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Method for preparing graphene energy storing material through electrochemical cathodic disbonding

A technology of cathodic stripping and energy storage materials, which is applied in the field of new materials, can solve the problems of high cost, reduce the conductivity of graphene materials, and oxidize the surface of graphene, and achieve the effects of low cost, easy industrialization and application, and easy control of the process

Active Publication Date: 2013-02-13
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although anodic oxidation can obtain graphene quickly, the anodic process easily causes the surface of graphene to be partially oxidized, making it contain some oxygen-containing functional groups and have certain structural defects, which greatly reduces the conductivity of graphene materials and limits its further application
Recently, Professor Loh et al. [J.Am.Chem.Soc.2011(133)8888] successfully synthesized multilayer graphene sheets by lithium ion intercalation and high-power ultrasound, with a yield of up to 70%, but the synthesis process takes a long time and requires Subsequent long-term high-power ultrasonic peeling, high-power ultrasonic is easy to chop graphene sheets, which limits the size of graphene
[0003] In summary, the current methods for preparing graphene have the following deficiencies: low yield, high cost, use of highly toxic chemical reagents, many oxygen-containing functional groups or more structural defects and other technical problems

Method used

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  • Method for preparing graphene energy storing material through electrochemical cathodic disbonding
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  • Method for preparing graphene energy storing material through electrochemical cathodic disbonding

Examples

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Effect test

Embodiment 1

[0027] Example 1: Preparation of graphene by exfoliating graphite rods in acetonitrile (AN) solution at cathode-10V

[0028] With Pt sheet as the anode and high-purity graphite rod as the cathode, in the acetonitrile solution of 0.5mol / L tetrabutyl ammonium hexafluorophosphate, constant voltage –10V, DC strong cathodic polarization for 2h, and then the product obtained from the cathode was Wash with water and ethanol for 5 times, disperse by ultrasonic (99W, 30kHz, 5h), centrifuge at a low speed of 1500 rpm, then centrifuge the obtained supernatant at a high speed of 13300 rpm, and finally dry the obtained solid product in vacuum at 40°C to obtain the product . TEM showed that graphite was exfoliated to form graphene material. A uniformly dispersed sol can be obtained by ultrasonically dispersing the dried product in N,N-dimethylformamide (DMF).

Embodiment 2

[0029] Example 2: Preparation of graphene by exfoliating graphite rods in N,N-dimethylformamide (DMF) solution at cathode-10V

[0030] With Pt sheet as anode and high-purity graphite rod as cathode, in DMF solution of 0.5mol / L tetrabutylammonium hexafluorophosphate, constant voltage -10V strong cathode polarization for 2h, and then the product obtained from the cathode was dehydrated with absolute ethanol Wash 5 times, ultrasonically (95W, 30kHz, 5h) disperse, centrifuge at a low speed of 1500 rpm, then centrifuge the obtained supernatant at a high speed of 13300 rpm, and finally vacuum dry the obtained solid product at 40°C to obtain the product. TEM showed that graphite was exfoliated to form graphene material.

Embodiment 3

[0031] Example 3: Preparation of graphene by exfoliating graphite rods in propylene carbonate (PC) solution at cathode-10V

[0032] With the Pt sheet as the anode and the high-purity graphite rod as the cathode, in a PC solution of 0.5mol / L tetrabutylammonium hexafluorophosphate, a constant voltage of -30V is strongly cathodically polarized for 0.5h, and then the product obtained from the cathode is anhydrous Wash with ethanol 5 times, disperse by ultrasonic (90W, 30kHz, 3h), centrifuge at low speed 1500 rpm, then centrifuge the obtained supernatant at high speed 13300 rpm, and finally vacuum dry the obtained solid product at 40°C to obtain the product. TEM showed that graphite was exfoliated to form graphene material.

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Abstract

The invention relates to the field of new materials, and in particular to a preparation method of graphene, which is the method for preparing a graphene energy storing material through electrochemical cathodic disbanding. The method comprises steps as follows: getting noble electrode as anode, high-purity graphite as cathode, a quaternary ammonium salt organic solvent as electrolyte, and voltage adjustable direct current power as the power supply; carrying out high cathodic disbanding under a constant voltage of -5 to -100V; inserting the solvated quaternary ammonium salt into laminated graphite under an effect of a high cathode voltage so as to generate expansion on a surface of the graphite electrode in a single layer or a plurality of layers; and decomposing the solvent to obtain gas under an electric potential effect of the high cathode, so as to further strip the graphite to obtain the graphene. The method is carried out under a direct current stabilized power supply without other special equipment; the method for preparing the graphene is simple, convenient and easy to carry, a process is easy to control, cost is low, no pollution is generated, and convenience is provided for industrial popularization and application; and prepared graphene can be widely applied to fields such as an energy storage field, an energy conversion field, an electronic device field and a biosensing field.

Description

technical field [0001] The invention relates to the field of new materials, in particular to a method for preparing graphene energy storage materials by electrochemical cathode stripping. Background technique [0002] Graphene is a single layer of carbon atoms through sp 2 Graphene is a new two-dimensional honeycomb carbon-based nanomaterial with a thickness of only 0.335nm that is hybridized and closely packed. Since its discovery in 2004, graphene has attracted widespread attention from the scientific and industrial circles. Graphene's unique two-dimensional structure makes it have excellent electrical properties, excellent chemical stability and thermodynamic stability, as well as physical and mechanical properties, and has been widely studied in sensor devices, optoelectronics, energy conversion and storage materials and apply. Especially graphene's high conductivity (64mS / cm) and high theoretical specific surface (2675m 2 / g), graphene has been considered as an ideal...

Claims

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Application Information

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IPC IPC(8): C01B31/04H01G11/86C01B32/19
Inventor 纪效波杨应昌宋维鑫朱裔荣陈启元李叙
Owner CENT SOUTH UNIV
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