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A dispersion of graphene in ethanol was achieved using solvent surface deposition, low boiling point solvents are preferred.
Published on 05 October 2010 on http://pubs.rsc.org | doi:10.1039/C0CC02688C
exchange from N-methyl-2-pyrrolidone (NMP) that enables However, most low boiling solvents, for example, water and
broader application of dispersed graphene. ethanol, have surface tension (72.8 mJ m 2 and 22.1 mJ m 2,
respectively) that are unsuitable for the direct exfoliation of
Since its discovery by Geim and coworkers in 2004,1 graphene graphene. Therefore, a more suitable method is required.
Downloaded by University of Groningen on 14 December 2010
has attracted widespread attention due to its unique properties, Coleman and coworkers recently reported that graphene
such as room temperature quantum effects, ambipolar electric could be prepared by exfoliation of graphite in a surfactant/
field effects, and high carrier mobility.2 Graphene of less than water solution, to yield large amounts of few-layer graphene
10 layers shows properties distinct from those of bulk sheets and small quantities of single-layer graphene sheet with
graphite3 and hence single- and few-layer graphenes are highly the aid of the surfactant.16
attractive materials for electronics, composites and devices. As Here, we report the discovery that graphene can form a
with carbon nanotubes, a major problem encountered is the relatively stable high concentration dispersion in ethanol using
preparation of graphene on a large scale. To date, several a solvent exchange process from NMP. The preparation of the
methods have been reported, including mechanical,1 epitaxial,4,5 graphene dispersion in ethanol is confirmed by spectroscopic
reduction of graphene oxide,6–10 and solvent dispersion of and microscopic techniques, and the generated film shows
graphite.11–14 Though the mechanical method can yield high good conductivity.
quality single-layer graphene sheets, it is time consuming and The preparation of the graphene dispersion in ethanol is
features low throughput, which makes it unsuitable for large shown in Scheme 1. Approximately, 200 mg of graphite in
scale production. There are also reports on epitaxial growth of 200 ml NMP was sonicated for 2 h, and centrifuged at
graphene on metal substrates,4,5 but this process requires very 4000 rpm for 30 min to remove large particles. The supernatant
high temperature and subsequent transfer of the sample to of graphene in NMP was decanted, and then 150 ml of the
other substrates. Compared with these methods, the latter two above supernatant was filtered through a 0.45 mm poly-
methods have obvious advantages, such as scalable production tetrafluoroethylene (PTFE) membrane. The obtained filter
and ease of solution processing. For example, chemical or cake was dispersed in 50 ml ethanol with mild sonication
thermal treatment of graphene oxide provides a material that and filtered again. This process was repeated five times (each
is conductive and can be used in device applications.9,10 time with 50 ml ethanol and ca. 10 min of sonication) and
However, the reduced graphene oxide still contains defects finally the filter cake was redispersed in 30 ml ethanol. This
and the original properties of graphene are not recovered.15 suspension was centrifuged at 1000 rpm for 30 min, the
Recently, several groups have shown that graphene can be supernatant was decanted and further sonicated for several
prepared by exfoliation of graphite in certain solvents, such as minutes to give the required homogeneous graphene dispersion
N-methyl-2-pyrrolidone (NMP),11 dimethylformamide in ethanol (the sample vial was sealed to prevent evaporation
(DMF),12 and o-dichlorobenzene (ODCB)13 to produce single- of ethanol). The repeated washing steps yield a stable dispersion
and few-layer graphene sheets. These above solvents have of graphene in ethanol containing o0.3 vol% NMP (see ESIw,
surface tensions close to 40 mJ m 2, and are suitable for direct Fig. S1).
exfoliation of graphene.11 However, these solvents hold their Using the solvent exchange process, graphene can form a
own disadvantages. Their high boiling points limit their relatively stable dispersion in ethanol, at a concentration
viability for real manipulation. Thus, dispersion of graphene of up to 0.04 mg ml 1 (Fig. 1a, right). Fig. 1b shows the
in low boiling solvents without surfactants or other stabilizers absorption spectrum of graphene in ethanol after dilution
is useful in many applications. For example, in composites and with ethanol, which is flat and featureless. Over one week,
a
Stratingh Institute for Chemistry, University of Groningen,
Nijenborgh 4, 9747 AG Groningen, The Netherlands.
E-mail: w.r.browne@rug.nl, b.l.feringa@rug.nl;
Fax: +31-050-363-4296
b
Physics of Nanodevices, Zernike Institute for Advanced Materials, Scheme 1 Procedure for the preparation of graphene in ethanol:
University of Groningen, The Netherlands.
(a) sonicate for 2 h, (b) centrifuge at 4000 rpm/30 min, (c) filter,
E-mail: b.j.van.wees@rug.nl
w Electronic supplementary information (ESI) available: Details of redisperse the filter cake in ethanol, and repeat this process 5 times,
experimental methods and additional TEM, IR data and determination (d) redisperse the filter cake in ethanol, centrifuge at 1000 rpm/30 min,
of residual NMP content. See DOI: 10.1039/c0cc02688c then pipette the supernatant and sonicate for several minutes.
This journal is c The Royal Society of Chemistry 2010 Chem. Commun., 2010, 46, 7539–7541 7539
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7540 Chem. Commun., 2010, 46, 7539–7541 This journal is c The Royal Society of Chemistry 2010
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This journal is c The Royal Society of Chemistry 2010 Chem. Commun., 2010, 46, 7539–7541 7541