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

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Problems solved by technology

This method has strict requirements on equipment, complicated operation, low controllabilit

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

Example Embodiment

[0018] Example 1

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

[0020] As attached figure 1 Transmission electron microscopy (TEM) shows that the prepared graphene is sheet-like with a length of 1 to 2 μm. As attached figure 2 Scanning electron microscope (SEM) shows that the thickness of the prepared graphene is 3 to 5 nm.

Example Embodiment

[0021] Example 2

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

Example Embodiment

[0023] Example 3

[0024] Weigh 18.9 g of nickelocene and 3.4 g of tetrabromoethylene at a molar ratio of 10:1, add them to the high temperature and high pressure reactor and stir them evenly. After sealing, the temperature was raised to 520°C in a nitrogen atmosphere and kept for 4 hours to obtain graphene. The generated graphene is repeatedly washed with pyridine to remove the unreacted nickelocene and the generated amorphous carbon and other small molecules. Then it is washed repeatedly with 0.3mol / l dilute nitric acid to remove residual metal and metal chloride impurities, and finally washed with deionized water until the filtrate is neutral, and dried 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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