddy current losses. When electromagnetic waves enter the surface of a material, the impedance matching principle of the material needs to be met, otherwise, the electromagnetic waves are reflected on the surface of the material, and meanwhile, when the electromagnetic waves enter the material, the material needs to have strong loss attenuation capacity, so that the electromagnetic wave energy is consumed in the material. Therefore, it is desirable that an ideal microwave absorbing material has strong electromagnetic wave attenuation capability and excellent impedance matching, so that as much electromagnetic wave as possible can be incident into the material and be attenuated in a large amount. In addition, the structure of the material also has great influence on the wave absorbing performance of the material.
The traditional wave-absorbing material often has the defects of large thickness, large density, high load, weak absorption strength and the like, so that the research and preparation of the wave-absorbing material meeting the characteristics of thinness, lightness, width and strength have very important significance. Since the discovery of graphene, graphene has been applied to various fields such as sensors, biological materials, and energy storage materials. It is widely studied due to its excellent physical/chemical properties, high specific surface area, high electron mobility and low density, and is considered to be a material well suited for microwave absorption, but its application in the microwave absorption field is greatly limited due to its serious agglomeration and accumulation.
Disclosure of Invention
The invention aims to provide a nitrogen-doped reduced graphene oxide aerogel and application thereof in preparation of a microwave absorbing material. The microwave absorbing material prepared by the invention can realize high-performance microwave absorption with ultra-low filling ratio and ultra-large absorption bandwidth.
The preparation method of the nitrogen-doped reduced graphene oxide aerogel comprises the following steps: ultrasonically and uniformly mixing the graphene oxide dispersion liquid, urea and ethylene glycol, and then transferring the mixture to a hydrothermal reaction kettle for hydrothermal reduction reaction to obtain nitrogen-doped reduced graphene oxide hydrogel; and (3) placing the hydrogel in an ethanol water solution to remove surface impurities, and finally freezing and drying to obtain the nitrogen-doped reduced graphene oxide aerogel with the ultralight three-dimensional porous structure.
The concentration of the graphene oxide dispersion liquid is 2-8 mg/mL.
The mass ratio of the graphene oxide to the urea is 3:10-3: 30.
The temperature of the hydrothermal reduction reaction is 160-240 ℃, and the reaction time is 1-5 hours.
The volume ratio of the ethylene glycol to the graphene oxide dispersion liquid is 1:3-1: 1.
The ethanol water solution is formed by mixing ethanol and water in a volume ratio of 1:9-3: 7.
The preparation method of the microwave absorbing material comprises the following steps: and uniformly mixing the prepared nitrogen-doped reduced graphene oxide aerogel with a carrier to obtain the microwave absorbing material.
According to the invention, the nitrogen-doped reduced graphene oxide aerogel is prepared by adopting a reduction method, the prepared aerogel has a three-dimensional porous net-shaped structure, the problem that pure graphene sheets are agglomerated and stacked under the action of van der Waals force is solved, the high specific surface area and the ultrahigh electron mobility required by a microwave absorbing material are provided, electromagnetic waves are subjected to multiple reflection and scattering among graphene sheets, the electromagnetic waves are attenuated for multiple times, the impedance matching and attenuation capacity of an absorber is remarkably improved, and the microwave absorbing performance of the graphene material is improved. The preparation method is short in preparation period and simple, the used reagent is non-toxic and harmless, and the prepared aerogel shows excellent dielectric property and microwave absorption property and has good application prospect.
Drawings
FIG. 1 shows the microwave absorption performance of the microwave absorbing material prepared from the nitrogen-doped reduced graphene oxide aerogel obtained from the graphene oxide and urea in example 1 in a mass ratio of 3:20 in application example 1 in the range of 2-18GHz, wherein the microwave absorbing material has the lowest reflection loss of-27.86 dB at 2mm and the maximum absorption bandwidth of 7.24GHz at 2.51 mm.
Fig. 2 is an XPS image of the nitrogen-doped reduced graphene oxide aerogel prepared from 3:20 mass ratio graphene oxide to urea in example 1, in which an C, N, O element characteristic peak is clearly seen, confirming the successful preparation of the nitrogen-doped reduced graphene oxide aerogel.
Fig. 3 is SEM and TEM images of the nitrogen-doped reduced graphene oxide aerogel prepared in example 1, which shows that the nitrogen-doped reduced graphene oxide aerogel has a three-dimensional porous structure and graphene sheets have a multi-fold structure.
Detailed Description
Example 1:
preparing 5mg/ml of water dispersion liquid from graphene oxide prepared by an improved Hummer method at room temperature, and carrying out ultrasonic treatment for 4 hours; respectively adding 6mL of oxygen into 100 mg, 200 mg and 300mg of ureaDissolving graphene aqueous dispersion, dropwise adding 4mL of ethylene glycol, carrying out ultrasonic treatment for 1 hour, transferring to a hydrothermal reaction kettle for hydrothermal reduction reaction at 200 ℃ for 3 hours, and cooling to room temperature after complete reaction to obtain nitrogen-doped reduced graphene oxide hydrogel; placing the hydrogel in an ethanol water solution (the volume ratio of ethanol to water is 1:9) for 10 hours to remove unreacted impurities on the surface of the material; and finally, freezing the purified hydrogel for 4 hours, and vacuumizing for 24 hours to obtain the nitrogen-doped reduced graphene oxide aerogel with the ultralight three-dimensional porous structure. The aerogel density was 22.73mg/cm3. Application example 1:
the nitrogen-doped reduced graphene oxide aerogel prepared in example 1 (a sample prepared from graphene oxide and urea in a mass ratio of 3: 20) and paraffin were uniformly mixed in a mass ratio of 1:9, pressed into a coaxial ring with an outer diameter of 7.00mm and an inner diameter of 3.04mm by using a compression ring die, and the microwave absorption performance of the material was analyzed by measuring the relevant electromagnetic parameters of the material in a range of 2-18GHz by using a vector network analyzer.
Claims (7)
1. The preparation method of the nitrogen-doped reduced graphene oxide aerogel is characterized by comprising the following specific steps: ultrasonically and uniformly mixing the graphene oxide dispersion liquid, urea and ethylene glycol, and then transferring the mixture into a hydrothermal reaction kettle for hydrothermal reduction reaction to obtain nitrogen-doped reduced graphene oxide hydrogel; and (3) placing the hydrogel in an ethanol water solution to remove surface impurities, and finally freezing and drying to obtain the nitrogen-doped reduced graphene oxide aerogel with the ultralight three-dimensional porous structure.
2. The method according to claim 1, wherein the graphene oxide dispersion has a concentration of 2 to 8 mg/mL.
3. The preparation method according to claim 1, wherein the mass ratio of the graphene oxide to the urea is 3:10 to 3: 30.
4. The method as claimed in claim 1, wherein the hydrothermal reduction reaction is carried out at a temperature of 160 ℃ and 240 ℃ for a period of 1-5 hours.
5. The preparation method according to claim 1, wherein the volume ratio of the ethylene glycol to the graphene oxide dispersion liquid is 1:3 to 1: 1.
6. The method according to claim 1, wherein the aqueous ethanol solution is prepared by mixing ethanol and water in a volume ratio of 1:9 to 3: 7.
7. A preparation method of a microwave absorbing material is characterized in that the nitrogen-doped reduced graphene oxide aerogel prepared by the method of any one of claims 1 to 4 is uniformly mixed with a carrier to obtain the microwave absorbing material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114195136A (en) * | 2022-01-05 | 2022-03-18 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
| CN114853502A (en) * | 2022-05-26 | 2022-08-05 | 哈尔滨工业大学（威海） | Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof |
| CN116218027A (en) * | 2023-02-08 | 2023-06-06 | 山东大学 | Aerogel wave-absorbing material, electromagnetic wave absorber, preparation method and application thereof |
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| CN114195136A (en) * | 2022-01-05 | 2022-03-18 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
| CN114195136B (en) * | 2022-01-05 | 2023-07-07 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
| CN114853502A (en) * | 2022-05-26 | 2022-08-05 | 哈尔滨工业大学（威海） | Ceramic/graphene aerogel wave-absorbing material and preparation method and application thereof |
| CN116218027A (en) * | 2023-02-08 | 2023-06-06 | 山东大学 | Aerogel wave-absorbing material, electromagnetic wave absorber, preparation method and application thereof |
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