Method for preparing graphene material by microwave irradiation in vacuum or inert gas environment

A technology of microwave irradiation and inert gas, applied in the direction of graphene, nanotechnology for materials and surface science, chemical instruments and methods, etc., can solve the problems of graphene being easy to burn, low final yield, and causing fire hazards , to achieve simple equipment, increase productivity, and avoid burning effects

Inactive Publication Date: 2011-08-03
无锡第六元素高科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ordinary microwave irradiation is carried out in the air, and the graphene obtained by first reduction is very easy to burn and even cause fire under microwave irradiation,

Method used

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  • Method for preparing graphene material by microwave irradiation in vacuum or inert gas environment
  • Method for preparing graphene material by microwave irradiation in vacuum or inert gas environment
  • Method for preparing graphene material by microwave irradiation in vacuum or inert gas environment

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment one: the present invention prepares the method for graphene material with microwave irradiation in vacuum or inert gas environment, comprises following preparation steps:

[0044] 1. Microwave irradiation steps: take 0.5g of graphite oxide particles (particle size 1-300mm) and place them in the vacuum chamber 6 of the microwave chamber 3, close the vacuum chamber top cover 4; close the first valve 1, and open the second valve 2 ;

[0045] 2. Turn on the mechanical pump 5 to pump the air pressure in the vacuum chamber 6 to the limit (4~8×10 -2 Torr);

[0046] 3. Close the second valve 2 and open the first valve 1; inject 99.999% nitrogen into the vacuum chamber 6 until the air pressure is higher than 100 Torr;

[0047] 4. Close the first valve 1, open the second valve 2, and pump the air pressure of the vacuum chamber 6 to the limit (4~8×10 -2 Torr);

[0048] 5. Repeat steps (3) and (4) twice to drive out the residual oxygen in the vacuum chamber;

[0049] ...

Embodiment 2

[0052] Embodiment two: the present invention prepares the method for graphene material with microwave irradiation in vacuum or inert gas environment, comprises following preparation steps:

[0053] 1. Microwave irradiation step: take 10g of graphite oxide particles (1-300 mm in diameter) and place them in the vacuum chamber 6 of the microwave chamber 3, close the vacuum chamber top cover 4; close the first valve 1, and open the second valve 2;

[0054] 2. Turn on the mechanical pump 5 to pump the air pressure in the vacuum chamber 6 to the limit (4~8×10 -2 Torr);

[0055] 3. Close the second valve 2 and open the first valve 1; inject 99.999% nitrogen into the vacuum chamber 6 until the air pressure is higher than 100 Torr;

[0056] 4. Close the first valve 1, open the second valve 2, and pump the air pressure of the vacuum chamber 6 to the limit (4~8×10 -2 Torr);

[0057] 5. Repeat steps (3) and (4) twice to drive out the residual oxygen in the vacuum chamber;

[0058] 6. ...

Embodiment 3

[0061] Embodiment three: the present invention prepares the method for graphene material with microwave irradiation in vacuum or inert gas environment, comprises following preparation steps:

[0062] 1. Microwave irradiation step: get 1000g of graphite oxide particles (1-300 mm in diameter) and place them in the vacuum chamber 6 of the microwave chamber 3, close the vacuum chamber top cover 4; close the first valve 1, and open the second valve 2;

[0063] 2. Turn on the mechanical pump 5 to pump the air pressure in the vacuum chamber 6 to the limit (4~8×10 -2 Torr);

[0064] 3. Close the second valve 2 and open the first valve 1; inject 99.999% nitrogen into the vacuum chamber 6 until the air pressure is higher than 100 Torr;

[0065] 4. Close the first valve 1, open the second valve 2, and pump the air pressure of the vacuum chamber 6 to the limit (4~8×10 -2 Torr);

[0066] 5. Repeat steps (3) and (4) twice to drive out the residual oxygen in the vacuum chamber;

[0067] ...

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Abstract

The invention relates to a method for preparing graphene material by microwave irradiation in a vacuum or inert gas environment. The method comprises the following steps: taking dry graphite particles to be placed in a vacuum cavity of a microwave chamber and closing a top cap of the vacuum cavity; pumping the air pressure in the vacuum cavity to be in an ultimate vacuum state; injecting gas into the vacuum cavity till driving residue oxygen in the vacuum cavity; starting the microwave irritation till the oxidation graphite explodes and breaks; closing the microwave irritation and filling the air pressure in the vacuum cavity to be in an atmosphere state; opening the top cap of the vacuum cavity and collecting the exploded and reduced oxidized graphite powder. The method has the advantages that the heating is concentrated due to microwave and the power is high; graphite is heated and oxidized in short time so that the oxidized graphite is heated and reduced instantly and rapidly expands to release a large quantity of gas; the vacuum cavity can effectively isolate the contact between oxygen and graphene so as to avoid the combustion of graphene in the high temperature reduction process, thereby increasing the reduction yield.

Description

technical field [0001] The invention relates to a method for preparing graphene materials by microwave irradiation in a vacuum or an inert gas environment, and the obtained products can be applied to multiple technical fields, including energy storage and coating materials. Specifically, the invention is a process for preparing graphene materials with high specific surface area and high conductivity. Background technique [0002] Graphene, English name Graphene, is a two-dimensional lattice structure in which carbon atoms are arranged in a hexagonal manner. As a single-layer carbon-atom planar material, graphene can be obtained by exfoliating graphite materials. Graphene has become the focus of scientific and industrial attention since the graphite crystal film 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 among known materials, but also very firm and hard; as a simpl...

Claims

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Application Information

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IPC IPC(8): C01B31/04
CPCC01B2204/32C01B31/0476C01B31/04B82Y40/00B82Y30/00C01B32/192
Inventor 瞿研
Owner 无锡第六元素高科技发展有限公司
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