Method for preparing graphene sheet

A technology of graphene sheet and graphite, which is applied in the field of graphene sheet preparation, can solve the problems that graphene cannot be prepared in batches, and achieve the effects of less structural defects, high efficiency, and good electrical and thermal conductivity

Active Publication Date: 2013-02-27
浙江东盛慧谷投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the deficiency that graphene cannot be prepared in batches in the prior art, the primary technical problem to be solved by the present invention is to provide a controllable method for preparing graphene sheets in batches

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Take a certain amount of expanded graphite and expand it in a muffle furnace at 400°C, and transfer the expanded graphite to ammonia water (NH 3 h 2 O) mechanically stirring in the solution for 30 minutes and then standing still for 5 hours, then vacuum suction filtration and washing with deionized water to neutrality, then transfer it to an ethanol solution for ultrasonic dispersion for 12 hours, then suction filtration and drying to obtain micro-nano graphene sheets;

[0045] (2) Transfer the dried micro-nano graphene sheets to oleum for 2 h, then filter and transfer to 5% by mass H 2 o 2 After soaking in the solution for 5h, filter and dry;

[0046] (3) Put the dried micro-nano graphene sheets into a constant temperature tank with a saturated ammonium carbonate solution at a constant temperature of 50°C, ultrasonically disperse for 45 minutes, then mechanically stir for 2 hours, then stand for 8 hours for suction filtration, and dry at low temperature to obtain...

Embodiment 2

[0049] (1) Take a certain amount of expanded graphite and expand it in a muffle furnace at 600°C, and transfer the expanded graphite to NH 3 h 2 O solution was mechanically stirred for 30 minutes and then stood still for 5 hours, then vacuum filtered and washed with deionized water until neutral, then transferred to an ethanol solution for ultrasonic dispersion for 10 hours, and then dried by suction to obtain micro-nano graphene sheets;

[0050] (2) Transfer the dried micro-nano graphene sheets to oleum for 4 hours, then filter and transfer to 5% by mass H 2 o 2 After 5h in solution, filter and dry;

[0051] (3) Put the dried micro-nano graphene sheet into a constant temperature tank filled with ethanol at a constant temperature of 50°C, ultrasonically disperse it for 45 minutes, then mechanically stir it for 2 hours, then let it sit for 6 hours, suction filter, and dry at low temperature to obtain the intercalated micro-nano Graphene sheets; transfer the intercalated nano...

Embodiment 3

[0054] (1) Take a certain amount of expanded graphite and expand it in a muffle furnace at 800°C, transfer the expanded graphite to NaOH solution and mechanically stir for 30 minutes, then stand still for 6 hours, then vacuum filter and wash with deionized water until neutral, It was then transferred to an ethanol solution for ultrasonic dispersion for 15 hours, and then dried by suction to obtain micro-nano graphene sheets;

[0055] (2) Transfer the dried graphite nanosheets to oleum and concentrated nitric acid (volume ratio 1:1) for immersion for 2 hours, then filter and transfer to 10 mass% H 2 o 2 After 5h in solution, filter and dry;

[0056] (3) Put the dried micro-nano graphene sheet into a constant temperature tank filled with ethyl acetate at a constant temperature of 60°C, ultrasonically disperse it for 60 minutes, then mechanically stir it for 2 hours, then let it sit for 8 hours, suction filter, and dry at low temperature to obtain the intercalated nanographene ...

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Abstract

The invention discloses a method for preparing a graphene sheet. The graphene sheet is prepared through the following steps: (1) expansible graphite is subjected to thermal expansion treatment so as to form wormlike graphite, the wormlike graphite is then soaked in alkaline solution, is subjected to suction filtration, is washed and then is put in the solvent to be subjected to ultrasonic dispersion, so that a micro-nano graphene sheet is obtained; (2) the micro-nano graphene sheet which is obtained in the step (1) is dispersed in inorganic strong protonic acid to be soaked, is subjected to suction filtration, is then transferred into H2O2 solution to be soaked and is subjected to suction filtrating, washing and drying; (3) the micro-nano graphene sheet which is treated through the step (2) is transferred into the solvent to be dispersed, is enabled to stand at constant temperature, and is then subjected to suction filtrating or drying to be secondarily expanded; and (4) the micro-nano graphene sheet which is treated in the step (3) is transferred into the solvent to be subjected to ultrasonic dispersion, is filtered, dried and transferred to a furnace in a reduction protective atmosphere and is subjected to high temperature deoxygenation reduction, so the graphene sheet is obtained. The method can be used for preparing the high quality pure graphene sheet in batches and is easy to popularize and apply.

Description

[0001] technical field [0002] The invention belongs to the field of carbon material preparation, in particular to a method for preparing graphene sheets. Background technique [0003] Graphene is a honeycomb with SP 2 The hybrid carbon material, as a single-layer carbon atom planar material, has a thickness of only 0.335nm, which is the thinnest known material and is very strong. Graphene has ultra-high conductivity and carrier properties, and can be widely used in electronic information technology; graphene has a large specific surface area up to 2630m 2 / g, such a high specific surface area makes graphene materials the first choice for energy storage, and it is very likely to be applied to hydrogen storage, supercapacitors or fuel cells. In 2004, Geim successfully prepared graphene by tape method and proved through experiments that it is a two-dimensional crystal material that can exist alone. This research result set off an upsurge in graphene research in recent year...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 吕树申符远翔王晓明莫冬传潘亚宏
Owner 浙江东盛慧谷投资发展有限公司
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