A ball mill auxiliary co 2 Method for preparing oligolayer graphene by intercalation

Abstract

The invention discloses a method for preparing single-layer graphene through CO2 intercalation assisted by ball milling. The method includes the steps that ball milling balls and graphite are added into a ball milling tank; the ball milling tank is fixed to a planetary ball mill for ball milling, and a ball milling sample is obtained; the ball milling sample is transferred into a high-temperature-resistant loading vessel and conveyed into a CVD tubular furnace protected by atmosphere to be sealed and vacuumized, and then CO2 gas is continuously introduced; heating is conducted to obtain an intercalation sample; the intercalation sample is dissolved in deionized water to be subjected to ultrasonic stripping for 0.5-2 h, a single-layer graphene solution is obtained, the single-layer graphene solution is vacuumized, dried and ground, and single-layer graphene powder is obtained. The microstructure and the stacking state of graphite are modified through mechanical ball milling so that the intercalation effect can be improved, CO2 is selected as an intercalation agent, energy conservation and environment friendliness are achieved, the CO2 gas will not be left in the graphene solution in the stripping process, introduction of impurities is avoided, the quality of graphene is improved, the complex cleaning process is omitted, and the preparation period is shortened.

Description

technical field [0001] The invention relates to a preparation method of graphene, in particular to a ball milling assisted CO 2 A method for preparing oligolayer graphene by intercalation. Background technique [0002] Due to its special electrical, optical, mechanical and thermal properties, graphene has good application potential in the fields of conductive materials, supercapacitors, conductive displays, conductive ink additives, sensors, biomedicine, and extraction. Since the first preparation of graphene, researchers have made great progress in the field of its preparation. At present, the preparation methods of graphene mainly include mechanical exfoliation method, CVD method, redox method, liquid phase or gas phase intercalation exfoliation method, thermal expansion method, crystal epitaxial growth method, arc discharge method, etc. Among them, the oxidation-reduction method has become one of the current methods for large-scale preparation of graphene due to its adv...

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Problems solved by technology

Although this method is low in cost, simple in process, and high in yield, it has a long reaction cycle and harsh reaction conditions, and the intercalation agent interhalogen compound (such as iodine chloride) used is corrosive, highly toxic, and highly irritating. , which forms iodine pentoxide when exposed to air, reacts with water or steam to release heat and produces toxic corrosive gas, and decomposes to produce highly toxic fumes when exposed to high heat, so it is not friendly to the environment and has serious safety hazards question

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