Preparation method of fewer-layer graphene

A few-layer graphene and graphite technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., to achieve the effects of high yield, simple operation, and easy mass production

Active Publication Date: 2012-07-18
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved in the present invention is to provide a preparation method of few-layer graphene for the deficiencies in the above-mentioned graphene preparation technology. The method is simple to operate, less time-consuming, low in cost, high in graphene yield, and easy to realize industrialization Large-scale production, the graphene prepared by this method has the advantages of less defects, less oxygen-containing groups, and high electrical conductivity

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  • Preparation method of fewer-layer graphene

Examples

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Embodiment 1

[0036] Add 2.08g of graphite powder to 300ml of aqueous solution containing 0.8g of tetraethylammonium tetrafluoroborate, 0.15g of sodium hydroxide and 50mg of thionine. After stirring evenly, place the suspension in an 855W ultrasonic cell disruptor Ultrasonic 6h. After the sonication, vacuum filter with a nylon microporous membrane, and wash the filter residue 3 times with 100ml of deionized water and 100ml of absolute ethanol, respectively, to remove residual substances. Then the filter residue was transferred to a watch glass, and vacuum-dried at 60° C. for 2 h to obtain dry graphite powder. Afterwards, place the dried graphite powder in a 900W microwave oven for 5 minutes of irradiation, add it to 700ml of N-methylpyrrolidone, and ultrasonicate it in a 250W ultrasonic cleaner for 12 hours. Then, the ultrasonically treated solution was transferred to a centrifuge tube, centrifuged at a speed of 5000 rpm for 10 minutes, and the upper layer solution was taken out to obtain ...

Embodiment 2

[0047] In this example, the graphite powder is first subjected to electrochemical pretreatment, and then the graphene is prepared in the same manner as in Example 1. The specific process is as follows:

[0048] Take 12g of graphite powder and press it into a rod shape, immerse in a mixed solution of 20ml dimethyl sulfoxide and 60ml water containing 0.8gNaCl as the cathode, and another graphite rod as the anode. Put a voltage of 5V on the two electrodes, and after 18 hours of reaction, the electrolyte is vacuum-filtered with a microporous membrane, and the graphite powder obtained by washing and filtering with 100ml of deionized water and 100ml of ethanol is collected for 3 times, and then the graphite powder is collected. Dry at 60°C for 2h.

[0049] The graphite powder prepared above was observed with a scanning electron microscope, and the results are shown in Figure 1. From Figure 1, it can be seen that the edges of the graphite particles have been peeled off, and the inte...

Embodiment 3

[0054] This example and Example 1 adopt basically the same method to prepare graphene, the difference is that 0.8g tetraethylammonium tetrafluoroborate and 0.15g sodium hydroxide are replaced by 0.54g tetraethylammonium hydroxide. Equally, can obtain the graphene dispersion liquid similar to that shown in Fig. 1 (a), its graphene yield is substantially identical with embodiment 1. Like Example 1, the dispersion was stable. Similar to Example 1, the graphene prepared by using the dispersion liquid has the advantages of few layers, few defects, few oxygen-containing groups, and high electrical conductivity.

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Abstract

The invention discloses a preparation method of fewer-layer graphene, which comprises the following steps of: putting graphite into solution containing a tetraalkyl-substituted quaternary ammonium cation and OH- for ultrasonic treatment in combination with a liquid phase intercalation technology and a microwave irradiation technology, so that the tetraalkyl-substituted quaternary ammonium cation is inserted into the middle of a graphite layer to form an intercalation layer, and the spacing of the graphite layer is increased; then carrying out microwave irradiation on the treated graphite, so that the graphite intercalation layer is decomposed to generate a large quantity of gas and further increase the spacing of the graphite layer; successively dispersing the treated graphite in a low-polarity organic solvent for ultrasonic treatment, so that the graphite is stripped to generate the grapheme; and finally carrying out centrifugal treatment to obtain upper-layer liquid after treatment, i.e. fewer-layer graphene dispersion liquid. The preparation method has the advantages of simplicity in operation, short time consumption, low cost, high grapheme yield, good repeatability and easy realization of industrialized mass production; and the fewer-layer graphene prepared by the preparation method is below 10 in quantity of layers and has the advantages of fewer defects, fewer oxygen-contained groups and high conductivity.

Description

technical field [0001] The invention relates to the technical field of graphene materials, in particular to a method for preparing few-layer graphene. Background technique [0002] Graphene is carbon atoms on a two-dimensional plane with sp 2 A single atomic layer crystal with a honeycomb lattice structure formed by hybridization, and few-layer graphene refers to graphene flakes with 3 to 10 layers. Since graphene was successfully prepared by scientists for the first time in 2004 (Novoselov, K.S. et al. Science. 2004, 306, 666), this new material has received extensive attention from scientists. Since graphene is a zero-bandgap semiconductor, the electrons moving on it are similar to massless relativistic particles, so graphene exhibits ultrahigh (greater than 15000cm 2 / V·s) electron mobility (Morozov.S.V.et al.Phys.Rev.Let.2008, 100, 016602), is expected to be used to develop a new generation of electronic components or transistors that are thinner and conduct electricit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19C01B32/194
Inventor 周明秦禄昌崔平唐捷
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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