Electrochemical stripping method for preparing fluorine-doped graphene

A fluorine doping and electrochemical technology, applied in chemical instruments and methods, graphene, inorganic chemistry, etc., can solve problems such as unfavorable industrialization promotion, increase production cost, highly toxic fluorine-containing substances, etc., and achieve a wide range of applications, The effect of low cost and high product quality

Inactive Publication Date: 2018-12-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] These methods for synthesizing fluorine-doped graphene have a large amount of raw materials and high temperature, which increases the production cost; especially these fluorine-containing compounds themselves have great toxicity, or produce highly toxic fluorine-containing substances in the reaction process, which is not necessary. Conducive to industrialization promotion

Method used

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  • Electrochemical stripping method for preparing fluorine-doped graphene
  • Electrochemical stripping method for preparing fluorine-doped graphene
  • Electrochemical stripping method for preparing fluorine-doped graphene

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Add the aqueous solution of ammonium tetrafluoroborate (0.5mol / L) to the electrolytic cell, then connect the positive electrode of the DC power supply with graphite paper, and connect the negative electrode of the DC power supply with the glassy carbon electrode, so that the graphite electrode and the glassy carbon electrode are immersed in the area of ​​the electrolyte solution The ratio is 0.5, and the two electrodes are separated by 1 cm. A cell voltage of 10V was applied, peeled off at room temperature for 1 h, the reaction product was filtered and washed, and sonicated in water for 15 min to obtain a fluorine-doped graphene slurry, and the slurry was freeze-dried to obtain a fluorine-doped graphene powder. The powder diagram of the prepared fluorine-doped graphene is as follows figure 1 As shown in the figure, the powder is about 1.8g, indicating that the method can be scaled up to produce fluorine-doped graphene on a large scale; the scanning electron microscope p...

Embodiment 2

[0034] Add the aqueous solution of tetraethylammonium tetrafluoroborate (0.1mol / L) to the electrolytic cell, then connect the positive electrode of the DC power supply with a graphite rod, and connect the negative electrode of the DC power supply with a copper electrode, so that the graphite electrode and the copper electrode are immersed in the electrolyte The area ratio of the solution is 1, and the two electrodes are separated by 1 cm. A cell voltage of 15V was applied, peeled off at room temperature for 1.5h, the reaction product was filtered and washed, and ultrasonicated in water for 15min to obtain a slurry of fluorine-doped graphene, and the slurry was freeze-dried to obtain a powder of fluorine-doped graphene. According to the analysis and test, the size of the nanosheet is 1-30 μm, the fluorine content is 5%, and the specific capacity of the electrode material can reach 150F / g.

Embodiment 3

[0036] Add an aqueous solution of sodium tetrafluoroborate (0.1mol / L) to the electrolytic cell, then connect the positive electrode of the DC power supply with graphite paper, and connect the negative electrode of the DC power supply with a platinum sheet electrode, so that the graphite electrode and the platinum sheet electrode are immersed in the area of ​​the electrolyte solution. The ratio was 0.25, and the two electrodes were separated by 1 cm. A cell voltage of 10 V was applied, peeled off at room temperature for 30 min, the reaction product was filtered and washed, and sonicated in water for 15 min to obtain a slurry of fluorine-doped graphene. According to the analysis and test, the size of the nanosheet is 1-40 μm, the fluorine content is 0.1%, and the specific capacity of the electrode material can reach 120F / g.

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Abstract

The invention discloses an electrochemical stripping method for preparing fluorine-doped graphene, and belongs to the technical field of controllable preparation and doped control of graphene materials. According to the method, negative ion fluorine-containing soluble salt serves as stripping electrolyte, water or nitrile serves as a solvent, graphite serves as a raw material, and fluorine-doped graphene nano-sheets are prepared by the electrochemical stripping method in a one-step manner. The preparation method has the advantages that the method is green, environmentally friendly, simple in device, convenient to operate, mild in condition, low in cost, and a process is easily amplified. The prepared fluorine-doped grapheme is high in quality and good in performance and has an important application prospect in the fields such as super-capacitors, lithium batteries, lubrication, conductive ink and catalysis.

Description

technical field [0001] The invention belongs to the technical field of controllable preparation of graphene materials and doping control thereof, in particular to a method for preparing fluorine-doped graphene by electrochemical exfoliation. Background technique [0002] Graphene is a two-dimensional structural material with a single layer or a small number of layers (<10 layers) of carbon. Due to its atomic thickness, high electrical conductivity, excellent electrical properties, and excellent chemical and thermodynamic stability, graphene has important applications in nanoelectronics, new energy storage, catalysis, adsorption, and environmental protection. Prospects, and has become an international material science research hotspot. So far, a variety of methods for preparing graphene have been developed, such as: mechanical exfoliation; chemical vapor deposition; solvent exfoliation; oxidation-reduction and electrochemical exfoliation. Studies have demonstrated that d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19H01G11/36
CPCC01B2204/04C01B2204/22C01B2204/32C01P2004/01C01P2004/03C01P2004/04H01G11/36Y02E60/13
Inventor 吴忠帅周锋郑双好师晓宇肖涵
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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