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High-concentration organic saline solution-based method for preparing graphene through electrochemical intercalation

An organic salt and aqueous solution technology, which is applied in the field of electrochemical intercalation preparation of graphene based on high-concentration organic salt aqueous solution, can solve the problems of affecting the crystal structure of graphene, uncontrollable number of graphene layers, destruction of graphite electrodes, etc., and achieves the preparation cycle. Short, continuous controllable intercalation, low cost effect

Active Publication Date: 2019-10-11
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, traditional electrochemistry uses the ions in the electrolyte and the generated bubbles to achieve intercalation and exfoliation on the electrode. Therefore, the decomposition of the electrolyte intensifies as the intercalation and exfoliation progress, causing serious damage to the graphite electrode. Once the carbon paper is peeled off on the electrode and enters the solution, the intercalation and stripping process stops. If the intercalation is not well realized before the peeling, it will cause the problem that the number of graphene layers prepared is uncontrollable, and due to the intercalation ions and The oxidation reaction between graphite will further affect the crystal structure of graphene

Method used

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  • High-concentration organic saline solution-based method for preparing graphene through electrochemical intercalation
  • High-concentration organic saline solution-based method for preparing graphene through electrochemical intercalation
  • High-concentration organic saline solution-based method for preparing graphene through electrochemical intercalation

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Effect test

Embodiment 1

[0038] Using lithium bistrifluoromethanesulfonylimide as the electrolyte, weigh 18.09g of lithium bistrifluoromethanesulfonylimide, add 3g of water (the mass concentration of the organic salt is 85.8%), place the solution in an oven at 50°C for 30min, and wait for The solution is clear and transparent as electrolyte for electrochemical intercalation of graphite. Add the prepared electrolyte solution into the electrolytic cell, choose graphite paper as the anode and connect it to the DC power supply, and use the platinum sheet as the cathode to connect it to the DC power supply. The distance between the two electrodes is 5cm, apply a voltage of 20V, and intercalate and expand at 25°C The electrode can last for 3 hours without peeling off, and graphene aggregates are obtained, and the actual picture is as follows figure 1 As shown, after vacuum filtration and cleaning, the graphene dispersion was obtained by dispersing in an 80W ultrasonic cleaning machine for 30 minutes, and th...

Embodiment 2

[0041] Using lithium bistrifluoromethanesulfonimide as the electrolyte, weigh 5 mL of lithium bistrifluoromethanesulfonimide and add 1 mL of water (the volume concentration of the organic salt is 83.3%), and place the solution in an oven at 50°C for 30 minutes, and wait for The solution is clear and transparent as a high-concentration brine electrolyte for electrochemical intercalation of graphite. Add the prepared electrolyte in the electrolytic cell, choose graphite paper as the anode and connect it to the DC power supply, and use platinum wire as the cathode to connect it to the DC power supply. The distance between the two electrodes is 8cm, apply a voltage of 15V, and intercalate and expand at 10°C The electrode does not peel off for 1 hour, and graphene aggregates are obtained. After vacuum filtration and cleaning, disperse in a 100W ultrasonic cleaner for 1 hour to obtain a graphene dispersion. Graphene powder.

[0042] Gained graphene powder is carried out X-ray diffr...

Embodiment 3

[0044] Sodium trifluoromethanesulfonate (NaCF 3 SO 3 ) as electrolyte, weigh 4gNaCF 3 SO 3 Add 1 g of water (the mass concentration of organic salt is 80%) and place the solution in an oven at 50° C. for 30 minutes until the solution is clear and transparent as a high-concentration brine electrolyte for electrochemical intercalation of graphite. Add the prepared electrolyte in the electrolytic cell, choose graphite paper as the anode and connect it to the DC power supply, and use silver wire as the cathode to connect it to the DC power supply. The distance between the two electrodes is 1cm, and a voltage of 5V is applied to expand the intercalation at 35°C. The electrode can last for 2 hours without peeling off, and graphene aggregates are obtained. After vacuum filtration and cleaning, they are dispersed in a 120W ultrasonic cleaner for 30 minutes to obtain a graphene dispersion. Graphene powder.

[0045] Scanning electron microscope analysis and X-ray diffraction analysi...

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Abstract

The invention provides a high-concentration organic saline solution-based method for preparing graphene through electrochemical intercalation, and belongs to the technical field of graphene preparation. In the preparation method, a high-concentration organic saline solution is used as an electrolyte, graphite is used as an anode, an inert conductive precious metal material is used as a cathode, and an electrochemical intercalation reaction is carried out to obtain graphene aggregates. By using the high-concentration organic saline solution as the electrolyte, quick decomposition of water can be inhibited, and continuous controllable intercalation of the graphite can be achieved. Fluorine-containing macromolecular organic salt is adopted in the method, under the action of voltage, the organic salt still has a stable structure, in the electrochemical intercalation reaction, the chemical reaction of intercalation ions and the graphite can be effectively avoided, the crystal structure of the graphite is protected from being damaged, and therefore, the high-quality graphene is prepared. The preparation method is short in preparation period, low in cost, environmentally friendly and simple, no acid liquid is generated, and massive industrial production is easily achieved.

Description

technical field [0001] The invention relates to the technical field of graphene preparation, in particular to a method for preparing graphene based on high-concentration organic salt solution electrochemical intercalation. Background technique [0002] Since the concept of graphene was proposed by the research team led by A.K.Geim of the University of Manchester in 2004, graphene, as another bright star in the carbon family, has been highly valued by physics, chemistry and materials scientists. [0003] So far, researchers at home and abroad have conducted extensive research on the preparation of graphene. Among them, the technology of electrochemical exfoliation and intercalation to prepare graphene has received more attention because of its cheap cost and simple operation. However, traditional electrochemistry uses the ions in the electrolyte and the generated bubbles to achieve intercalation and exfoliation on the electrode. Therefore, the decomposition of the electrolyte...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01B32/19
Inventor 阎兴斌杨娟王正军
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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