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Method for synthesizing graphene

A graphene and halogenated hydrocarbon technology, applied in the field of chemical synthesis, can solve the problems of complex operation, low controllability, difficult to mass-produce, etc., and achieve the effects of high purity, avoidance of damage, and complete flakes

Active Publication Date: 2011-01-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has strict requirements on equipment, complicated operation, low controllability, and difficulty in large-scale production, so it is only suitable for laboratory research

Method used

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  • Method for synthesizing graphene
  • Method for synthesizing graphene
  • Method for synthesizing graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 18.6g of ferrocene and 18.1g of 1,2,4-trichlorobenzene in a molar ratio of 1:1, add them into a high temperature and high pressure reactor and stir evenly. After sealing, raise the temperature to 500°C under nitrogen atmosphere, and keep it warm for 0.1h. The resulting product was washed repeatedly with acetone to remove unreacted ferrocene and generated amorphous carbon and other small molecular substances. Then wash repeatedly with 0.5mol / l dilute hydrochloric acid to remove residual metal and metal chloride impurities, and finally wash with deionized water until the filtrate is neutral, and dry in a common oven at 100°C to obtain graphene.

[0020] as attached figure 1 As shown by transmission electron microscopy (TEM), the prepared graphene is in the form of sheets with a length of 1-2 μm. as attached figure 2 As shown by a scanning electron microscope (SEM), the thickness of the prepared graphene is 3-5 nm.

Embodiment 2

[0022] Weigh 1.9 g of cobaltocene and 15.4 g of carbon tetrachloride in a molar ratio of 0.1:1, add them into a high-temperature and high-pressure reactor and stir evenly. After sealing, raise the temperature to 460°C in an argon atmosphere and keep it warm for 2 hours. The resulting product was washed repeatedly with absolute ethanol to remove unreacted cobaltocene and generated amorphous carbon and other small molecular substances. Then wash repeatedly with 0.1mol / l dilute sulfuric acid to remove residual metal and metal chloride impurities, and finally wash with deionized water until the filtrate is neutral, and dry in a common oven at 100°C to obtain graphene.

Embodiment 3

[0024] 18.9 g of nickelocene and 3.4 g of tetrabromoethylene were weighed in a molar ratio of 10:1, added to a high-temperature and high-pressure reactor and stirred evenly. After sealing, the temperature was raised to 520° C. under a nitrogen atmosphere, and the temperature was kept for 4 hours to obtain graphene. The generated graphene was washed repeatedly with pyridine to remove small molecular substances such as unreacted nickelocene and generated amorphous carbon. Then wash it repeatedly with 0.3mol / l dilute nitric acid to remove residual metal and metal chloride impurities, and finally wash it with deionized water until the filtrate is neutral, and dry it in a common oven at 100°C.

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Abstract

The invention discloses a new method for quickly preparing graphene. A metal catalyst and a halogenated hydrocarbon are used as raw materials; and after the raw materials are reacted in a high-temperature and high-pressure reaction kettle under the inert atmosphere, the reaction product is purified to obtain the graphene. The method has the advantages of simple process flow and low reaction equipment requirement; and the prepared graphene has low layer number and is of large and complete sheet. The method provides a new path for large-scale application of the graphene in industrialized products such as lithium batteries, capacitors and the like.

Description

technical field [0001] The invention relates to graphene, in particular to a preparation method of graphene, and belongs to the technical field of chemical synthesis. Background technique [0002] Graphene is a single-layer or multi-layer two-dimensional carbon atom crystal, which exhibits superior performance in electricity, heat and mechanics, and is expected to be used in high-performance electronic devices, composite materials, field emission materials, gas sensors and energy storage, etc. field has been widely applied. At the same time, the scientific community believes that graphene is very likely to replace silicon and become a future semiconductor material, so it has very broad application prospects (Li, X.L.; Wang, X.R.; Zhang, L.; Lee, S.W.; Dai, H.J. Chemically Derived, Ultrasmooth Graphene Nanoribbon Semiconductors. Science 2008, 319, 1229-1232.). [0003] The preparation method of graphene mainly contains following several at present: One, graphite oxide-reduc...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 宋怀河刘庆华陈晓红
Owner BEIJING UNIV OF CHEM TECH
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