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Graphene
Graphene-Based Materials: Synthesis, Characterization,

Properties, and Applications
Xiao Huang, Zongyou Yin, Shixin Wu, Xiaoying Qi, Qiyuan He, Qichun Zhang,
Qingyu Yan, Freddy Boey, and Hua Zhang*
From the Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . .1877
2. Graphene-Based Materials. . . . . . . . . . . 1878
3. Applications of Graphene and
Graphene-Based Materials . . . . . . . . . . 1885
4. Conclusion and Outlook . . . . . .. . . . . . . 1893
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Graphene, a two-dimensional, single-layer sheet of sp2

hybridized carbon atoms, has attracted tremendous
attention and research interest, owing to its exceptional
physical properties, such as high electronic conductivity,
good thermal stability, and excellent mechanical strength.
Other forms of graphene-related materials, including
graphene oxide, reduced graphene oxide, and exfoliated
graphite, have been reliably produced in large scale.
The promising properties together with the ease of
processibility and functionalization make graphenebased materials ideal candidates for incorporation into
a variety of functional materials. Importantly, graphene
and its derivatives have been explored in a wide
range of applications, such as electronic and photonic
devices, clean energy, and sensors. In this review, after a
general introduction to graphene and its derivatives, the
synthesis, characterization, properties, and applications of
graphene-based materials are discussed.
2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
small 2011, 7, No. 14, 18761902
Graphene-Based Materials
1. Introduction
Graphene is a 2D single layer of carbon atoms with
the hexagonal packed structure.[1,2] The carbon bonds are
sp2 hybridized, where the in-plane C-C bond is one of the
strongest bonds in materials and the out-of-plane bond,
which contributes to a delocalized network of electrons, is
responsible for the electron conduction of graphene and provides the weak interaction among graphene layers or between
graphene and substrate. With these unique structural characteristics, graphene has shown exceptional physical properties,
which have attracted enormous research interest in both scientific and engineering communities.[317]
One of the most remarkable properties of graphene is
that its charge carriers behave as massless relativistic particles or Dirac fermions, and under ambient conditions they
can move with little scattering. This unique behavior has
led to a number of exceptional phenomena in graphene.[18]
First, graphene is a zero-bandgap 2D semiconductor with
a tiny overlap between valence and conduction bands.[18]
Second, it exhibits a strong ambipolar electric field effect so
that the charge carrier concentrations of up to 1013 cm2 and
room-temperature mobilities of 10 000 cm2 s1 are measured.[18] Third, an unusual half-integer quantum Hall effect
(QHE) for both electron and hole carriers in graphene has
been observed by adjusting the chemical potential using the
electric field effect.[19,20] In addition, graphene is highly transparent, with an absorption of 2.3% towards visible light.[6]
Its thermal conductivity, k, is measured with a value of
5000 W mK1 for a single-layer sheet at room temperature.[21]
Graphene also possesses the excellent mechanical strength.
The intrinsic mechanical properties of free-standing monolayer
graphene membranes were measured by nano-indentation
in an atomic force microscope.[3] The breaking strength
is 42 N m1 and the Young's modulus is 1.0 TPa, indicating it
is one of the strongest materials ever measured.
Up until now, versatile methods have been developed for
fabrication, growth, or synthesis of graphene and its derivatives. In graphite, the adjacent graphene layers are bound
by weak van der Waals forces.[22] Therefore, the pristine
graphene can be obtained from the mechanical exfoliation
of graphite using adhesive tapes.[14,18] The bottom-up growth
of graphene sheets is an alternative to the mechanical exfoliation of bulk graphite. Chemical vapor deposition (CVD)
has been used to grow single- and few-layer graphene
sheets on metal surfaces, such as Ni and Cu.[8,2356] Largearea epitaxial graphene films up to a few micrometers in
size can be subsequently transferred to other substrates.
Carbon segregation can also become graphene layers on
carbon-containing substrates, such as SiC,[5772] through hightemperature annealing. However, these methods are impractical for large-scale solution-based processes. Therefore, the
oxidation and exfoliation of graphite oxide, followed by the
chemical reduction,[73] has been used to prepare reduced
graphene oxide (rGO) sheets[74116] or chemically functionalized graphene (CFG). This is one of the most developed
methods in the literature, and several types of reduction
agents have been reported, such as hydrazine,[7486,9093]
strong alkaline media,[117] vitamin C,[116] and bovine serum
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albumin (BSA).[118] Besides the reduction with chemical

agents, electrochemical,[109,119121] photochemical[87,122] and
thermal[94,111,123131] reduction methods have been developed as well. As the precursor of rGO, graphene oxide
(GO) sheets,[5972,132145] exfoliated from graphite oxide,
are obtained by the Hummers method, via the reaction of
graphite with a mixture of potassium permanganate (KMnO4)
and concentrated sulfuric acid (H2SO4).[7478,8082,146]
GO sheets are thus highly oxidized and characterized by the
dominant presence of epoxides, alcohols, and carboxylic acid
groups.[147,148] These functional groups render GO and rGO
advantageous compared to the pristine graphene, in terms of
the tunability in electrical and optical properties via chemical
reactions.[149,150] Unfortunately, rGO shows electric conductivity several orders lower than the pristine graphene because
of the incomplete reduction and the presence of numerous
defects, which disrupt the sp2 network.[75,77,80,150152] In order
to overcome the poor conductivity of rGO, several methods
have been developed. For example, the non-oxidation liquidphase exfoliation of graphite has been demonstrated, which
can produce large-area single-layer graphene by ultrasonication of graphite in both aqueous[153] and non-aqueous[154]
solutions. Re-intercalation and ultrasonication of thermally
exfoliated expandable graphite (EG) can produce singlelayer graphene sheets as well.[155] Even without ultrasonication, the readily dispersible graphene sheets from intercalated
compounds of graphite have been reported by using ternary
potassium salt as the intercalation agent.[156] One-step electrochemical exfoliation of graphite into graphene layers has
also been realized in ionic liquids.[157] Moreover, the arc
discharge method,[158] and the direct chemical synthesis of
graphene in solution have been developed from nongraphitic
substances, such as the reaction of ethanol and sodium followed by pyrolysis,[159] and the organic synthesis of graphenelike polyaromatic hydrocarbons.[160]
Besides the graphene-based 2D sheets, other graphenerelated materials have been fabricated/synthesized as well,
such as zero dimensional (0D) graphene quantum dots,[161163]
1D graphene nanoribbons (GNRs),[5,163181] and graphene
nanomeshes (GNMs).[182187] These materials are expected to
possess different electrical and optical properties, due to the
variation in size and geometry, and the presence of a large
X. Huang, Dr. Z. Y. Yin, S. X. Wu, X. Y. Qi, Q. Y. He, Prof. Q. C. Zhang,

Prof. Q. Y. Yan, Prof. F. Boey, Prof. H. Zhang
School of Materials Science and Engineering
Nanyang Technological University
50 Nanyang Avenue, Singapore 639798, Singapore
Fax: +656790-9081
Website: http://www.ntu.edu.sg/home/hzhang/
E-mail: hzhang@ntu.edu.sg
Prof. F. Boey, Prof. H. Zhang
Centre for Biomimetic Sensor Science
Nanyang Technological University
50 Nanyang Drive, Singapore 637553, Singapore
X. Y. Qi
Singapore Institute of Manufacturing Technology
71 Nanyang Drive, Singapore 638075, Singapore
DOI: 10.1002/smll.201002009
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amount of edge defects. For example, the GNRs and GNMs

have exhibited band opening with much enhanced onoff
ratios in field-effect transistors (FETs) compared to 2D
graphene sheets.[5,182]
Featuring unique physical and chemical properties, and
having reliable synthetic methods for both solid and solution-phase processes, graphene and its derivatives have been
incorporated into a number of functional materials to form
composites, and have been used as building blocks for various kinds of applications, including FETs,[18,75,76,110,188216]
memories,[85,86,217233] photovoltaic devices,[23,80,84,161,234252]
photocatalysis,[251,253256] sensors,[75,119,257266] cell cultures,[83]
intracellular imaging,[267] and matrices for matrix-assisted
laser desorption/ionization time-of-flight mass spectroscopy
(MALDI-TOF-MS).[82,268,269] In the following context, we
will focus on the synthesis and characterization of graphenebased materials, the exploration of their properties, and
studies of their applications.
2. Graphene-Based Materials
Pristine graphene is a hydrophobic material, and has
no appreciable solubility in most solvents. Nevertheless,
the processing of graphene composites concerns itself
foremost with the solubilization of graphene. To improve
the solubility of graphene, different functional groups
have been attached to the carbon backbone by chemical
modification,[73,101,270,271] covalent,[272296] or noncovalent
functionalization.[74,77,152,287,289,290,293,297306]
It is impossible to directly disperse hydrophobic graphite
flakes or graphene sheets in water without the assistance
of dispersing agents. Because of the presence of oxygencontaining groups, the chemically reduced graphene oxide
(rGO), or so called chemically modified graphene, can form
the homogeneous aqueous suspension by controlled reduction of graphene oxide (GO) with hydrazine and dialysis
while maintaining the pH of the solution at about 10 by the
addition of amonia.[73] However, the resulting solubility of
rGO in water is very limited, with a value of <0.5 mg/mL.[73]
Besides water, a number of organic solvents, such as
ethanol, acetone, dimethyl sulfoxide (DMSO), and tetrahydrofuran (THF), can be used to give suspensions of highly
reduced GO sheets, when mixed with dimethyl formamide
(DMF) and water in a volume ratio of 90:9:1 for (the added
solvent):DMF:water.[101]
Metal ions and functional groups have been used to
modify rGO sheets as well. The sequential chemical reaction
of GO sheets in water with KOH and then with hydrazine
has shown to produce K-modified graphene (hKMG) sheets,
which can lead to a homogeneous aqueous suspension.[270] In
addition, p-phenyl-SO3H groups were introduced on GO, and
after reduction the lightly sulfonated rGO can be readily dispersed in water at reasonable concentrations (2 mg/mL) in
the pH range of 3 to 10.[271]
Covalent modification of graphene involves the reaction
of functional molecules and the oxygenated groups on the
GO or rGO surface, such as carboxyl groups at the periphery,
and epoxy, hydroxyl, and C=C groups in the basal plane
1878 www.small-journal.com
Hua Zhang studied at Nanjing University

(B.S., M.S.), and completed his Ph.D. at
Peking University (with Zhongfan Liu) in
1998. After postdoctoral work at Katholieke Universiteit Leuven (with Frans De
Schryver) and Northwestern University
(with Chad Mirkin), and working at NanoInk
Inc. and the Institute of Bioengineering and
Nanotechnology (Singapore), he joined
Nanyang Technological University in 2006.
He was promoted to a tenured associate
professor in March 2011. He is an Associate
Editor of the International Journal of Nanoscience, on the Editorial Board of NANO,
and on the Advisory Committee of IOP
Asia-Pacific. His research interests focus on carbon materials (graphene and CNTs)
and their applications; controlled synthesis, characterization, and application of novel
nanomaterials; and surface fabrication from the micro- to nanometer scale. He has
published more than 120 papers with over 2220 citations and an H-index of 26.
of GO or rGO.[148] For example, rGO dispersions in THF,

CCl4, and 1,2-dichloroethane (EDC) were obtained by converting the edge carboxylic acid groups of rGO into octadecylamines, which sterically stabilized the graphene sheets.[272]
The treatment of GO with organic isocyanates could lead
to the derivatization of both the edge carboxyl and surface
hydroxyl functional groups via the formation of amides or
carbamate esters (RnCO) (Figure 1A).[273] Esterification of
the carboxylic groups in GO with the hydroxyl groups in
poly(vinyl alcohol) (PVA) was also realized in the synthesis
of GOpolymer composite sheets.[274] On the other hand, the
basal surface of GO can be functionalized by the nucleophilic
ring-opening reaction between the epoxy groups of GO and
the amine groups of an amine-terminated organic molecular,
such as 1-(3-aminopropyl)-3-methylimidazolium bromide (an
ionic liquid) (Figure 1B) and 3-amino-propyltriethoxysilane
(APTS).[275,276] Also, rGO platelets were covalently functionalized with diazonium salts (e.g., sodium dodecylbenzenesulfonate, SDBS), and the resulting rGO was readily dispersed
in several polar organic solvents (Figure 1C).[277] Additionally, by the [2+1] cycloaddition of nitrenes onto the C=C
double bonds, a number of different organic compounds, such
as azido-phenylalanine (Figure 1D) and azidotrimethylsilane,
have been attached to the graphene surfaces.[278280] Recently,
the surface of graphene was covalently functionalized by
grafting polystyrene-polyacrylamide (PS-PAM) through insitu free-radical polymerization.[281]
Compared to covalent functionalization, noncovalent
functionalization based on the van der Waals force or the
interaction between rGO and stabilizers not only gives less
negative impact on the structure of graphene and its derivatives, but also provides the feasibility to tune their solubility
and electronic properties.
The first noncovalent functionalized stable graphene
dispersion was produced by reducing an aqueous GO
dispersion with hydrazine in the presence of poly(sodium
4-styrenesulfonate) (PSS).[152] In this experiment, the rGO
sheets were stabilized via the association with the hydrophobic backbone of PSS, while the hydrophilic sulfonate side
groups sustained the whole graphenePSS complex in water.
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Noncovalent functionalization of graphene sheets through

the interaction was reported by using the water-soluble
aromatic organic molecule 1-pyrenebyturate (PB) as a stabilizer; and through subsequent vacuum filtration, large-area
flexible PBgraphene films with layered structures could
be prepared.[297] This approach provides a general route for
the preparation of functionalized graphene through the
interaction. Other reports based on this strategy have shown
significantly improved solubility and conductivity of the functionalized graphene sheets.[289,298,300,301]
2.1. GraphenePolymer Composites
Figure 1. A) Isocyanate treatment of GO where organic isocyanates

react with the hydroxyl (left oval) and carboxyl groups (right oval) of
GO sheets to form carbamate and amide functionalities, respectively.
Reproduced with permission.[273] Copyright 2006, Elsevier, Inc.
B) Covalent functionalization of epoxy groups of GO by an ionic liquid.
Reproduced with permission.[276] Copyright 2009, Royal Society of
Chemistry. C) Covalent functionalization of rGO with diazonium salts.
Reproduced with permission.[277] Copyright 2008, American Chemical
Society. D) Functionalization of exfoliated microcrystalline graphene
(G) with azido-phenylalanine (Phe-N-G) in o-dichloro-benzene (ODCB)
by nitrene chemistry. Reproduced with permission.[278] Copyright 2009,
Royal Society of Chemistry.
In addition, biomolecules have been involved in the functionalization process of graphene based on the van der Waals
force, such as using single-strand DNA (ssDNA) to stabilize
aqueous suspensions of single-layer graphene sheets.[299]
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Because of their good conductivity, thermal stability, and

excellent mechanical strength, graphene and its derivatives
are important filler materials for polymer composites. The
properties and performances of graphenepolymer composites not only depend on the quality of graphene filler
and polymer matrix, but also depend on the dispersity of
the filler, the bonding between the filler and matrix, and the
ratio of filler to matrix. These factors are mainly determined
by the fabrication processes. Similar to the conventional
polymer processing, the methods applied for the fabrication
of graphenepolymer composites are solution mixing,[307312]
melt blending,[313315] and in-situ polymerization.[316327]
Solution mixing is one of the most commonly used
methods for preparation of polymer composites, since it is
straightforward, requires no special instruments, and allows
for large-scale production. One of the major concerns in
solution mixing is the solubility or dispersity of graphene
sheets in the polymer solution. For example, the water soluble polymer, such as poly(vinyl alcohol) (PVA), is easy to
be mixed with aqueous GO dispersions at various concentrations.[307,328] However, the low solubility of GO and rGO
in organic solvents poses great challenge in synthesis of
graphenepolymer composites in organic solutions. One way
to solve this problem is to use ultrasonication to produce
short-time metastable dispersions of GO or other graphene
derivatives, which are then mixed with polymer solutions,
such as poly(methyl methacrylate) (PMMA),[329] polycaprolactone (PCL),[308] polyurethane (PU),[309,330] and polyaniline
(PANI).[310] High-speed shearing has also been utilized to
mix graphene-based fillers and the polymer matrices, while
ice baths have been used to prevent extra heating from the
shearing process.[311] However, re-aggregation of the rGO
sheets might occur during the slow process of solvent evaporation. Therefore, it is important to modify the graphene
sheets or graphene derivatives with functional molecules, in
order to increase the solubility in various kinds of solvents.
For example, after GO sheets were functionalized with
phenyl isocyanate and mixed with polystyrene (PS) solution
in DMF,[331] they were further reduced to rGO. During the
experiment, the polymer matrix prevented the re-aggregation
of rGO sheets and the dispersed suspension maintained very
well. However, these studies only rely on the stabilizers with
weak electronic delocalization systems (such as small aromatic molecules), which limit the solubility of the obtained
rGO based materials.
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Recently, in our group, a specially designed conjugated

polyelectrolyte (CPE), PFVSO3 with a planar backbone and
charged sulfonate and oligo(ethylene glycol) (OEG) side
chains, was used to modify rGO sheets (Figure 2A,B).[77] Due
to the strong interaction between PFVSO3 and rGO, the
resulting CPE-functionalized rGO (PFVSO3-rGO) shows
excellent solubility and stability in a variety of polar solvents,
including water, ethanol, methanol, DMSO, and DMF. In
order to further improve the solubility of graphenepolymer
composites in both high polarity (such as water and ethanol)
and low polarity (such as toluene and chloroform) solvents,
an amphiphilic coil-rod-coil conjugated triblock copolymer
(PEG-OPE, chemical structure shown in Figure 2C),[74] which
is composed of one lipophilic -conjugated oligomer and two
hydrophilic PEG coils, has been designed and synthesized
to modify rGO sheets. The conjugated rigid-rod backbone
of PEG-OPE can attach to the basal plane of rGO by the
strong interaction (Figure 2D), whereas the lipophilic
side chains and two hydrophilic coils of the backbone fly
away from the rGO surface to form an amphiphilic outerlayer. As a result, the obtained graphenepolymer composite
are soluble in both organic low-polarity and water-miscible
high-polarity solvents (Figure 2E).
Melt compounding is another popular fabrication method
in industry for high-yield fabrication of polymer composites,
which involves the blending of filler materials and polymer
matrices using high-shear forces at elevated temperatures.
Polylactide (PLA)-exfoliated graphite (EG) composites have
been successfully prepared by mixing PLA chips and EG in
a mechanical mixer at 175200 C.[313] In another example,
graphene platelets were obtained by thermal reduction of

GO, and then melt-blended with polyethylene terephthalate
(PET) at 285 C to give the PETgraphene composite.[314]
However, melt compounding is not as effective as the solution mixing method, in terms of the ability to achieve good
dispersity and distribution of the filler materials in the matrix.
In addition, the use of high shear forces can sometimes break
the filler materials, such as carbon nanotubes and graphene
sheets.[315]
In-situ polymerization involves the mixing of monomer
solution and the suspensions of graphene- based materials,
in the presence of catalysts at proper reaction conditions.
Epoxy is a typical polymer suitable for in-situ polymerization.[316318,332] For example, a graphene nanoplatelet suspension was mixed with epoxy resins and subjected to high-shear
mixing. While stirring and heating the mixture to remove
the solvent, epoxy curing agent was added to finalize the
polymerization process.[316] Polyaniline (PANI) is another
type of polymer, which is usually synthesized by in-situ
polymerization.[319323] Since the polymerization of PANI is
an oxidative process, an oxidative agent, such as ammonium
persulfate, is added to the reaction solution to facilitate the
polymerization.[321] In addition to solution-based oxidation,
graphenePANI composite can be prepared by the in-situ
anodic electropolymerization,[324] where graphene paper
was obtained using H2 reduction of thermally expanded GO,
followed by filtration and vacuum drying. PANI was then
electrochemically deposited with the graphene paper as the
working electrode in a three-electrode cell containing the
electrolyte with aniline monomers. Besides epoxy and PANI,
Figure 2. A) Chemical structure of the designed PFVSO3. B) Schematic illustration of PFVSO3-stabilized rGO sheets. Reproduced with permission.[77]
C) Chemical structure of PEG-OPE. D) Schematic illustration of PEG-OPE stabilized rGO sheets. E) Photograph of PEG-OPE-rGO dispersed in different
solvents. [PEG-OPE-rGO] = 1.22 mgmL1. Reproduced with permission.[74]
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other polymers such as silicone,[325] polystyrene,[326] and

poly(vinyl choloride/vinyl acetate) copolymer[327] have been
hybridized with graphene via the in-situ polymerization.
By employing the aforementioned methods, graphene
and graphene derivatives are mostly randomly stacked in
the polymer matrix. To enhance the directional mechanical
strength of graphenepolymer composite, layer-by-layer
(LbL) assembling has been carried out to prepare freely
standing composite membranes. For example, the LbL fabrication was conducted using the LangmuirBlodgett (LB)
technique to transfer GO sheets onto multilayer films of
polyelectrolytes [poly(allylamine hydrochloride) (PAH) and
poly(sodium 4-styrene sulfonate) (PSS)].[333]
To date, graphenepolymer composites have shown
improved properties in electrical conductivity, electrochemical capacity, mechanical strength, and thermal stability and
conductivity. One of the mostly employed host polymers is
PANI, and many reports on graphenePANI composites have
achieved enhanced electrochemical performances.[310,319324]
For example, the flexible graphenePANI composite paper
prepared by in-situ electropolymerization has exhibited a
good electrochemical capacitance of 233 F/g, and 135 F/cm3
for gravimetric and volumetric capacitance, respectively. It
surpasses many carbon-based flexible electrodes as a promising candidate for supercapacitors.[324] In another report,
by coating graphene nanosheets (GNS) with 2 nm PANI
nanoparticles, a high capacitance of 1046 F/g was achieved
compared to 115 F/g for pure PANI.[321] In addition to PANI
nanoparticles, PANI nanofibers have been incorporated with
GO sheets, which exhibited a specific capacitance of 531 F/g
at a mass ratio of 100:1 for PANI:GO.[323]
In addition to the conducting polymers, insulating polymers have also been used to host graphene-based fillers. The
electrical conductivity of polystyrenegraphene composites
were studied at different composition ratios.[331] Percolation occurred at only 0.1 vol% loading of functionalized
graphene sheets (FGS), which was lower than many other 2D
filler materials. This low percolation threshold can be attributed to the high aspect ratio of the graphene sheets, their
homogeneous dispersion in the polymer matrix, as well as
the good fillermatrix interfacial interaction induced by the
surface functional groups. With the other polymer matrices,
poly(vinyl chloride/vinyl acetate) copolymer/graphene composites exhibited a percolation threshold of 0.15 vol%,[327]
while the PETgraphene composites showed a percolation
threshold of 0.47 vol%, and a conductivity of 2.11 S/m was
obtained with only a loading of 3.0 vol%.[314]
As mentioned in the Introduction, the single-layer
graphene sheet is one of the strongest materials ever measured, with a breaking strength of 42 N m1 and a Youngs
modulus of 1.0 TPa.[3] Using graphene derivatives as filler
materials, a number of reports have shown the enhanced
mechanical properties of graphenepolymer composites.
Functionalized GO layers were embedded in the polyelectrolyte multilayers of PAH and PSS by LbL assembly. The
resulting composite membrane showed huge improvement in
the elastic modulus, from 1.5 GPa for pure polymer membrane to 20 GPa for 8 vol% of graphene loading. These polyelectrolyte-based membrane materials are conductive and
small 2011, 7, No. 14, 18761902
flexible and exhibit good mechanical properties, which can

be used in capacitive pressure sensors, an alternative to the
stiff silicon in micro-electromechanical systems (MEMS).[333]
In another report, strong and ductile poly(vinyl alcohol)
(PVA)graphene composites were made by vacuum filtration. At 3 wt% of GO loading, a Young's modulus of 4.8 GPa
and tensile yield strength of 110 MPa were achieved. To further improve the interaction of the graphene filler and the
polymer matrix, thus facilitating the effective load transfer,
polyurethane (PU) was covalently bonded with GO platelets, and the Young's modulus and hardness were increased
by 900% and 327%, respectively. The resulting improved
hardness indicates a high resistance to scratching, which is
important in surface coating applications.[309] The effective
enhancement of mechanical properties of these polymer
graphene composites arises from not only the intrinsic properties of graphene, but also the good dispersion of filler, as
well as the effective interfacial interaction between the filler
and host polymer, which prevents the movement of polymer
chains under the external force.
The thermal stability of polymers is generally characterized by the glass transition temperature (Tg), above which
the molecular chains begin to slide pass each other when
an external force is applied. By adding stiff filler materials,
which interfere with the flowing process of the chains, the Tg
of polymer composites can be increased. For example, after
poly(amido amine) (PAMAM) was mixed with graphitic
nanoplatelets (FNPs) in THF by ultrasonication and highspeed shearing, the obtained composite exhibited up to a
30 C increase in Tg with 15 wt% loading of the filler.[329]
The performance of the composites was further enhanced
by replacing the FNPs with functionalized graphene sheets
(FGSs) as the nanofiller, which was obtained by the thermal
exfoliation of highly oxidized graphite oxide. Compared to
FNPs, FGSs possess a larger amount of single-layer graphene
sheets with wrinkled morphology and functionalized surfaces,
which in turn give stronger fillermatrix interactions. With a
loading of 0.05 wt% FGS, there is an increase of 30 C in Tg
for the formed PAMAMFGS composite, while with a loading
of 1 wt% FGS, the improvement of Tg in poly(acrylonitrile)
(PAN)FGS composite reaches more than 40 C.[311] Importantly, at a <1 wt% loading of nanofiller, the FGS surpasses
all other carbon-based nanofillers in terms of the improved
glass transition temperature of polymers.
Since elastomers such as silicone foams are usually operated at above the glass transition temperature, their thermal
stability is determined by measuring the degradation temperature. For example, FGSs have been successfully embedded
in silicone through an in-situ foaming process. Thermogravimetric analysis (TGA) showed an increase of up to 55 C in
the degradation temperature of siliconeFGS composites
with 0.25 wt% loading of the filler.[325] Another example
shows that when PLA a degradable polymer commonly
used in biological applications, was composited with EG, the
thermal degradation temperature of PLAEG composite was
improved by 10 C at a loading of only 0.5 wt% of EG.[313]
Graphene has shown excellent thermal conductivity, with
a measured k value of ,000 W/mK for a single-layer sheet at
room temperature.[21] Therefore, its embedment in a polymer
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matrix is expected to significantly enhance the thermal conduction of the composite. Thermally exfoliated graphite nanoplatelets were incorporated in an epoxy matrix. It was found
that the introduction of few-layer graphene (layer number:
4) resulted in a thermal conductivity enhancement of more
than 30 times at k = 6.44 W/mK with a loading of 25 vol%
of graphene.[316] This result outperforms conventional fillers,
such as silver, alumina, and silica, which require 5070%
loading to achieve a similar result. In addition, when FGSs
were added as the filler in silicon foam matrix, 0.25 wt% of
loading had led to a 6% increase in the ultimate thermal conductivity.[325] The large aspect ratio, 2D geometry, high stiffness, and low thermal interface resistance of graphene have
caused the enhanced thermal conductivity in these reports.
Such composite foams with excellent heat dissipation property are advantageous for coatings on electrical wires to eliminate conductive heat.
2.2. GrapheneMetal Nanoparticle Composites

The attractive properties of graphene and its derivatives have made them ideal templates for the synthesis
of metal nanoparticles (NPs), such as Au,[81,87,118,334359]
Ag,[81,360362] Pd,[165,334,341,349,363368] Pt,[118,334,369] Ni,[370] and
Cu.[341] Dependent on the type of the anchored NPs, the
graphenemetal NP composites have been applied in a
broad range of areas, such as surface-enhanced Raman scattering (SERS),[81,337] catalysis,[349,363] and electrochemical
sensing.[119,348,371373] The graphenemetal NP composites can
be prepared by chemical reduction,[334,336,339,373,374] photochemical synthesis,[87,98] microwave assisted synthesis,[341]
electroless metallization,[81] and thermal evaporation.[375]
One of the most straightforward approaches to prepare
graphenemetal NP composites is the direct chemical reduction of the metal precursors in the presence of GO or rGO
suspensions. The GO and rGO sheets possess defects and
residual oxygenated functional groups, which can act as the
nucleation sites for the growth of metallic nanostructures. The
first grapheneAu NP composite was prepared by the reduction of AuCl4 with NaBH4 in a rGO octadecylamine (ODA)
solution.[339] The ODA functionalization of rGO offers good
solubility to the composites in low-polarity solvents, e.g.,
THF. In addition to Au NPs, Pd NPs supported on GO were
prepared by bubbling hydrogen through a suspension of
Pd2+GO in ethanol, and the obtained composites were used
as catalysts in the SuzukiMiyaura coupling reaction.[349] The
pd/GO and pd/rGO composites exhibited higher catalytic
activities compared to conventional Pd/carbon catalysts, with
turnover frequencies exceeding 39 000 h1, accompanied by
very low Pd leaching (<1 ppm).
To impart better solubility and thus improved processibility of graphenemetal NP composites in polar solvents,
after GO sheets were functionalized with 3,4,9,10-perylene
tetracarboxylic acid (PTCA) and reduced to rGO with
hydrazine, Au NPs were deposited on rGO by the reduction
of HAuCl4 with amino-terminated ionic liquid (IL-NH2).
The resulting composites were water-soluble with welldistributed Au NPs with a high surface coverage, which could
be attributed to the presence of additional carboxylic acid

groups from PTCA.[340]
In addition to spherical metal NPs obtained in most
reported syntheses, Au nanorods have been successfully prepared on rGO films,[336,374] which were immersed in growth
solutions of cetyl trimethylammonium bromide (CTAB),
HAuCl4, and ascorbic acid. It was found that the growth
of Au nanorods could be realized on both rGO and seedmodified rGO films.[374] The fabricated Au nanorods give significantly enhanced Raman signals of rGO34 times higher
at the rod tip,[374] which is much higher than that of snowflake-shaped Au structures deposited on rGO.[335]
Recently, by using GO as template, for the first time, our
group has synthesized dispersible Au square sheets, which
are exclusively hexagonal close-packed (hcp) and stable
under ambient conditions. The hcp Au square sheet exhibited an edge length of 200500 nm and a thickness of ~2.4 nm
(~16 Au atomic layers).[359] The properties of this unique Au
nanostructure are currently under investigation.
In addition to the single-phase metal NPs, bimetallic
NPs supported on graphene sheets were prepared in a seedmediated sequential approach. For example, after Pd seeds
were formed on graphene by reducing H2PdCl4 using
HCOOH, Pt nanodendrites were epitaxially grown on the Pd
seeds by further reduction of K2PtCl4 with ascorbic acid.[373]
The prepared graphene/bimetallic dendrite composites exhibit
higher electyrocatalytic activity toward methanol oxidation
than platinum black (PB) or commercial E-TEK Pt/C catalysts. The enhanced performance arises from both the good
electrocatalytic activity of Pt branches supported on Pd cores,
and the highly electrochemically active surface of graphene.
As a green, facile, and efficient synthetic route, photochemical reduction can be applied as a supplement or alternative to the chemical- reagent-based reduction for the
synthesis of graphenemetal NP composites.[87,98] Fluorescent
Au nanodots (NDs) on octadecyl thiol (ODT)-coated rGO
sheets were synthesized by the photochemical reduction of
HAuCl4 in ethanol.[87] These Au NDs self-assemble into short
ND-chains on rGO surfaces, along the <100> direction of
the rGO lattice (Figure 3A).[87] It is demonstrated that the
organic molecules with self-assembled patterns on graphene
surface can further direct the orientation and arrangement of
the in-situ synthesized NPs.
Other methods, such as microwave- assisted reduction[341]
and electroless metalization,[81] have also been attempted to
prepare graphenemetal NP composites. In the microwave
irradiation method, the formation of metal NPs and the
reduction of GO took place simultaneously, which allows
for large-scale and highly efficient production. Additionally,
this method can be applied to a number of metal precursors,
such as those for Cu, Pd, Au, and Ag.[341] For the electroless
deposition method,[81] Ag NPs were synthesized on GO and
rGO surfaces, by heating the GO or rGO films adsorbed on
3-aminopropyltriethoxysilane (APTES)-modified Si/SiOx
substrates in a AgNO3 aqueous solution, without the use
of any reduction agent and surfactants (Figure 2B).[81] It is
demonstrated that the GO sheets, compared to rGO, facilitate the growth of AgNPs with higher density and smaller
sizes, which can be due to the larger amount of functional
small 2011, 7, No. 14, 18761902
Figure 3. A) Transmission electron microscopy (TEM) image of ODT-capped Au NDs synthesized in situ and assembled on a rGO surface. Inset of
(A) is a high-resolution TEM image of an Au ND. Reproduced with permission.[87] B) Scanning electron microscopy (SEM) image of Ag NPs densely
grown on GO sheets. Reproduced with permission.[81] Copyright 2009, American Chemical Society. C) Au NPs on monolayer, bilayer, and trilayer
graphene, respectively. D) Statistics of the size and density of Au NPs on n-layer graphenes. Reproduced with permission.[375] Copyright 2010,
American Chemical Society.
groups present in GO compared to rGO. Similar phenomenon is also reported in the GO/rGO templated growth of
Ni nanocrystals, where the higher degree of oxidation of
graphene sheets has led to larger nucleation density of Ni
NPs.[370]
As discussed above, the surface chemistry of chemically modified graphene can affect the nucleation density of
anchored metal NPs,[81] whereas the lattice atomic structure
of rGO can direct the assembly and pattern formation of
Au NDs.[87] In addition to these observations, the number of
pristine graphene layers also showed a direct impact on the
particle size and density of thermally evaporated Au NPs,[375]
i.e., the particle size decreased and density increased with
increasing layer numbers of the graphene film (Figure 3C,D).
Two factors have been considered to cause this interesting
phenomenon. First, the surface free energy of graphene is
dependent on the layer number, which controls the interaction between graphene and the evaporated Au atoms.
Second, the diffusion coefficient of Au atoms varies on different surfaces, which determines the outcome of the competition between nucleation and growth of the Au islands.[375]
It is also suggested that, the different densities and sizes of
NPs observed in SEM could be used to identify the layer
numbers of graphene, which might give an alternative to
small 2011, 7, No. 14, 18761902
the identification method based on atomic force microscopy

(AFM) measurements.
2.3. GrapheneSemiconductor Nanomaterial Composites

There is great demand for the synthesis of graphene
semiconductor nanomaterial composites because of their
promise in electronics, optics, and energy-based applications
such as solar cells, Li-ion batteries, and supercapacitors. To
date, various kinds of semiconductor nanomaterials have been
synthesized and supported on graphene-based templates,
which include TiO2,[88,122,251,253,254,256,376386] ZnO,[78,80,387391]
SnO2,[392397] MnO2,[398401] Co3O4,[402406] Fe3O4,[407417]
NiO,[221]
Cu2O,[78,79,420]
RuO2,[421,422]
Fe2O3,[418,419]
CdS,[238,245,423428] and CdSe.[100,429432] The synthetic methods
for preparation of these graphenesemiconductor nanomaterial composites include in-situ crystallization,[378,380,424]
solution mixing,[256,376,404] microwave-assisted growth,[400,402]
electrochemical deposition,[78,80,429] and vapor deposition.[221]
The in-situ crystallization approach has been considered
as one of the most commonly used methods to synthesize
composites of GO or rGO and semiconductor nanomaterials. For example, grapheneCdS composites were prepared
1883
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X. Huang et al.
by mixing GO and Cd(CH3COO)2 in DMSO, which was

then heated in an autoclave at 180 C for 12 h.[424] During
the synthetic process, the hydrothermal process results in the
simultaneous formation of CdS nanoparticles (NPs) and the
reduction of GO to rGO in DMSO, which acts as both
the solvent and the sulfur source. Time-resolved fluorescence
spectroscopy data showed a picosecond ultrafast electron transfer process from CdS NPs to the graphene sheet,
which demonstrates the potential optoelectronic application of this grapheneCdS hybrid material. In another work,
grapheneCo3O4 hybrid material was synthesized by reacting
Co(NO3)26H2O and ammonia solution in the presence of
GO sheets, followed by drying and heating at 450C to result
in the Co3O4graphene composite used for the Li ion battery application.[403] The in-situ crystallization approach is
also applicable to synthesis of many other types of semiconductor nanostructures on graphene-based templates such
as MnO2 nanoneedles,[398] TiO2 rods,[380] and SnO2 NPs.[433]
Alternatively, the in-situ microwave irradiation offers a
fast and easy way to synthesize graphenesemiconductor
NP composites, which has been applied to prepare graphene
MnO2 NPs[400] and grapheneCo3O4 NPs.[402] For example,
after a water suspension of rGO was mixed with potassium permanganate powders by ultrasonication, the mixture was heated in a household microwave oven for only
5 min to obtain the grapheneMnO2 NP composites.[400]
Another efficient and direct means to prepare graphene
semiconductor NP composites is the solution mixing
approach.[256,376,379,404] For example, commercialized TiO2
NPs (P25) were mixed with Nafion-coated graphene to fabricate dye-sensitized solar cells, where the Nafion served as a
glue to tightly bind graphene sheets and NPs.[379] In another
example, after the pre-synthesized CdS NPs were functionalized with benzyl mercaptan molecules and then mixed with
rGO sheets, the benzyl mercaptan-capped CdS NPs absorbed
on rGO surfaces through interactions.[423] However, in
some cases the pre-synthesized NPs from an organic synthetic
route are not compatible with the aqueous dispersion of GO
sheets. In order to solve this problem, a two-phase approach
was developed to prepare grapheneTiO2 composites. For
example, after a solution of oleic acid-capped TiO2 nanorods
in toluene was mixed with GO water suspension and stirred
for 24 h, the TiO2 nanorods were able to assemble on the GO
surface at the water/toluene interface.[256]
Very recently, a novel strategy used to prepare grapheneencapsulated metal oxides hybrids has been developed. In
this work, after the negatively charged GO sheets wrapped
around the positively charged Co3O4 NPs (modified by aminopropyltrimethoxysilane, APS) through the electrostatic
interaction, GO was chemically reduced to rGO. The obtained
composites were successfully used for the Li ion battery
application (Figure 4AC).[404] This approach is essentially
important for the preparation of graphenemetal oxide NP
composites as anode materials for lithium ion storage due to
the following reasons. First, the graphene encapsulation can
suppress the aggregation of oxide NPs during the charge
discharge process. Second, it gives rise to high oxide content
in the composites (91.5 wt%). Third, an overall high electroconductivity of the composite is maintained by the graphene
Figure 4. A) Schematic illustration of fabrication of grapheneencapsulated metal oxide NPs. B) Typical SEM image of grapheneencapsulated Co3O4. C) Cycle performance of graphene-encapsulated
Co3O4. Reproduced with permission.[404]
network. Consequently, the anode made from the graphene

Co3O4 NP composites showed a very high reversible capacity
of 1100 mA h g1 in the first 10 cycles, and over 1000 mA h g1
after 130 cycles (Figure 4C).
Thin-film-based applications require postsynthetic deposition of the composite materials on substrates by techniques
such as spin-coating, drop casting, and transfer printing.
Therefore, the direct electrochemical deposition of NPs on
graphene-based substrates is an attractive approach to prepare certain types of graphenesemiconductor nanomaterial
hybrid films, for example, ZnO, Cu2O, and CdSe.[78,80,429] For
instance, ZnO nanorods were deposited on spin-coated rGO
thin films on quartz, using an oxygen-saturated aqueous solution of ZnCl2 and KCl as the electrolyte.[80] It is found that
the crystal quality of the deposited ZnO nanorods depends
on the thickness of the rGO thin films. For example, the thick
rGO film electrode with low resistivity gives better quality
of the deposited ZnO nanorods. This method has also been
applied to deposit Cu2O nanostructures on rGO films, spincoated on flexible polyethylene terephthalate (PET) substrates.[78] Different from the random deposition of ZnO
and Cu2O on rGO films, the ordered CdSe NP patterns on
graphene films were realized through a templated electrochemical process.[429] In this work, after graphene was epitaxially grown on Ni film, a layer of mesoporous silica film was
formed on the graphene sheets via a solgel process. Then
CdSe NPs were electrochemically deposited on the graphene
surface through the precoated porous silica film. This work
demonstrates a ligand-free process for the pattern formation
small 2011, 7, No. 14, 18761902
of NPs on graphene sheets, without affecting the combined

electronic properties of the semiconductor NPs and the
graphene layers.
3. Applications of Graphene and

3.1. Field-Effect Transistors
2.4. Other Graphene-Based Composites

It has been demonstrated that graphene-based materials
are able to wrap around organic nanowires to form core
shell wire structures.[242,434] Many small organic molecules,
e.g., N,N-dioctyl-3,4,9,10-perylenedicarboximide (PDI), are
able to self-assemble via noncovalent interactions to form
nanostructures with distinctive morphologies. For example,
by using GO as an atomic template and structural scaffold
in the nucleation and assembly of PDI molecules, PDIGO
coreshell wires were formed through interactions.[242]
The obtained organic hybrid structure outperformed its
individual components in donoracceptor-type solar cells.
Graphenepeptide hybrid nanowires were prepared as well,
by mixing an organic peptide solution (diphenylalanine in
1,1,1,3,3,3-hexafluoro-2-propanol) and graphene aqueous
solution with mild shaking.[434] These coreshell structures
were subsequently calcinated to remove the peptide cores,
and gave rise to hollow graphene shells, which could be
applied as supercapacitor electrodes.
Moreover, graphenecarbon nanotube (CNT) composites have been prepared and applied in transparent conductors,[435] Li ion batteries,[436] and supercapacitors.[437,438]
Despite its low cost and availability for large-scale synthesis,
the chemically converted graphene (CCG) or rGO suffers
from the defects and oxygen groups, leading to worse electronic properties compared to pristine graphene. Hence,
the combination of rGO and CNT in a transparent conductor has shown the expected enhancement in film conductivity.[435] Another advantage of grapheneCNT composites
lies in the fact that the basal spacing between the graphene
layers can be enlarged with CNT spacers, which benefits the
storage capacity of Li ions forbattery-based applications.[436]
In order to extend the advantage of CNT spacers, a 3D
CNT/graphene sandwiched (CGS) structure with CNT pillars grown between the graphene layers was developed via
a CVD process.[438] The supercapacitor based on the CGS
composites exhibits a specific capacitance of 385 F g1 at
10 mV s in 6 m KOH solution. The significantly enhanced
electrochemical performance of CGS could be due to the
following reasons. First, the walls of the CNTs can act as a
structural buffer for the large volume expansion of catalyst particles during the redox reaction. Second, the CNTs
can provide an additional diffusion path on the surface of
graphene, which facilitates the diffusion and migration of
electrolyte ions during the rapid chargedischarge processes.
Third, the interconnection of CNTs with graphene maintains a conductive network for the transport of electrons.
Recently, using GO as the only carbon source, our group has
successfully prepared novel rGO/carbon nanowire (CNW)
composites by a simple, one-step annealing process.[132] As a
proof of concept, the micropatterned rGO/CNW composites,
used as channel materials for FETs, exhibit excellent sensing
properties in detection of dopamine.
small 2011, 7, No. 14, 18761902
One of the most extensively explored applications

of graphene is the field-effect transistor (FET). The first
graphene-based FET was reported by Novoselov et al. in
2004,[18] where single- and few-layer graphene (FLG) with
sizes up to 10 m was obtained by mechanical exfoliation of
highly oriented pyrolytic graphite (HOPG). 2D FLG behaves
with metallic characteristics and exhibits a strong ambipolar electric field effect. The pristine graphene could not
be used for the fabrication of effective FET devices because
the onoff current ratio (Ion/Ioff < 30 at 300 K)[18] is quite
low due to its zero bandgap. Later the top-gate graphene
FET was fabricated and the saturating transistor characteristics were observed.[188] The saturation velocity depends on
the charge-carrier concentration which is attributed to scattering by interfacial phonons in the SiO2 layer which supports the graphene channel. The electrostatic modulation of
the channel through an efficiently coupled top-gate yields the
transconductance as high as 150 S m1. These results demonstrate the feasibility of such graphene devices for analogue
and radio-frequency circuit applications where bandgap engineering/opening is unnecessary.
In order to improve the onoff current ratio for effective
transistor applications, graphene structures with narrow widths
and atomically smooth edges, termed graphene nanoribbons
(GNRs), have been intensively studied both theoretically
and experimentally.[5,169172,177,439440] Generally, four methods
have been reported to fabricate GNRs as summarized in
Table 1. Among these methods, the oxygen plasma etching
with electron-beam-generated etch mask has realized the
fabrication of GNRs with widths ranging from 15 to 100 nm.
The largest energy gap of 200 meV is achieved in the thinnest 15 nm wide GNRs[170] because the lateral confinement
of charge carriers creates an energy gap near the charge
neutrality point and the band-gap scales inversely with the
ribbon width. Other methods, such as directly unzipping
multiwalled carbon nanotubes (MWCNTs)[177] and oxygen
plasma etching templated with dielectric nanowires,[169]
have been subsequently demonstrated. However, the reduction in ribbon width based on these methods is restricted to
the dimension of the MWCNTs or the etch masks, and the
resulting bandgap opening and onoff ratio from the corresponding transistors are small. In order to realize sub-10-nm
wide GNRs, a chemical route was developed to prepare
solution-phase-derived, stable suspensions of GNRs with
noncovalent polymer functionalization.[5] GNRs based on
this method exhibited ultrasmooth edges with possibly welldefined zigzag or armchair-edged structures. Electrical transport experiments showed that all of the sub-10-nm GNRs
were semiconductors and afforded graphene FETs with
onoff ratio of 107 at room temperature.[5]
Although GNRs have shown semiconductor properties due to the bandgap opening of graphene, the practical
devices and circuits often require high driving current or
1885
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X. Huang et al.
graphene oxide (GO),[223,441] graphene

Au hybrid systems,[104] graphenepolymer
composites,[218] and rGO-electrodes.[219,220]
Current References
In the graphene-based nonvolaonoff
tile memory device with ferroelectric
ratio
gating,[217] the binary information, i.e., high
N.A.
[170]
and low resistance states of the graphene
working channel, can be switched by controlling the polarization of the ferroelectric thin film induced by the electrostatic
12
[169]
doping of graphene. In the case of GObased memory devices, the properties of
desorption/absorption of oxygenated func7
[5]
10
tional groups on the GO sheets[441] and
the unique charge trapping properties of
GO[223] have enabled the switching effect
with the threshold voltage of 1 and 1.4 V,
>100
[177]
respectively.[223,441]
Thanks to the feasibility of large-area
production of rGO films, the fabrication
of both conductivity- and type-switching memory devices
has been successfully demonstrated in a rGO/Au NP hybrid
system (Figure 6).[104] The real-time type-switching of the carrier types in the rGO-FETs can be controlled by applying a
gate bias to adjust the charges in the Au NPs, thus in turn
Table 1. Comparison of methods used for generation of GNRs and the resulting onoff
current ratio obtained from the GNR-based FETs.
Methods for
preparation
of graphene
Methods for
Width of graphene
Maximum
generation of
nanoribbons
bandgap opening
graphene nanoribbons
[nm]
[meV]
Mechanically
peeled from
graphite
crystals
Oxygen plasma with

e-beam lithography
generated resist
pattern as etch mask
15
200
Mechanically
peeled from
graphite crystals
Oxygen plasma with

dielectric nanowire as
etch mask
15
N.A.
Exfoliation plus
ultrasonication
based on
expandable graphite
Chemical
derivation
400
Unzipping multiwall
carbon nanotubes
Plasma etching
N.A.
transconductance. Therefore, a dense array of ordered nanoribbons is desirable, which, however, remains a significant
challenge. Alternatively, another type of graphene nanostructures, called graphene nanomesh (GNM)[182,183] or nanoperforated graphene,[184] was developed, which not only opens
the bandgap of graphene but also provides
high driving current. With block copolymer
lithography, the fabricated GNMs could
have variable periodicities with a neck
width as small as 5 nm. The FETs fabricated with GNM as the channel material,
referred to as GNM-FETs, can support
currents 100 times greater than individual
GNR devices, while the onoff ratio, which
can be tuned by varying the neck width,
is comparable with that achieved in individual GNR devices (Figure 5). Additionally, the block copolymer lithography is
scalable, and allows for the rational design
and fabrication of GNM-FET devices with
standard semiconductor processing.
3.2. Memory Devices
Graphene-related
materials
have
also been widely explored in memory
devices.[222] It was demonstrated theoretically by Gunlycke et al. that when
the graphene nanostrips are under a
non-equilibrium state, e.g., in the presence of a ballistic current, both spinpolarized and spin-unpolarized nanostrip
states exist, which could be switched
through the applied bias in a binary
memory device. After that, extensive
experimental investigations on graphenerelated memory devices were carried
out, based on pristine graphene,[217]
Figure 5. A) Schematic of a GNM-FET. B) Drain current (Id) versus drainsource voltage (Vd),
recorded at different gate voltages for a GNM device with a channel width of 2 mm and
channel length of 1 mm. The on-state conductance at Vg = 10 V is comparable to an array
of 100 parallel GNR devices. C) Transfer characteristics for the device in B at Vd = 210, 2100,
and 2500 mV. The ratio between Ion and Ioff for this device is 14 at Vd = 2100 mV. D) Transfer
characteristics at Vd = 2100 mV for GNMs with different estimated neck widths of 15 nm
(device channel width 6.5 m and length 3.6 m), 10 nm (channel width 2 mm and length
1 mm), and 7 nm (channel width 3 mm and length 2.3 mm). Reproduced with permission.[182]
Copyright 2010, Nature Publishing Group.
small 2011, 7, No. 14, 18761902
memory device exhibits a high onoff ratio

(104105) and low switching threshold
voltage (0.51.2 V), which are related to the
sheet resistance of the rGO electrode. The
rGO films in this work are prepared from
the thermal reduction of GO at 1000 C.
We have also developed a method to fabricate highly reduced GO films by chemical reduction with smeared hydrazine at
low temperature (e.g., 100 C) combined
with a multilayer stacking technique.[85]
The resulting rGO films show a low sheet
resistance of 160500 sq1. By using
them as the electrodes in memory devices
with a configuration of rGO/P3HT:PCBM/
Al, a high onoff current ratio of up to106
is achieved.
3.3. Photovoltaic Devices

Owing to its good electronic conductivity, optical transparency, and large
specific surface area, graphene-based
materials have been extensively explored
in the field of photovoltaics. Until now,
lots of studies on graphene-based photovoltaic applications have been reported, in
which graphene-based materials are used
as the transparent electrodes,[23,80,105,234,244,248,435,442] electron
acceptor,[161,237238,246,376,378379] and light absorber.[161]
Figure 6. A) Operation principle of type-switching memory device. B) Typical hysteresis

curve of type-switching memory device based on GO and NPs. It exhibited both n-type and
p-type characteristics near zero gate bias voltage. C) Real-time switching of the reduced GO
channel type. After applying a large positive (or negative) top-gate bias, a small back-gate
bias was used to confirm the p-type (or n-type) behavior of the channel. D) Switching the
inverter functionality by using a transistor that consisted of graphene and NPs. Reproduced
with permission.[104]
affecting the charges in the FET channel. Importantly, such

type-switching behavior of the rGO-based devices is successfully applied to build the reconfigurable inverter logic gates
by controlling the charges in the Au NPs.[104]
Graphenepolymer composites have been investigated
in memory devices as well, through a reliable and low-cost
synthetic route.[218] As reported, GO was modified by a
conjugated-polymer of triphenylamine-based polyazomethine (TPAPAM), and then incorporated into a nonvolatile memory device. This device exhibits a typically bistable
electrical switching and nonvolatile rewritable memory
effect. An onoff current ratio of more than 103 is achieved.
Under application of a constant voltage stress, both
the on and off states from such TPAPAMGO-based
memory device are stable up to 108 read cycles at a read
voltage of 1.0 V.
The use of indium tin oxide (ITO) and some metal
materials as electrodes in memory devices has been limited
because of their brittle nature, high cost, and insufficient element resources. Consequently, the memory device based on
polymer composites of poly(3-hexyl thiophene) (P3HT) and
methanofullerene [6,6]-phenyl C61-butyric acid methyl ester
(PCBM) bulk-heterojunction (BHJ) on rGO film electrode
has been developed in our group.[86] The currentvoltage
(IV) curves from this rGO/P3HT:PCBM/Al memory show
the electrical bistable behavior, a write-once-read-manytimes (WORM) memory effect. The carrier transport mechanism related to the conductivity-switching is affected by the
polarization of PCBM domains and the formation of a localized internal electrical field among the adjacent domains. The
small 2011, 7, No. 14, 18761902
3.3.1. Transparent Electrodes

Graphene-based transparent electrodes are mainly employed
in three types of photovoltaic devices: organic,[23,105,244,435,442]
inorganicorganic hybrid,[80] and dye-sensitized solar cells.[234]
In the organic photovoltaic (OPV) solar cells, the highest
power conversion efficiency (PCE, ) of 1.71% has been
reported based on the use of large-area, continuous, transparent, and highly conducting few-layer graphene films
deposited by the CVD process.[244] The good performance is
attributed to the noncovalent modification of the graphene
films with pyrene buanoic acid succidymidyl ester. In another
report, CVD-deposited-graphene is successfully transferred
onto a flexible PET substrate for fabrication of OPV devices.
It is worth noting that the graphene/PET-based and ITO/PETbased OPV devices showed comparable performances with an
of 1.18 and 1.27%, respectively.[23] Importantly, the CVDgrown graphene-based solar cells show outstanding capability
to be operated under bending conditions with bending angles
up to 138, while the ITO-based devices display cracks and
irreversible failure under bending of only 60. Therefore, the
epitaxially grown graphene used as a highly flexible, transparent,
and continuous electrodes for OPVs presents itself as a potential replacement for ITO in flexible photovoltaic applications.
As an alternative to CVD-grown graphene, rGO film has
been used as transparent electrode as well.[80] In this study,
ZnO film is electrochemically deposited on the rGO electrode
1887
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and subsequently incorporated to a hybrid solar cell based on a

ZnOP3HT system. The PCE of the inorganicorganic hybrid
solar cell with a layered structure of quartz/rGO/ZnO NR/
P3HT/PEDOT:PSS/Au (PEDOT:PSS = poly(3,4-ethylenediox
ythiophene):poly(styrenesulfonate)) is around 0.31% (Device
II in Figure 7A). The rGO film with a higher conductivity
after thermal annealing gives a higher work function, which is
changed from 5.0 to 4.7 eV. It results in a better matching
between the conduction band of ZnO and Fermi level of rGO,
thus improving the performance of the fabricated hybrid solar
cells. In addition, the chemically derived rGO films have been
transferred onto PET substrates, used as transparent and flexible electrodes in OPV devices,[84] with a configuration of rGO/
PEDOT:PSS/P3HT:PCBM/TiO2/Al. Importantly, we found that
when the optical transmittance of rGO is above 65%, the performance of the OPV devices mainly depends on the charge
transport efficiency through the rGO electrodes, whereas if the
transmittance is less than 65%, the performance of the devices
is dominated by the light transmission efficiency.
In addition to OPV devices, graphene has been used
as the transparent electrode for dye-sensitized solar cells
(DSSCs).[234] A graphene thin film, prepared by dip coating in
a hot, aqueous GO dispersion followed by thermal reduction,
exhibits a high conductivity of 550 S/cm and a transparency
of more than 70% over the 10003000 nm range. It was used
to fabricate a solid-state graphene/TiO2/dye/spiro-OMeTAD/
Au device (Spiro-OMeTAD = 2,2,7,7-tetrakis(N,N-di-pmethoxyphenilamine)-9,9-spirobifluorene) (Figure 7B). This
is the first demonstration of a solid-state DSSC based on a
graphene electrode; however the PCE (0.26%) of this device
is lower than that (0.84%) of the corresponding fluorine tin
oxide (FTO)-based solid-state DSSC.
3.3.2. Electron Acceptors
Graphene has emerged as a new electron-accepting material in photovoltaic device applications because of its unique
2D structure and high electron mobility. To date, to the best

of our knowledge, graphene-based materials that have been
used as an electron acceptor in photovoltaic devices include
functionalized graphene,[237] a grapheneTiO2 composite,[376]
and a layered graphenequantum dot hybrid.[238]
In order to fabricate functionalized graphene-based
photovoltaic devices, GO sheets were first reacted with
phenyl isocyanate to change their surfaces from hydrophilic
to hydrophobic. The resulting solution-processed functionalized graphene (SPFGraphene) was then mixed with poly(3octylthiophene) (P3OT) to form the P3OT/SPFGraphene
composite, which was used as the active layer in the bulk
heterojunction (BHJ) OPV device.[237] After optimizing the
annealing process (160 C for 20 min) for the fabricated OPV
device, the best PCE of 1.4% was obtained. This work suggests the promises of SPFGraphene materials to serve as a
competitive alternative to PCBM as the electron acceptor for
high-performance OPV devices.
The grapheneTiO2 composite, as another type of effective electron acceptor, has been used as the photoanode in
DSSCs.[376] In fabricated DSSCs, the graphene works as a
bridge which could enhance the charge transport rate to prevent the charge recombination and increase the light collection efficiency, thus improving the photoelectrical conversion
efficiency of DSSCs. Compared with pure TiO2 photoanodebased DSSCs, the short-circuit current density for the
grapheneTiO2 photoanode based device is increased by
45%, without sacrificing the open-circuit voltage. As a result,
the total conversion efficiency is measured as 6.97%, which
shows a 39% increase compared to that of pure TiO2-based
DSSCs.
A simple bottom-up approach, i.e., the electrophoretic
deposition of graphene layers followed by the chemical
bath deposition of a CdSe quantum dot (QD) layer, is
used to create a novel graphene/CdS-QD bilayer structure,
which works as the electron transfer system in photovoltaic
devices.[238] The best performance with a PCE of 16% is
obtained from the photovoltaic device
fabricated with eight repeated graphene/
CdS-QD bilayers. In this work, the significantly improved photoresponse, especially
the photocurrent, suggests that graphene
is a good candidate for the collection and
transport of photogenerated charges.
3.3.3. Light Absorbers
Figure 7. A) Under simulated globe sun illumination, the obtained IV curves for ZnO/P3HT
hybrid solar cells by using I) one-step and II) two step reduced GO films as electrodes. Inset:
schematic illustration of the fabricated solar cell. Reproduced with permission.[80] B) Top:
illustration of dye-sensitized solar cell using graphene film as electrode. The four layers
from bottom to top are Au, dye-sensitized heterojunction, compact TiO2, and graphene film.
Bottom: IV curve of graphene-based cell (black) and the FTO-based cell (grey), illuminated
under AM solar light (1 sun). Reproduced with permission.[234] Copyright 2008, American
Chemical Society.
The tunable bandgap and large optical

absorptivity of graphene are appealing
characteristics for the efficient light harvesting. By using small organic compounds,
graphene QDs that contain 168 conjugated carbon atoms have been synthesized
via a stepwise solution-based chemical
route.[161] The uniform-sized graphene
QDs are made highly soluble after their
edges are covalently reacted with 1,3,5trialkyl phenyl moieties. This novel solubilization strategy enables the QDs to act
small 2011, 7, No. 14, 18761902
as light absorbers (sensitizers) and to replace the traditionally used ruthenium complexes in nanocrystalline TiO2 solar
cells. However, the resulting energy conversion performance is not high, which requires improvement by covalently
binding functional groups to the QDs for higher charge injection, or optimizing the preparation procedure for the electrode. Nevertheless, this solubilization strategy opens exciting
opportunities to tune the optical and electronic properties of
graphene for photovoltaics.
3.4. Sensing Platforms

3.4.1. FET Sensors
Chemical and biological sensors based on graphene
(or graphene derivatives) field-effect transistors (GFETs)
are receiving continuous interest due to their high sensitivity,[258] low noise,[19,20,258] facile fabrication, and biocompatible nature.[83,443] Gas sensors based on GFET have shown
promising results, even being able to detect the absorption
of a single gas molecule.[258] Recently, several groups have
reported GFET-based biosensors, which include the detection of biomolecules such as DNA[444] and protein,[94,445] and
biosignals arose from the interaction between graphene and
bacteria[446] or cells.[75,447]
In a typical GFET-based sensor, graphene is used as conducting channel between drain and source electrodes. Gate
potential is applied through back-gate (typical SiO2 thin
layer) or top-gate (electric double layer in electrolyte) for gas
and biosensing, respectively. The absorption of analyte molecules or change of local environment leads to the change of
its electrical conductance.
The first gas sensor based on GFET was prepared by using
mechanically exfoliated graphene as the channel material.[258]
An outstanding single-molecule-detection limit is achieved.
Such excellent performance is attributed to the high carrier

mobility of graphene[1819] and the resulting extremely low
noise.[1920]
By electrochemical gating through the top gate, GFET
is readily configured as a biosensor in physiological buffer
solution. It has been shown that GFET is sensitive to the pH
value of an electrolyte,[448] and is able to detect protein in the
nanomolar scale in bovine serum albumin (PBS) buffer.[445]
Recently, the Lieber group reported that compared to a
nanowire-based sensor, GFET gave competitive performance for recording bioelectrical signals from living cells.[447]
Besides the mechanically exfoliated graphene, the epitaxially
grown graphene is also used as the channel material, which is
able to detect DNA with single-base-mismatch sensitivity.[444]
Reduced graphene oxide (rGO), prepared from chemical
or thermal reduction of chemical derived GO, is a promising substitute for pristine graphene as a channel material
due to its low cost and large-scale production. For example,
a GFET sensor is used for the detection of chemical warfare
agents and explosives at a sensitivity in the part-per-billion
(ppb) level based on rGO thin films, which are fabricated by
spin-coating GO sheets on a Si/SiOx substrate, followed by
subsequent chemical reduction.[108] In another example, a
flexible GEFT sensor, fabricated by ink-jet-printed rGO films
on PET), is used to detect NO2 and Cl2 vapors with an air
sample at the ppb level.[116] Recently, our group reported a
flexible GFET sensor using a micopatterned rGO thin film as
the channel material to detect chemicals, metal ions and proteins.[75] Moreover, such a sensor is able to detect hormonal
catecholamine molecules and their dynamic secretion from
living cells in physiological buffer solution.[75]a] As shown
in Figure 8, neuron cells (PC12) are directly cultured on a
relatively long channel (1 cm) of rGO thin film. The source
drain current is continuously monitored to detect the secretion of catecholamine molecules by PC12 cells in the high K+
solution.[75a]
Figure 8. A) Schematic illustration of the experimental setup of front-gate GFET for sensing application. B) Schematic illustration of the interface
between a PC12 cell and GFET. C) Real-time response of rGO/PET FET to the vesicular secretion of catecholamines from PC12 cells stimulated by
high K+ solution. Reproduced with permission.[75a] Copyright 2010, American Chemical Society.
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A hybrid material of rGO and Au NPantibody conjugates has also been employed as the channel material for
protein detection.[94] The target protein immunoglobulin G
(IgG) interacts specifically with the anti-IgG-conjugated Au
NPs, resulting in the change of electrical characteristics of the
device. A detection limit of 2 ng/mL IgG is achieved, which
is among the lowest detection limit for carbon-nanomaterialbased sensors.
3.4.2. Electrochemical Sensors
Graphene-based materials possess large specific surface area, excellent conductivity, and availability for surface functionalization, which are important characteristics
in the electrochemical applications.[449] Until now, many
graphene-based electrochemical sensors have been reported
to detect glucose,[119,265,344,348,371,450460] ascorbic acid,[461463]
dopamine,[462470] H2O2,[343,372] DNA,[257] DNA bases,[259] and
antigen.[471] It has been shown that graphene and graphenebased materials are promising supplements or replacements
for conventional carbon materials, such as carbon nanotubes
and graphite.[472] Even superior performance of graphenebased electrochemical sensors compared to carbon nanotubes has been reported, which is attributed to the presence
of more sp2-like planes and edge defects in graphene.[462,464]
In a typical set up of electrochemical sensing, a graphene
thin film is used as the electrode.[462,466] For example, the
epitaxially grown graphene is prepared on a silicon carbide
substrate by the CVD process, and then incorporated as the
working electrode in a three-electrode electrochemical cell.
Anodization is used to generate oxygenated groups on the
surface of graphene. It is shown that the resulting sensing
platform exhibits good detection ability towards nucleic acids,
uric acids, dopamine, and ascorbic acid, as well as to differentiate single-stranded DNA from double-stranded DNA.[466]
In another report, by using a microwave plasma-enhanced
CVD method, graphene nanoflakes are grown on silicon substrates, which are used to simultaneously detect dopamine,
ascorbic acide, and uric acide. The graphene flakes process
abundant graphitic edge planes and defects, which are essentially responsible for the fast electron transfer and good electrocatalytic activity observed in this work.[462]
In addition to the direct use of graphene as the working
electrode, graphene or graphene derivatives have been
used to modify the conventional glassy carbon electrode[119,257,265,451,465] and Au electrode.[259] The glassy carbon
electrode is usually functionalized with APTES, which contains the positively charged amine groups to absorb GO
sheets. The adsorbed GO sheets, electrochemically reduced to
rGO, are further modified with, for example, glucose oxidase
(GOx) used for glucose detection.[119] Recently, we have used
rGO-modified glassy carbon electrode to detect methicillinresistant Staphylococcus aureus (MRSA) DNA by using the
electrochemical impedance spectroscopy. The detection limit
of 100 fm for MRSA DNA is achieved.[257] The modification
of glass carbon electrode can also be carried out by directly
drop-casting a rGO suspension[451] or a mixed slurry of rGO
solution and polymer (e.g., chitosan) on the electrode surface.[265] In the latter case, the rGO is further treated with
nitrogen plasma. The obtained N-doped rGO results in high

electrocatalytic activity for H2O2 reduction, fast electron
transfer for glucose oxidase, and a low glucose detection limit
(0.01 mm). In another approach, pyrene-grafted poly(acrylic
acid) (PAA) modified-graphene sheets are deposited alternatively with poly(ethyleneimine) (PEI) on a glassy carbon
electrode via an LbL assembly approach.[452] The obtained
multilayer graphenepolymer films display enhanced electron transfer and excellent electrocatalytic activity for H2O2.
The surface modification of Au electrode is realized
with thiol-terminated molecules, e.g., n-octadecylmercaptan
(C18H37SH), which are used to adsorb graphene sheets via the
noncovalent interaction.[259] In this report, the heterogeneous
electron transfer blocked by the thiol molecules have been
restored by graphene sheets, and the graphene-modified Au
electrode gives a smaller interfacial capacitance compared
with the pure Au electrode.
In order to take advantages of the good catalytic activity
of noble metal NPs, grapheneNP composites have been
applied in electrochemical sensing.[343,372,471,473] In one of the
attempts, a grapheneAu NP composite is mixed with chitosan solution and used to modify a Au electrode for sensing
H2O2 and O2, which exhibits good electrocatalytical activity.
By further hybridizing this composite with glucose oxidase
(GOD), the graphene/Au NPs/GOD/chitosan electrode
shows excellent response to glucose with a linear range from
2 to 10 mm at 0.2 V.[473] In addition, graphenePt NP is used
to modify glassy carbon electrode, which exhibits superior
detection performance compared to the electrode only modified by graphene, with a wide linear range and low detection limit for H2O2 and trinitrotoluene (TNT).[372] In these
reports, the enhanced performance of graphenemetal NP
composites arise from the excellent electrical conductivity
and high specific surface area of graphene, as well as the
synergistic effect from the graphene and the anchored metal
NPs.[372,473] In addition to using grapheneNP composites to
modify the electrode, nanogold enwrapped graphene nanocomposites (NGGNs) are employed as trace labels in
clinical immunoassays, where horseradish peroxidase (HRP)conjugated anti-carcinoembryonic antigen (CEA) is attached
to the surface of NGGNs, used as the secondary antibodies
for the detection of CEA.[471] Compared to the HRP-antiCEA-nanogold used as the antibody, the graphene-containing
sandwich immunoassay exhibits higher sensitivity and lower
detection limit, which is attributed to the improved electron
transfer between the analyte and the electrode via graphene.
3.4.3. Fluorescence Sensors
Fluorescence-based detection method is sensitive, selective, rapid, and cost-effective in the analysis of biomolecules.
One of the strategies to use graphene in fluorescence-based
bio-detection takes the advantage of graphene's capability in
fluorescence quenching,[261,262,264,474476] induced by the fluorescence resonance energy transfer (FRET).[477] Recently, a
graphene-based DNA and protein sensing platform has been
demonstrated by binding the dye-labeled ssDNA to GO,
which completely quenches the fluorescence of dyes (e.g.,
fluorescein amidite (FAM), a fluorescein-based dye). During
small 2011, 7, No. 14, 18761902
the detection process, a target molecule (i.e., the complementary ssDNA), hybridizes with the dye-labeled DNA to form
dsDNA, leading to restoration of the dye's fluorescence.[475]
The prepared platform is used to detect HIV-1 target DNA
and human thrombin, resulting in good selectivity and sensitivity of the detection. By replacing GO with rGO in a
similarly constructed sensing platform, detection of thrombin
with high sensitivity and excellent specificity is also achieved.
The reported detection limit of 31.3 pm is two orders magnitude lower than that detected by CNT-based florescent
sensors.[264]
In a different approach, GO is complexed with a watersoluble and positively charged organic dye, 4-(1-pyrenylvinyl)-N-butylpyridinium bromide (PNPB), through ion
exchange. The fluorescence of the dye is quenched upon the
formation of PNP+GO complex. The quenched fluorescence
will be turned on, if the dye can interact with an analyte more
strongly than does with GO. Amongst several tested target
molecules, DNA is able to complex with the dye to form the
PNP+DNA complex, and the dye leaves from the GO surface to switch on the fluorescence. But other molecules, such
as RNA, glucose, and proteins, do not show a similar effect.
Therefore, the PNP+GO-based DNA sensing platform is
highly selective over a broad range of common surfactants
and biomolecules.[474]
Another strategy for graphene-based fluorescence sensing
is based on the photoluminescent property of GO itself.[478479]
As reported recently, GO exhibits the near-UV to blue fluorescence,[149,480] which originates from the recombination
of electronhole pairs, localized within the small sp2 carbon
domains embedded in the carbonoxygen sp3 matrix.[149]
Based on this feature of GO, an immune-biosensor system
has been developed. In this work, after GO sheets are patterned on an amino-modified glass surface, antibodies of the
target rotavirus are immobilized on the GO sheets through a
carbodiimide-assisted amidation reaction. At the same time,
an antibody (Ab)-DNA-Au NP complex is synthesized in
solution, which can selectively bind to the target rotavirus
attached to the GO surface (Figure 9AC). Once the binding
event takes place, fluorescence resonance energy transfer

between the Au NP and GO occurs, and the reduction in GO
fluorescence is detected.[478] This selective and sensitive platform can be expanded further to a GO microarray format for
the multiple pathogen analysis.
3.4.4. Matrices for Mass Spectrometry
Laser desorption/ionization mass spectrometry (LDI-MS)

is an important tool for accurate, fast, and sensitive analysis
of biomolecules,[481] organic molecules,[269] and metal clusters.[482] MALDI-TOF MS is one of the most popular types
of LDI-MS, which provides an accurate and easy approach
for high-molecular-mass species.[268,483] However, for lowmass analytes (with a molecular mass of <500 Da), matrix
ion interference and detector saturation are unavoidable in
MALDI-TOF MS, which poses difficulties in the characterization of small molecules. Hence, many substances have been
tested as a matrix to eliminate matrixion interference, such
as porous silicon,[484] graphite particles,[485] and activated
carbon.[486] Graphene, as a novel carbon-based material, has
recently been used as the matrix in MALDI-TOF MS for
the detection of small molecules of amino acids, polyamines,
anticancer drugs, nucleosides, and steroids.[269] Compared
to conventional matrices, e.g., -cyano-4-hydroxycinnamic
acid (CHCA), several advantages of using graphene as the
matrix are demonstrated, which include a lower laser power
threshold for desorption/ionization and a higher signal for
small molecules, simple sample preparation, and eliminated
interference of matrix background ions.[269] In our group,
rGO is used to detect octachlorodibenzo-p-dioxin (OCDD),
a well-known human carcinogen and environmental pollutant. A detection weight of as low as 500 pg is achieved,
whereas conventional organic matrices of 2,5-dihydroxybenzoic acid (DHB), CHCA, and sinapic acid (SA) do not show
observable signals. The superior performance of rGO matrix
arises from the effective desorption/ionization process, which
is facilitated by -conjugated networks of rGO for energy
absorption and electron transfer, and the presence of oxygencontaining functional groups for interaction with the released radicals.[82]
Surface-enhanced laser desorptio/
ionization time-of-flight mass spectrometry (SELDI-TOF-MS) is another type of
LDI-MS. Instead of using a matrix such as
in MALDI-TOF MS, SELDI-TOF-MS utilizes a template for the direct extraction,
amplification, desorption, and ionization of
the analyte.[487] Few-layer graphene sheets
are used as the SELDI analysis platform to
detect ssDNA and other biomolecules.[488]
The DNA strands are able to bind to the
graphene surfaces, via interactions,
Figure 9. A) Illustration of a GO-based immune-biosensor. B) Fluorescence scanning images and evidently, after loading of DNA, the
of a GO immunoarray depend on the number of Au NPs in the Ab-DNA-AuNP complexes,
graphene flakes are able to disperse in
which were synthesized with Au NP/Ab molar ratios of 1:150, 10:150, and 30:150. C) Relative
water. The binding force between DNA and
fluorescence emission intensity compared to the fluorescence intensity of the pristine GO
(F0) when treated with three different Ab-DNA-AuNP complexes. The average quenching graphene favors the desorption/soft ionizaefficiencies were 0.41 for Au/Ab = 1:150, 0.61 for Au/Ab = 10:150, and 0.76 for Au/Ab = tion processes, and thus a detection limit of
30:150. Ab = antibody. Reproduced with permission.[478]
100 fm toward ssDNA is obtained.[488]
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3.5. Patterning of Graphene-Based Materials

There is increasing demand on the fabrication of patterned graphene thin films with well-controlled feature size
and periodicity, and tunable electronic properties, such as
patterned graphene electrodes, arrays of graphene nanoribons (GNRs), and nanomeshes (GNMs). Various methods
have been developed to generate graphene-based patterns,
which include the conventional photolithography,[200,489491]
nanosphere lithography,[492,493] e-beam lithography,[494,495]
direct laser writing,[224] scanning tunneling microscopy
(STM) lithography,[167,496] local anodic oxidation,[497,498] tipbased thermal chemical reduction,[499] dip-pen nanolithography (DPN),[500] microcontact printing,[501,502] plasma etc
hing,[164,166,182,200,490,494] transfer printing,[200,490,503] scratching
method,[76,504] as well as the direct growth of graphene on
prepatterned catalyst substrates.[24,505506]
Conventional photolithography uses light to transfer a
geometric feature from a photo mask to a photoresist film,
which allows for high throughput and good quality control. In a typical experiment, patterned graphene films with
various feature sizes and shapes are fabricated as follows. A
substrate is first modified with a photoresist, e.g., functionalized perfluorophenylazide (PFPA) such as PFPA-silane for
a silicon or glass substrate or PFPAdisulfide for gold films.
Then a suspension of graphene flakes is spin-coated onto the
modified substrate, which is, after drying, subjected to UVirradiation through a photomask. Upon light irradiation, the
azido group on PFPA is converted to the highly reactive singlet perfluorophenylnitrene that can undergo C=C addition
reactions with the adjacent graphene. The subsequent ultrasonication and rinsing processes result in the removal of nonreacted graphene, and the graphene film with desired patterns
is obtained.[489] The photolithography process, based on other
photoresists and lift-off strategies, can be applied to different
graphene- based substrates, such as HOPG[490] and epitaxially grown graphene films.[491] For example, a novel method
is developed to fabricate line patterns of pristine graphene
from HOPG.[490] In this work, after graphene patterns are
made on HOPG by photolithography and O2 plasma etching,
a gold film is deposited on the patterns. Peeling off the gold
film results in the exfoliation of patterned graphene layers
from the bulk HOPG, which can be transferred to other substrates followed by etching away the gold film.
Another conventional means to fabricate patterns for
graphene-based materials is based on the electrostatic
adsorption of the target graphene materials on a patterned
molecular layer. For example, microcontact printing is used
to generate positively charged 11-amino-1-undecanethiol
(AUT) patterns on Au surface[501] or APTES on Si/SiOx[502]
to absorb negatively charged GO sheets, resulting in line patterns[502] or dot arrays[501] of GO sheets. Recently, by using
dip-pen nanolithography (DPN), an AFM-based lithography
method,[507516] AUT patterns have been generated, which
are used to precisely position GO sheets on Au surfaces.[500]
Direct growth of epitaxial graphene film on prepatterned
catalyst substrate presents another route to achieve patterned graphene films,[24,505,506] which offers better electrical
properties compared to those films made from chemically
derived graphene suspensions. Typically, a layer of catalyst

(e.g., Ni) is lithographically patterned on a Si/SiO2 substrate,
which is used to grow graphene sheets by CVD. The patterned graphene layer can be moved to other substrates, by
either transfer with a polydimethylsiloxane (PDMS) stamp,
or etching SiO2 to leave the graphene layer on the surface
of aqueous solution followed by scooping it with the target
substrate.[24]
Other types of top-down lithographic techniques have also
been used to pattern graphene thin films or large area pristine graphene sheets, such as focused ion beam lithography
(FIB)[166] and e-beam lithography (EBL),[494] which can provide much smaller sized graphene patterns compared to conventional photolithography. GNR arrays that are 2030 nm
wide are fabricated by using EBL to deposit Al lines on
large-area pristine graphene and then etching the unprotected areas of graphene with O2 plasma.[494] However, GNR
of only a few nanometers in width is required for fabrication
of room-temperature FETs with a large bandgap and high
onoff current ratios, since the energy gap of a GNR scales
inversely with the ribbon width.[170,171] A chemical etching
method is thus developed to further reducing the widths of
the EBL-prepared GNRs, in order to improve the onoff
ratio in FET applications.[494] In gas-phase chemical etching
process, the etching gas O2 is mixed with Ar, H2, and NH3,
which are used as the dilution gas or provide a reducing environment. The etching rate depends on the ratio of mixed gas,
the reaction temperature, and layer numbers of graphene.
As a result, GNRs with widths of 5 nm are fabricated
(Figure 10A), which are used as FET channel materials with
an onoff ratio of 104.
Nanoscale featured structures, such as block co-polymer
films,[182] nanowires,[166] nanospheres,[492,493] can also be used
as effective etch masks in lithographic processes. Graphene
nanomeshes (GNMs) were generated for the first time using
poly(styrene-block-methyl methacrylate) (P(S-b-MMA))
block copolymer thin films with cylindrical domains as the
etch mask, where CHF3-based reactive-ion etching (RIE)
and O2 plasma etching are combined to generate holes in the
graphene layers (Figure 10B).[182] In nanosphere lithography,
uniformly sized spherical particles are able to assemble into
monolayer, forming closely packed hexagonal lattice arrangement with tunable periodicity controlled by the particle size.
Figure 10. A) AFM images of a GNR array after chemical narrowing.

Reproduced with permission.[494] Copyright 2010, Nature Publishing
Group. B) SEM image of a GNM structure after removing the top SiOx
mesh mask. Scale bar = 100 nm. Reproduced with permission.[182]
Copyright 2010, Nature Publishing Group.
small 2011, 7, No. 14, 18761902
Arrays of graphene nanodisks are thus

prepared by using a polystyrene (PS)assembled monolayer as the etch mask.[492]
Alternatively, an assembled monolayer of
silica nanospheres is used as the template
for the deposition of a porous metal film,
which in turn serves as the etch mask for
the fabrication of GNMs instead of nanodisk arrays.[493] Both the block copolymer
and nanosphere lithography are powerful
tools to fabricate GNMs with tunable
periodicity and neck width. The former
method is able to generate GNMs with
periodicity of 2739 nm and a neck width
down to 5 nm,[182] whereas the latter one Figure 12. A) Topography of a cross shape of reduced GO formed after an AFM tip heats the
provides possibilities to fabricate GNMs contact to 330 C scanned across the GO sheet at 2 mm/s. Reproduced with permission.[499]
with periodicity ranging from 100 nm to Copyright 2010, American Association for the Advancement of Science. B) Graphene
bent junction connecting
several micrometers and a neck width of nanostructures patterned by STM lithography. An 8-nm-wide 30 GNR
an armchair and a zigzag ribbon. Reproduced with permission.[167] Copyright 2008, Nature
[493]
less than 20 nm.
Publishing Group.
Since the aforementioned lithographic methods require multiple steps
and special experimental setups, a facile approach to gen- a GO sheet via temperature control (Figure 12A).[499] The
erate graphene patterns has recently been developed in our rGO nanoribbons with widths down to 12 nm are generated.
group. A sharp nonmetal object is used to directly scratch The reduced region shows increase of four orders of magnithe graphene films. The generated rectangular rGO patterns tude in conductivity compared to that of GO.
By using STM lithography, smaller features in graphene,
(Figure 11A) are successfully used as electrodes in electronic
devices.[76] The scratching process is later developed and con- as well as atomic structures, can be imaged and precisely
ducted by an AFM tip, which is controlled programmablly tailored.[167,496] This technique is therefore extremely
with a NSCRIPTOR DPN system.[517] By using this method, attractive, because it allows for the engineering of the elecvarious single-layer GO patterns such as gaps, ribbons, tronic property of the graphene nanostructures. In addition
squares, triangles, and zigzags are easily fabricated on Si/SiO2 to lithographical patterning of GNRs with predetermined
energy gaps, STM can generate more complicated archi(Figure 11B).[504]
Another type of patterning methods is the local anodic tectures as well, such as a GNR bent junction which conoxidation lithography by AFM.[497,498] Usually, a bias voltage nects an armchair and a zigzag ribbon (Figure 12B).[167]
is applied between the graphene substrate and the conducting Recently, STM has been used to remove hydrogen in
AFM tip, which creates an electric field to induce electro- hydrogen-saturated graphene, and nanoscaled graphene
chemical oxidation of the graphene at room temperature with structures are obtained. Importantly, it is observed that the
controlled humility. Although the feature width obtained in electronic property of graphene patterns with feature size
this technique could reach as low as <30 nm, the experiment smaller than 20 nm does not change compared to hydrogencan only be carried out in conducting substrates. Recently, an saturated graphene. But if the graphene patterns are larger
AFM-based thermal chemical lithography process has been than 20 nm, the intrinsic property of pristine graphene is
developed for controllable reduction of nanoscale regions in restored.[496]
4. Conclusion and Outlook
Figure 11. A) SEM image of patterned rGO electrodes generated by the scratching method.
Reproduced with permission.[76] B) SEM image of fabricated GO patterns by AFM lithography.
Inset: enlarged AFM image. Reproduced with permission.[504] Copyright 2010, American
Chemical Society.
small 2011, 7, No. 14, 18761902
Graphene exhibits a unique chemical

structure, and outstanding electronic, optical,
thermal, and mechanical properties. Its
derivatives, e.g., epitaxially grown graphene,
graphene oxide (GO), reduced GO (rGO),
and exfoliated graphite, have been produced
with various synthetic methods in order to
meet the increasing requirements for thin
film processing, composite incorporation,
and device integration.
A great number of materials have been
composited with graphene derivatives
namely,polymers,metal NPs,semiconductor
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NPs, CNTs, organic materials, and so on. The properties of

these functional hybrid materials not only depend on the
individual components, but also on the interactions between
them. Therefore, it is important to control the distribution,
density, kind of chemical bonding, as well as 3D arrangement of the components in graphene-based composites for
enhancing their performances. This has been demonstrated in
some reports, such as the graphene-wrapped Co3O4 NPs in
a Li ion battery,[404] and the 3D grapheneCNT sandwiched
structure for a supercapacitor.[438] Future efforts are still in
need to improve the fabrication techniques and provide new
possibilities in achieving improved properties. In addition,
the residual functional groups and defects in GO and rGO,[81]
and the layer number of pristine graphene,[375] have shown
some effects on the nucleation density of deposited metal
NPs; whereas the lattice of rGO is able to direct the assembly
of anchored Au nanodots.[87] It can be anticipated that, given
its rich surface chemistry and 2D configuration, graphenebased materials may serve as templates for the growth of
both inorganic and organic crystals with unusual morphologies and properties.
Graphene-based applications in FETs, memory, photovoltaic devices, and sensing platforms have been summarized.
The onoff ratio of FETs has been improved greatly via the
fabrication of GNRs and GNMs. On the other hand, GO/
rGO thin films have shown advantages in memory devices,
due to the ease of processing, and functional group-induced
charge controlling properties. In photovoltaic applications,
graphene-based materials are able to function as the transparent electrodes, electron acceptors and light absorbers. In
particular, thin films made of graphene-based materials have
shown promises as cheap, flexible, and durable supplements
to conventional transparent ITO electrodes in optoelectronic devices. Although the electrical and optical properties
of GO/rGO can be controlled by varying their size (related
to edge defects),[161] surface functionality,[77] and degree
of reduction,[149] the effective tuning of their bandgap via
chemical routes remains great challenge. In sensing applications, graphene-based materials, featured with good conductivity, large specific surface area and functionalizable surfaces,
have demonstrated accurate, rapid, selective, sensitive, and
even single-molecular sensing abilities. Future investigations
on graphene-based sensing platforms, combined with versatile sensing strategies, are expected to continuingly lower the
detection threshold.
One of the major contributions of graphene patterns lies in
the generation of GNRs and GNMs, with controllable feature
size and density. However, the current fabrication of ordered
GNRs arrays from pristine graphene with high onoff current
ratio only relies on e-beam lithography, and has not been realized in large scale with a facile procedure. Nanoscale features
can be made in graphene-based substrates by using AFM based
anodic oxidation, thermal reduction, and STM lithography,
with tunable local electronic properties. GO sheets have
been deterministically positioned on substrates by interaction
with molecular patterns generated by microcontact printing
or dip-pen nanolithography. As a future research direction, it
would be useful to directly write small graphene entities, such
as graphene quantum dots or GNRs on substrates for precise
and rapid device integration, and to prepare molecular patterns on large-area graphene films in order to partially functionalize the graphene film and thus modify its properties.
Acknowledgements
This work was supported by AcRF Tier 1 (RG 20/07) and AcRF
Tier 2 (ARC 10/10, No. MOE2010-T21-060) from MOE, CRP
(NRF-CRP22007-01) from NRF, ASTAR SERC Grants (No. 092
101 0064) from ASTAR, CREATE program (Nanomaterials for
Energy and Water Management) from NRF, and New Initiative Fund
FY 2010 (M58120031) from NTU in Singapore. Q.Y. appreciates the
support from A*STAR SERC grant 1021700144 and Singapore MPA
23/04.15.03 grant.
This Review is part of the Special Issue dedicated to Chad Mirkin
in celebration of 20 years of inuential research at Northwestern
University.
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Published online: June 1, 2011
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reviews

Graphene-Based Materials: Synthesis, Characterization,

From the Contents

Graphene, a two-dimensional, single-layer sheet of sp2

small 2011, 7, No. 14, 18761902

albumin (BSA).[118] Besides the reduction with chemical

X. Huang, Dr. Z. Y. Yin, S. X. Wu, X. Y. Qi, Q. Y. He, Prof. Q. C. Zhang,

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

amount of edge defects. For example, the GNRs and GNMs

Hua Zhang studied at Nanjing University

of GO or rGO.[148] For example, rGO dispersions in THF,

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

small 2011, 7, No. 14, 18761902

Noncovalent functionalization of graphene sheets through

Figure 1. A) Isocyanate treatment of GO where organic isocyanates

Because of their good conductivity, thermal stability, and

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

Recently, in our group, a specially designed conjugated

graphene platelets were obtained by thermal reduction of

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

small 2011, 7, No. 14, 18761902

other polymers such as silicone,[325] polystyrene,[326] and

flexible and exhibit good mechanical properties, which can

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

2.2. GrapheneMetal Nanoparticle Composites

be attributed to the presence of additional carboxylic acid

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

small 2011, 7, No. 14, 18761902

the identification method based on atomic force microscopy

2.3. GrapheneSemiconductor Nanomaterial Composites

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

by mixing GO and Cd(CH3COO)2 in DMSO, which was

network. Consequently, the anode made from the graphene

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

small 2011, 7, No. 14, 18761902

of NPs on graphene sheets, without affecting the combined

3. Applications of Graphene and

2.4. Other Graphene-Based Composites

One of the most extensively explored applications

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

graphene oxide (GO),[223,441] graphene

Oxygen plasma with

Oxygen plasma with

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

small 2011, 7, No. 14, 18761902

memory device exhibits a high onoff ratio

3.3. Photovoltaic Devices

Figure 6. A) Operation principle of type-switching memory device. B) Typical hysteresis

affecting the charges in the FET channel. Importantly, such

3.3.1. Transparent Electrodes

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

and subsequently incorporated to a hybrid solar cell based on a

2D structure and high electron mobility. To date, to the best

The tunable bandgap and large optical

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

small 2011, 7, No. 14, 18761902

3.4. Sensing Platforms

Such excellent performance is attributed to the high carrier

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

nitrogen plasma. The obtained N-doped rGO results in high

2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim

small 2011, 7, No. 14, 18761902

event takes place, fluorescence resonance energy transfer