Method for preparing graphene powder at large scale
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A large-scale preparation and graphene powder technology, applied in the direction of graphene, nano-carbon, etc., can solve problems such as difficult to achieve large-scale preparation, and achieve the effect of high yield, less powder defects, and simple equipment
Inactive Publication Date: 2013-08-21
SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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[0005] Chinese invention patent CN 101139090A published "A Method for Preparation of Two-Dimensional Single-layer Graphe
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Embodiment 1
[0038] (1) Weigh 3g of graphite, add 20g of concentrated nitric acid (67wt%) and 1.6g of hydrogen peroxide (30wt%), stir for 9 hours to obtain a uniform suspension;
[0039] (2) Place the suspension in an ultrasonic cell disruptor (800W) for 60 minutes, and continuously inject He gas at a rate of 0.1 L / min;
[0040] (3) After the ultrasound and aeration, vacuum filter, and wash the filter residue 3 times with deionized water to make it neutral, and then dry the filter residue in an oven at 60°C for 8 hours to obtain a dry graphite intercalation compound;
[0041] (4) Place in a microwave muffle furnace and calcinate at 400°C for 60 seconds;
[0042] (5) Add it to 610g of N-methylpyrrolidone to obtain a dispersion, sonicate in an ultrasonic cell disruptor (1200w) for 60mim, and continuously feed it at a rate of 0.1L / min per liter of N-methylpyrrolidone while ultrasonically breath;
[0043] (6) Centrifuge the above dispersion in a centrifuge at 600 rpm for 30 minutes, remove t...
Embodiment 2
[0051] The operation of this example is the same as that of Example 1, except that the stirring time of graphite in concentrated nitric acid and hydrogen peroxide in step (1) is 3 hours, and the solvent used for dispersing ultrasound in step (5) is changed to N,N-di Methylformamide, the obtained graphene performance is similar to that of Example 1, and has the advantages of few layers, few defects, and high electrical conductivity.
Embodiment 3
[0053]The operation of this example is the same as that of Example 1, except that in step (2) the power of ultrasonic treatment is set to 1200W, and the ultrasonic treatment is 30min; Consumption 150g, ethanol consumption 150g; The performance of prepared graphene is similar to that of Example 1, and has advantages such as few layers, few defects, and high electrical conductivity.
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Abstract
The invention relates to a method for preparing high-quality graphene powder at low cost and large scale. The method comprises the following steps of: adding graphite to mixed solution containing an oxidizing agent and an intercalator, stirring evenly and then performing ultrasonic treatment, and simultaneously, continuously introducing He to form a graphite intercalation compound intercalated with the intercalator and He gas molecules; next, filtering, washing and drying, and performing thermal treatment in air to realize the first time of stripping of the graphite intercalation compound; later, dispersing the graphite intercalation compound in an organic solvent and performing ultrasonic treatment again under the condition of continuously introducing He; and then centrifuging and removing precipitate, and filtering, washing and drying the solution of the upper layer, thereby obtaining the graphene powder. The method provided by the invention is safe and environment-friendly, simple to operate and suitable for large-scale production; the prepared graphene has few defects and good electrical conductivity.
Description
technical field [0001] The invention relates to a method for preparing graphene powder on a large scale, and belongs to the technical field of new inorganic materials. Background technique [0002] In 2004, Andre K. Geim of the University of Manchester in the United Kingdom prepared graphene materials. Since then, graphene has attracted widespread attention for its unique structure and photoelectric properties. Graphene is a carbon atom with sp 2 A carbon material with a single-layer two-dimensional honeycomb lattice structure formed by hybrid orbital bonding and a six-membered ring structure. The structure of a material determines its performance. The unique structure of graphene brings it unique properties, such as extremely high electron mobility, the highest mechanical strength known to date, and extremely high Thermal conductivity and large specific surface area, these excellent properties determine the application of graphene in many fields, such as lithium-ion batt...
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IPC IPC(8): C01B31/04C01B32/19
Inventor 丁古巧徐传艳李修兵孙静徐旭光谢晓明江绵恒
Owner SHANGHAI INST OF MICROSYSTEM & INFORMATION TECH CHINESE ACAD OF SCI
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