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Preparation method of porous graphene

A technology of porous graphene and thin-layer graphene, applied in graphene, chemical instruments and methods, nanotechnology for materials and surface science, etc. , to achieve the effect of high specific surface area, good application prospect and simple process

Active Publication Date: 2013-06-12
苏州格瑞丰纳米科技有限公司
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  • Abstract
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Problems solved by technology

[0003] At present, there are many methods for preparing graphene at home and abroad, including direct mechanical exfoliation (Novoselov, K.S.et al., Science, 2004,306,666), chemical vapor deposition (Li X.S.et al., Science, 2009,324,1312), Chemical transformation (oxidation (Li, D., et.al.,. Nature Nanotech.2008, 3, 101) or fluorination. Liu, L.H. et al., Nano Lett. 2010, 3754), cleavage of intercalated graphite ( Park, S.et al., NatureNanotech.2009, 4, 217), liquid phase chemical cleavage (Blake, P.et al.Nano Lett.2008, 8, 1704) and other methods, but in terms of graphene punching There are not many results, and the preparation of perforated graphene mostly adopts the preparation process of activated carbon, that is, the method of mixing and heating graphene with strong alkali or potassium chloride (YanwuZ., et al., science, 2011, 322, 1537), although this method can punch holes on the surface of graphene, the preparation process is quite complicated and cannot be widely promoted

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preparation example Construction

[0028] As mentioned above, in view of the deficiencies in the prior art, the present invention aims to provide a method for preparing porous graphene. As one of the more preferred embodiments, the preparation method may include the following steps:

[0029] 1) preparing intercalated graphite;

[0030] 2) taking a polar solvent to replace the intercalated matter in the intercalated graphite to prepare intercalated graphite containing a large amount of polar solvent;

[0031] 3) Microwave irradiation of intercalated graphite containing polar solvents to prepare porous worm-like expanded graphite;

[0032] 4) Ultrasonic and dry the expanded graphite to prepare porous graphene.

[0033] Obviously, this preparation method can also be extended to prepare other two-dimensional material systems, for example, porous BN, MoS2, WS2, MoSe2, MoTe, TaSe, NbSe, NiTe, Bi2Te materials, etc.

[0034] The aforementioned porous graphene contains a large number of pore structures, the pore size...

Embodiment 1

[0043] Embodiment 1: put 10g flake graphite (325 order) in the mixed solution of 20ml concentrated nitric acid and the vitriol oil, fully stir 2 hours, treat that the graphite in the solution becomes dark blue completely, stop stirring, prepare mixed acid intercalation graphite ( Its XRD diagram is shown in figure 1 ), the resulting intercalated graphite was put into a polar solvent, fully stirred and infiltrated for 24 hours, and then dried. Place the dried intercalated graphite in a microwave oven, separate the microwave source from top to bottom, select a microwave power of 5kw, and microwave for 1 minute. Take out the expanded graphite powder, add it to a polar solvent, and ultrasonicate for 2 hours. After being ultrasonically opened, they are dried to obtain porous graphene (see figure 2 and image 3 )

Embodiment 2

[0044] Embodiment 2: 10g flake graphite (325 mesh) and 50g ferric chloride are divided into two zones and put into a glass container, the temperature at one end of graphite is 360°C, and the temperature at one end of ferric chloride is 400°C. After reacting for 24 hours and cooling down, break the glass container, take out the intercalated graphite inside, and wash it. Add ethanol and put it into a ball mill to grind for 10 hours, then take it out and put it into an autoclave containing ethanol, raise the temperature to 120°C, heat for 10 hours, take it out, and dry it. Put the dried intercalated graphite into a microwave oven, separate the microwave source from top to bottom, select the microwave power as 5kw, and microwave time for 30s, take out the expanded graphite powder, add it to water, and ultrasonicate for 2 hours, until all the graphite is ultrasonicated After being opened, it is dried to obtain porous graphene.

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Abstract

The invention discloses a preparation method of porous graphene. The preparation method comprises the following steps of: (1) mixing intercalated graphite with a polar solvent to ensure that the polar solvent is fully absorbed by the intercalated graphite; and (2) carrying out microwave radiation on the intercalated graphite with the polar solvent to ensure that the intercalated graphite is fully dissociated to form graphene and a plurality of holes are formed in the surface of the graphene, thereby obtaining perforated thin-layer graphene. Preferably, the preparation method also comprises the following steps of fully washing and drying the perforated thin-layer graphene to obtain the target product. The preparation method disclosed by the invention is simple in process, strong in operability and beneficial to preparing perforated thin-layer graphene powder at a low cost and on a large scale; and the obtained thin-layer graphene with a porous structure has the advantages of high specific surface area, permeability of the solvent and good application prospect.

Description

technical field [0001] The invention relates to a preparation method of a graphene material, in particular to a preparation method of a porous graphene, which belongs to the field of new nanometer materials. Background technique [0002] Graphene is a two-dimensional carbon nanostructure material composed of single-layer graphite sheets. In 2004, the A.K.Geim group of the University of Manchester in the United Kingdom made a breakthrough in the preparation of single-atom-thick graphite samples by mechanical exfoliation (Novoselov, K.S. et al., Science, 2004, 306, 666). The mobility of graphene can exceed ~104cm2 / V s, thermal conductivity (3500-5300W / mK). It is considered to be one of the most promising materials for constructing future nanoelectronic circuits in a bottom-up manner, and is expected to be obtained in future high-speed nanoelectronics, energy conversion devices, filling components of functional composite materials, biochemical sensors, etc. application. The ...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B21/064C01B19/04C01G41/00C01G39/00B82Y30/00C01B32/19
Inventor 刘立伟郭玉芬李伟伟朱超廖书田龚佑品龙明生徐建宝
Owner 苏州格瑞丰纳米科技有限公司
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