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A kind of method for preparing graphene by high-pressure reduction

A graphene and high-pressure technology, applied in the field of graphene material preparation, can solve the problems of many graphene defects, violent explosion process, uncontrollable product loss, etc., and achieve the effect of simple preparation process, simple operation and short reduction time

Active Publication Date: 2016-01-13
THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The explosion process of this method is relatively violent, the product loss is uncontrollable, and the obtained graphene has many defects.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Take the graphite oxide prepared by the Hummers method, and obtain graphene oxide powder after microwave peeling; then weigh 500 mg of graphene oxide powder and place it in a spark plasma sintering furnace. -4 Under the vacuum condition of Pa, argon gas was introduced as protective gas, pressurized to 10MPa, calcined at 2000℃ for 10 minutes, and cooled to room temperature naturally after heating. The conductivity of the obtained graphene material after reduction was 185 S / m.

[0042] Before reduction, the atomic ratio of carbon and oxygen (carbon-to-oxygen atomic ratio C / O) in graphene oxide was only 4.28. After reduction, the C / O was increased to 9.27 due to the removal of a large number of oxygen-containing functional groups. The C / O of graphene is 6.2.

Embodiment 2

[0044] First, graphite oxide was prepared according to the Staudenmaier method, and graphene oxide powder was obtained after thermal expansion and exfoliation, and 500 mg was weighed and placed in a high-temperature calcining furnace. in 6×10 -4 Under the vacuum condition of Pa, nitrogen was introduced as protective gas, pressurized to 20MPa, calcined at a high temperature of 1500 ° C for 6 minutes, and naturally cooled to room temperature after heating. The conductivity of the obtained graphene material after reduction is 205S / m. Before reduction, the atomic ratio of carbon and oxygen in graphene oxide (the ratio of carbon to oxygen atoms, C / O) is low, only 5.10. After reduction, due to the removal of a large number of oxygen-containing functional groups, the C / O was increased to 13.97, which was superior to the graphene prepared by chemical reduction with hydrazine hydrate.

Embodiment 3

[0046] First, graphite oxide was prepared according to the Brodie method, and graphene oxide powder was obtained after ultrasonic and thermal reduction, and then 500 mg of the graphene oxide powder was weighed and placed in a high-temperature calcining furnace. in 6×10 -4 Under the vacuum condition of Pa, pass helium gas as protective gas, pressurize to 40MPa, calcinate at a high temperature of 1200℃ for 3 minutes, and naturally cool down to room temperature after heating. The conductivity of the obtained graphene material after reduction is 278 S / m. Before reduction, the atomic ratio of carbon element and oxygen element (the ratio of carbon to oxygen atom to C / O) in graphene oxide is lower, which is only 6.34. After reduction, due to the removal of a large number of oxygen-containing functional groups, the C / O is increased to 37.4, which is superior to the graphene prepared by chemical reduction with hydrazine hydrate.

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Abstract

The invention relates to a method for preparing graphene by virtue of high-pressure reduction. In the method, high-temperature high-pressure reduction processing is performed on graphene oxide in an inert atmosphere so as to completely remove the oxygen-containing functional groups in graphene oxide, and the structural defects of graphene are repaired at the same time, so as to obtain high-quality graphene. The method can be used for avoiding the excessive use of chemical reagents, brings less pollution to environment and can be applied to the reduction of various powder of graphene oxide prepared by various methods.

Description

technical field [0001] The invention relates to the field of graphene material preparation, and more particularly, to a process for reducing graphene oxide to high-quality graphene through a process of high-pressure thermal reduction. Background technique [0002] Graphene, the English name Graphene, has become the focus of scientific and industrial attention since it was discovered by scientists at the University of Manchester in 2004. The thickness of graphene is only 0.335 nanometers, which is not only the thinnest one of the known materials, but also very strong and hard; as a simple substance, it transfers electrons faster than all known conductors and semiconductors at room temperature (graphene Electrons move at 1 / 300 the speed of light). Due to graphene's special atomic structure, the behavior of carriers (electrons and holes) in it must be described by Relativistic Quantum Mechanics. Specifically, graphene is a two-dimensional material with a single atomic layer, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 刘琼馨瞿研孙丹萍
Owner THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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