CN-122010109-A - Nitrogen doping method of gamma-graphite alkyne and application thereof

Abstract

The invention belongs to the technical field of nano materials, in particular to a nitrogen doping method of gamma-graphite alkyne and application thereof, the invention adopts a hydrothermal method to prepare graphite alkyne oxide, takes melamine as a nitrogen source, takes graphite alkyne oxide as a framework, realizes in-situ doping of nitrogen element and reduction of the graphite alkyne oxide simultaneously through high-temperature calcination, the method is simple and easy to implement, the processing period is short, the doping amount is easy to control, dangerous chemicals such as concentrated sulfuric acid and concentrated nitric acid are not involved, the production safety is greatly improved, and the prepared nitrogen doped gamma-graphite alkyne has the advantages of high purity, high specific surface area, nano-scale aperture, excellent wave absorption performance, gas sensitivity and ferromagnetism.

Inventors

• ZHANG YUCHEN
• YANG WUBIN
• LI FUYANG
• YANG TONGSHENG
• LIANG HAO

Assignees

• 贵州铂韬电子科技有限公司

Dates

Publication Date

20260512

Application Date

20260116

Claims (9)

1. 1. The nitrogen doping method of the gamma-graphite alkyne is characterized by comprising the following steps of: 1) Preparing gamma-graphite alkyne dispersion liquid, namely weighing gamma-graphite alkyne, placing the gamma-graphite alkyne in deionized water, and fully dispersing the gamma-graphite alkyne by adopting ultrasonic dispersion and mechanical stirring modes to prepare the gamma-graphite alkyne dispersion liquid; 2) Adding oxidant into gamma-graphite alkyne dispersion liquid, magnetically stirring, placing the mixture in a high-pressure reaction kettle for hydrothermal reaction, naturally cooling and extracting the mixture after the hydrothermal reaction is finished to obtain a mixture, soaking the mixture in hydrochloric acid to remove the oxidant which is not completely reacted, carrying out suction filtration after the soaking is finished to obtain a precipitate, washing the precipitate to be neutral with deionized water, and drying the precipitate to obtain the gamma-graphite alkyne oxide; 3) And (3) preparing the nitrogen-doped gamma-graphite alkyne, namely uniformly mixing melamine and oxidized gamma-graphite alkyne, calcining at a high temperature in an inert gas atmosphere, and cooling to room temperature to obtain the nitrogen-doped gamma-graphite alkyne.
2. 2. The method for doping gamma-graphite alkyne with nitrogen according to claim 1, wherein in the step 1), the mass-volume ratio of gamma-graphite alkyne to deionized water in the gamma-graphite alkyne dispersion solution is 1 mg/1-3 ml.
3. 3. The method for doping nitrogen into gamma-graphite alkyne according to claim 1, wherein in the step 2), the amount of the oxidant is 1.5-2.5 times of the mass of the gamma-graphite alkyne, and the oxidant is potassium permanganate.
4. 4. The method for doping gamma-graphite alkyne with nitrogen as claimed in claim 1, wherein in the step 2), the hydrothermal reaction is carried out at 180-200 ℃ for 2-5 hours.
5. 5. The nitrogen doping method of gamma-graphite alkyne as claimed in claim 1, wherein in the step 2), the mass fraction of hydrochloric acid is 37%, and the soaking time is 36-60 h.
6. 6. The method for doping gamma-graphite alkyne with nitrogen as claimed in claim 1, wherein in the step 2), the drying process is carried out at a temperature of 70 ℃ for 24-36 hours.
7. 7. The nitrogen doping method of gamma-graphite alkyne according to claim 1, wherein in the step 3), the mass ratio of melamine to gamma-graphite alkyne oxide is 20-35:1.
8. 8. The method for doping gamma-graphite alkyne in nitrogen according to claim 1, wherein in the step 3), the high-temperature calcination is performed by heating the material from room temperature to 700-900 ℃ and then calcining at constant temperature for 2-4 hours. The rate of temperature rise was 5℃/min.
9. 9. Use of a nitrogen-doped gamma-graphite alkyne prepared by a nitrogen doping method of a gamma-graphite alkyne according to any one of claims 1 to 8 in the preparation of magnetic materials, radar stealth materials, electromagnetic shielding materials or gas monitoring materials.

Description

Nitrogen doping method of gamma-graphite alkyne and application thereof Technical Field The invention belongs to the technical field of nano materials, and particularly relates to a nitrogen doping method of gamma-graphite alkyne and application thereof. Background With the acceleration of industrialization and the continuous expansion of urban scale, the problems of electromagnetic radiation and gas pollution are increasingly serious, and the problems have become a global challenge threatening human health and ecological environment. Wherein, the human activities such as industrial production, automobile exhaust, fossil fuel combustion and the like discharge a large amount of toxic and harmful gases into the atmosphere, and the air pollutants not only directly harm human health, but also can cause environmental problems such as acid rain, photochemical smog, greenhouse effect and the like, thereby causing profound influence on an ecological system. Long-term exposure to contaminating gases can lead to respiratory diseases, cardiovascular diseases and even cancer, which are serious threats to human life health. And the problems of electromagnetic interference, signal leakage and the like not only affect the performance of equipment, but also have obvious influence on the life quality of people. For example, long-term exposure to electromagnetic radiation can cause irreversible damage, resulting in various diseases such as childhood leukemia, fetal malformation, and failure of healthy development of teenagers, and also has a risk of cancer. A large amount of electromagnetic pollution can also affect plants, so that the plants cannot grow normally, and the genes are mutated and even die. In addition, electromagnetic waves interfere with electronic equipment, instruments, communication signals and the like, and normal use is affected. Therefore, the development of the multifunctional electronic material with the wave absorbing performance and the gas-sensitive performance has important significance, namely the absorption of electromagnetic waves by the wave absorbing material is realized, the influence of electromagnetic interference on the gas-sensitive performance is reduced, the material support is provided for improving the stability and the reliability of the gas sensor, and meanwhile, the absorption of gas molecules by the gas-sensitive material is utilized to regulate and control the electromagnetic parameters of the wave absorbing material, the dynamic regulation and control of the wave absorbing performance is realized, and a feasible path is provided for developing the intelligent tunable wave absorbing material. Although carbon-based materials are generally considered to have wave-absorbing properties and can also be used as gas-sensitive materials, conventional carbon-based wave-absorbing materials are not magnetic and generally need to be compounded with magnetic materials to balance their high-conductivity characteristics so as to achieve better impedance matching, but this tends to result in complex manufacturing processes and increased costs. The graphite alkyne is composed of all-carbon macromolecules with two-dimensional planar network structures, which are formed by conjugated connection of benzene rings through 1, 3-diacetylene bonds, and has rich carbon chemical bonds, a large conjugated system, wide interplanar spacing, excellent chemical stability and semiconductor performance. Graphite alkynes have special electronic structures and natural pore characteristics, making the charge distribution extremely unbalanced, and are considered as non-candidates for excellent wave-absorbing materials. In order to further optimize the performance of graphite alkyne and expand its application range, researchers have begun to explore the way to modulate the electrical, magnetic and dielectric properties of materials by doping with heteroatoms (such as nitrogen, boron, sulfur, etc.). Nitrogen doped graphite alkyne (N-GY) materials have attracted considerable attention in recent years due to their unique electronic structure and controllable energy band characteristics. The introduction of nitrogen atoms not only can adjust the conductivity and dielectric constant of the gamma-GY, but also can enhance the multiple relaxation process of the material by introducing additional defect states and polarization centers. In addition, nitrogen doping can introduce more heterogeneous interfaces, so that more interface polarization is promoted, and the electromagnetic wave loss capacity of the material is further improved. Meanwhile, defects and empty bits formed in the doping process can bring magnetism to the graphite alkyne, so that the high dielectric property of the graphite alkyne is balanced, and the impedance matching property of the graphite alkyne is improved. Therefore, nitrogen doping provides a new idea for the design of high-performance electromagnetic wave absorbing materials. At present, through lit