Two-dimensional gamma-graphdiyne powder and preparation method thereof

A powder and single alkyne technology, applied in the field of two-dimensional carbon material semiconductor, can solve the problems of weak controllability, high energy consumption, and high power requirements in the experimental process, and achieves low toxicity, low energy consumption, and easy application. Effect

Inactive Publication Date: 2021-02-26
NORTHWEST UNIV(CN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its own preparation characteristics, the ball milling method has weak controllability and high energy consumption in the experimental process; the ultrasonic irradiation method has high requirements for the power of the experimental equipment, which limits the industrial application of this method to a certain extent

Method used

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  • Two-dimensional gamma-graphdiyne powder and preparation method thereof
  • Two-dimensional gamma-graphdiyne powder and preparation method thereof
  • Two-dimensional gamma-graphdiyne powder and preparation method thereof

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preparation example Construction

[0030] This embodiment provides a kind of preparation method of γ-graphite monoyne powder, and concrete steps are:

[0031] (1) After the calcium carbide is crushed and ground, use a ball mill to perform ball milling on the initially crushed calcium carbide and hexabromobenzene for a short period of time to refine the particle size, and the ball milling time is 0.5h to 1.5h;

[0032] (2) After ball milling, calcium carbide and hexabromobenzene are mixed with a solvent to make a slurry, the mouth of the slurry container is sealed, and stirred at a constant temperature at a temperature of 75°C to 85°C to make the slurry coupling reaction, and after the reaction is completed, the slurry is dried;

[0033] (3) Anneal the powder obtained by drying in a tube furnace under an argon or nitrogen atmosphere at an annealing temperature of 300°C to 700°C to volatilize residual hexabromobenzene;

[0034] (4) powder after annealing, carry out dilute acid washing, deionized water washing and...

Embodiment 1

[0043] Prepare hexabromobenzene and calcium carbide at a molar ratio of 1:5.75. After crushing and grinding 4g of calcium carbide, add 14mL of absolute ethanol for 1h ball milling; add 6g of hexabromobenzene and 14mL of absolute ethanol for 1h ball milling; After the slurry is mixed, add absolute ethanol to 150mL, stir evenly at room temperature, and stir at a constant temperature of 80°C for 28h. The mixed slurry was dried at 70°C; the dried powder was annealed in a tube furnace at 400°C for 2 hours in an argon atmosphere; after annealing, the powder was washed with dilute nitric acid, deionized water, and absolute ethanol in sequence; After drying at 70°C, black fluffy γ-graphyne powder was obtained without further treatment. The final sample is as follows: figure 1 Photos shown.

[0044] figure 2 For the SEM photo of the black fluffy γ-graphite monoyne powder obtained in Example 1, it can be seen that the sample is stacked by many flakes and has a large specific surface ...

Embodiment 2

[0046] Prepare hexabromobenzene and calcium carbide according to the molar ratio of 1:12, crush and grind 2.91g of calcium carbide, add 20mL of absolute ethanol for 1h ball milling; add 2.09g of hexabromobenzene, add 20mL of absolute ethanol for 1h ball milling; After mixing the slurry obtained by ball milling, add absolute ethanol to 150mL, stir evenly at room temperature, and stir at a constant temperature of 80°C for 23h. The final mixed slurry was dried at 70°C; the dried powder was annealed in a tube furnace at 400°C for 2 hours in a nitrogen atmosphere; after annealing, the powder was washed with dilute nitric acid, deionized water, and absolute ethanol in sequence; After drying at 70°C, black fluffy γ-graphyne powder was obtained without further treatment.

[0047] Figure 7 For the black fluffy γ-graphite monoyne powder SEM photograph that embodiment 2 obtains, it can be seen that the sample is stacked by many flakes and has a large specific surface area; Figure 8 I...

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Abstract

The invention discloses a preparation method of gamma-graphdiyne powder. The preparation method comprises the following steps: using hexabromobenzene and calcium carbide powder in a molar ratio of 1:(3-18) as reaction precursors, mixing the reaction precursors with absolute ethyl alcohol to prepare slurry; sealing the opening of a slurry container, and stirring for 23-28 hours at a constant temperature of 75-85 DEG C so that the precursor in the slurry is subjected to a coupling reaction; and after the reaction is finished, removing impurities through annealing and washing to obtain high-purity fluffy gamma-graphdiyne powder. According to the preparation method of the gamma-graphdiyne powder, the experimental process is more transparent and controllable, the requirement for preparation instruments is low, energy consumption in preparation is low, most of preparation processes can be conducted in the normal-temperature and normal-pressure air atmosphere, the preparation toxic and sideeffects are small, the operation environment is good, and the preparation method can be applied and popularized to industrial production and preparation of the gamma-graphdiyne powder.

Description

technical field [0001] The invention belongs to the field of two-dimensional carbon material semiconductors, and in particular relates to a preparation method of γ-graphite monoyne powder. Background technique [0002] Graphyne is a new all-carbon nanostructure material following fullerene, carbon nanotubes, and graphene. In 1968, the famous theorist Baughman confirmed the existence of the graphyne structure through theoretical calculations. Graphdiyne has rich carbon chemical bonds, large conjugated system, wide interplanar spacing, and excellent chemical stability. It is known as the most stable allotrope of synthetic diacetylene carbon. Due to its special electronic structure and semiconductor properties similar to silicon, graphdiyne is expected to be widely used in the fields of electronics, semiconductors and new energy. Scientists also predict that it will have an extraordinary impact in the field of new energy. [0003] Graphdiyne contains sp 2 A new type of carbo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/205
CPCC01B32/205
Inventor 贠江妮满振武杨锦杨燕伟庞俊坤刘竹青闫军锋赵武张志勇
Owner NORTHWEST UNIV(CN)
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