reviews

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

2. Graphene-Based Materials. . . . . . . . . . . 1878
3. Applications of Graphene and
Graphene-Based Materials . . . . . . . . . . 1885
4. Conclusion and Outlook . . . . . .. . . . . . . 1893
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 graphene-
based 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.

1876 wileyonlinelibrary.com © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim small 2011, 7, No. 14, 1876–1902
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 σC-C bond is one of the
strongest bonds in materials and the out-of-plane π bond,
which contributes to a delocalized network of electrons, is
responsible for the electron conduction of graphene and pro-
vides the weak interaction among graphene layers or between
graphene and substrate. With these unique structural charac-
teristics, graphene has shown exceptional physical properties,
which have attracted enormous research interest in both sci-
entific and engineering communities.[3–17]
One of the most remarkable properties of graphene is
that its charge carriers behave as massless relativistic parti-
cles 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 cm−2 and
room-temperature mobilities of ∼10 000 cm−2 s−1 are meas-
ured.[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 trans-
parent, with an absorption of ∼2.3% towards visible light.[6]
Its thermal conductivity, k, is measured with a value of
∼5000 W mK−1 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 m−1 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 deriva-
tives. 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 exfo-
liation 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.[8,23–56] Large-
area 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,[57–72] through high-
temperature annealing. However, these methods are imprac-
tical 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[74–116] or chemically function-
alized 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,[74–86,90–93]
strong alkaline media,[117] vitamin C,[116] and bovine serum
small 2011, 7, No. 14, 1876–1902 © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
albumin (BSA).[118] Besides the reduction with chemical
agents, electrochemical,[109,119–121] photochemical[87,122] and
thermal[94,111,123–131] reduction methods have been devel-
oped as well. As the precursor of rGO, graphene oxide
(GO) sheets,[59–72,132–145] 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).[74–78,80–82,146]
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 conduc-
tivity several orders lower than the pristine graphene because
of the incomplete reduction and the presence of numerous
defects, which disrupt the sp2 network.[75,77,80,150–152] In order
to overcome the poor conductivity of rGO, several methods
have been developed. For example, the non-oxidation liquid-
phase exfoliation of graphite has been demonstrated, which
can produce large-area single-layer graphene by ultrasoni-
cation of graphite in both aqueous[153] and non-aqueous[154]
solutions. Re-intercalation and ultrasonication of thermally
exfoliated expandable graphite (EG) can produce single-
layer graphene sheets as well.[155] Even without ultrasonica-
tion, 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 elec-
trochemical 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 fol-
lowed by pyrolysis,[159] and the organic synthesis of graphene-
like polyaromatic hydrocarbons.[160]
Besides the graphene-based 2D sheets, other graphene-
related materials have been fabricated/synthesized as well,
such as zero dimensional (0D) graphene quantum dots,[161–163]
1D graphene nanoribbons (GNRs),[5,163–181] and graphene
nanomeshes (GNMs).[182–187] 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: +65–6790-9081
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
www.small-journal.com 1877
 reviews
amount of edge defects. For example, the GNRs and GNMs
have exhibited band opening with much enhanced on–off
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 solu-
tion-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 var-
ious kinds of applications, including FETs,[18,75,76,110,188–216]
memories,[85,86,217–233] photovoltaic devices,[23,80,84,161,234–252]
photocatalysis,[251,253–256] sensors,[75,119,257–266] 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 graphene-
based 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,[272–296] or noncovalent
functionalization.[74,77,152,287,289,290,293,297–306]
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 oxygen-
containing groups, the chemically reduced graphene oxide
(rGO), or so called chemically modified graphene, can form
the homogeneous aqueous suspension by controlled reduc-
tion 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 tetrahy-
drofuran (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 dis-
persed 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 © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
X. Huang et al.
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 Katho-
lieke 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 Nano-
science, 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 con-
verting the edge carboxylic acid groups of rGO into octade-
cylamines, 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 GO–polymer 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 function-
alized with diazonium salts (e.g., sodium dodecylbenzenesul-
fonate, SDBS), and the resulting rGO was readily dispersed
in several polar organic solvents (Figure 1C).[277] Addition-
ally, 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.[278–280] Recently,
the surface of graphene was covalently functionalized by
grafting polystyrene-polyacrylamide (PS-PAM) through in-
situ free-radical polymerization.[281]
Compared to covalent functionalization, noncovalent
functionalization based on the van der Waals force or the π–π
interaction between rGO and stabilizers not only gives less
negative impact on the structure of graphene and its deriva-
tives, 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 hydro-
phobic backbone of PSS, while the hydrophilic sulfonate side
groups sustained the whole graphene–PSS complex in water.
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Graphene-Based Materials
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
(μG) with azido-phenylalanine (Phe-N-μG) 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 func-
tionalization 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]
small 2011, 7, No. 14, 1876–1902 © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
Noncovalent functionalization of graphene sheets through
the π–π interaction was reported by using the water-soluble
aromatic organic molecule 1-pyrenebyturate (PB−) as a sta-
bilizer; and through subsequent vacuum filtration, large-area
flexible PB−–graphene films with layered structures could
be prepared.[297] This approach provides a general route for
the preparation of functionalized graphene through the π–π
interaction. Other reports based on this strategy have shown
significantly improved solubility and conductivity of the func-
tionalized graphene sheets.[289,298,300,301]
2.1. Graphene–Polymer Composites
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 graphene–polymer com-
posites 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 graphene–polymer composites are solution mixing,[307–312]
melt blending,[313–315] and in-situ polymerization.[316–327]
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 sol-
uble polymer, such as poly(vinyl alcohol) (PVA), is easy to
be mixed with aqueous GO dispersions at various concen-
trations.[307,328] However, the low solubility of GO and rGO
in organic solvents poses great challenge in synthesis of
graphene–polymer 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] polycapro-
lactone (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 evap-
oration. 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 aro-
matic molecules), which limit the solubility of the obtained
rGO based materials.
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 reviews
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 π–π 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 graphene–polymer
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 π-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 π–π 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 outer-
layer. As a result, the obtained graphene–polymer 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 175–200 °C.[313] In another example,
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 mgmL−1. Reproduced with permission.[74]
1880 www.small-journal.com © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
X. Huang et al.
graphene platelets were obtained by thermal reduction of
GO, and then melt-blended with polyethylene terephthalate
(PET) at 285 °C to give the PET–graphene composite.[314]
However, melt compounding is not as effective as the solu-
tion 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 polymeriza-
tion.[316–318,332] For example, a graphene nanoplatelet suspen-
sion 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.[319–323] 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,
graphene–PANI 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,
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Graphene-Based Materials
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 graphene–polymer composite, layer-by-layer
(LbL) assembling has been carried out to prepare freely
standing composite membranes. For example, the LbL fab-
rication was conducted using the Langmuir–Blodgett (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, graphene–polymer composites have shown
improved properties in electrical conductivity, electrochem-
ical capacity, mechanical strength, and thermal stability and
conductivity. One of the mostly employed host polymers is
PANI, and many reports on graphene–PANI composites have
achieved enhanced electrochemical performances.[310,319–324]
For example, the flexible graphene–PANI 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 prom-
ising 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 poly-
mers have also been used to host graphene-based fillers. The
electrical conductivity of polystyrene–graphene composites
were studied at different composition ratios.[331] Percola-
tion 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 attrib-
uted to the high aspect ratio of the graphene sheets, their
homogeneous dispersion in the polymer matrix, as well as
the good filler–matrix interfacial interaction induced by the
surface functional groups. With the other polymer matrices,
poly(vinyl chloride/vinyl acetate) copolymer/graphene com-
posites exhibited a percolation threshold of 0.15 vol%,[327]
while the PET–graphene 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 meas-
ured, with a breaking strength of 42 N m−1 and a Young’s
modulus of 1.0 TPa.[3] Using graphene derivatives as filler
materials, a number of reports have shown the enhanced
mechanical properties of graphene–polymer composites.
Functionalized GO layers were embedded in the polyelec-
trolyte 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 mem-
brane to ∼20 GPa for 8 vol% of graphene loading. These poly-
electrolyte-based membrane materials are conductive and
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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 filtra-
tion. At 3 wt% of GO loading, a Young's modulus of 4.8 GPa
and tensile yield strength of ∼110 MPa were achieved. To fur-
ther improve the interaction of the graphene filler and the
polymer matrix, thus facilitating the effective load transfer,
polyurethane (PU) was covalently bonded with GO plate-
lets, 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 prop-
erties 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 character-
ized 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 high-
speed shearing, the obtained composite exhibited up to a
30 °C increase in Tg with 1–5 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 filler–matrix interactions. With a
loading of 0.05 wt% FGS, there is an increase of 30 °C in Tg
for the formed PAMAM–FGS 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] Impor-
tantly, 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 oper-
ated at above the glass transition temperature, their thermal
stability is determined by measuring the degradation temper-
ature. For example, FGSs have been successfully embedded
in silicone through an in-situ foaming process. Thermogravi-
metric analysis (TGA) showed an increase of up to 55 °C in
the degradation temperature of silicone–FGS 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 PLA–EG 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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 reviews
matrix is expected to significantly enhance the thermal con-
duction of the composite. Thermally exfoliated graphite nano-
platelets 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 50–70%
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 con-
ductivity.[325] The large aspect ratio, 2D geometry, high stiff-
ness, and low thermal interface resistance of graphene have
caused the enhanced thermal conductivity in these reports.
Such composite foams with excellent heat dissipation prop-
erty are advantageous for coatings on electrical wires to elim-
inate conductive heat.
2.2. Graphene–Metal Nanoparticle Composites
The attractive properties of graphene and its deriva-
tives have made them ideal templates for the synthesis
of metal nanoparticles (NPs), such as Au,[81,87,118,334–359]
Ag,[81,360–362] Pd,[165,334,341,349,363–368] Pt,[118,334,369] Ni,[370] and
Cu.[341] Dependent on the type of the anchored NPs, the
graphene–metal NP composites have been applied in a
broad range of areas, such as surface-enhanced Raman scat-
tering (SERS),[81,337] catalysis,[349,363] and electrochemical
sensing.[119,348,371–373] The graphene–metal NP composites can
be prepared by chemical reduction,[334,336,339,373,374] photo-
chemical synthesis,[87,98] microwave assisted synthesis,[341]
electroless metallization,[81] and thermal evaporation.[375]
One of the most straightforward approaches to prepare
graphene–metal NP composites is the direct chemical reduc-
tion 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 graphene–Au NP composite was prepared by the reduc-
tion 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 Suzuki–Miyaura 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 h−1, accompanied by
very low Pd leaching (<1 ppm).
To impart better solubility and thus improved proces-
sibility of graphene–metal 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 well-
distributed Au NPs with a high surface coverage, which could
1882 www.small-journal.com © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
X. Huang et al.
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 pre-
pared 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 seed-
modified rGO films.[374] The fabricated Au nanorods give sig-
nificantly enhanced Raman signals of rGO—34 times higher
at the rod tip,[374] which is much higher than that of snow-
flake-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 exhib-
ited an edge length of 200–500 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 seed-
mediated 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 cata-
lysts. 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, photo-
chemical reduction can be applied as a supplement or alter-
native to the chemical- reagent-based reduction for the
synthesis of graphene–metal 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 graphene–metal 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, facili-
tate 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, 1876–1902
Graphene-Based Materials

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 phenom-
enon 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 chemi-
cally 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 inter-
action between graphene and the evaporated Au atoms.
Second, the diffusion coefficient of Au atoms varies on dif-
ferent surfaces, which determines the outcome of the compe-
tition 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
the identification method based on atomic force microscopy
(AFM) measurements.
2.3. Graphene–Semiconductor 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,[88,122,251,253,254,256,376–386] ZnO,[78,80,387–391]
SnO2,[392–397] MnO2,[398–401] Co3O4,[402–406] Fe3O4,[407–417]
Fe2O3,[418,419] NiO,[221] Cu2O,[78,79,420] RuO2,[421,422]
CdS,[238,245,423–428] and CdSe.[100,429–432] The synthetic methods
for preparation of these graphene–semiconductor nano-
material 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 nanomate-
rials. For example, graphene–CdS composites were prepared

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 reviews 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 elec-
tron transfer process from CdS NPs to the graphene sheet,
which demonstrates the potential optoelectronic applica-
tion of this graphene–CdS hybrid material. In another work,
graphene–Co3O4 hybrid material was synthesized by reacting
Co(NO3)2·6H2O and ammonia solution in the presence of
GO sheets, followed by drying and heating at 450°C to result
in the Co3O4–graphene composite used for the Li ion bat-
tery application.[403] The in-situ crystallization approach is
also applicable to synthesis of many other types of semicon-
ductor 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 graphene–semiconductor
NP composites, which has been applied to prepare graphene–
MnO2 NPs[400] and graphene–Co3O4 NPs.[402] For example,
after a water suspension of rGO was mixed with potas-
sium permanganate powders by ultrasonication, the mix-
ture was heated in a household microwave oven for only
5 min to obtain the graphene–MnO2 NP composites.[400] Figure 4. A) Schematic illustration of fabrication of graphene-
Another efficient and direct means to prepare graphene– encapsulated metal oxide NPs. B) Typical SEM image of graphene-
semiconductor NP composites is the solution mixing encapsulated Co3O4. C) Cycle performance of graphene-encapsulated
approach.[256,376,379,404] For example, commercialized TiO2 Co3O4. Reproduced with permission.[404]
NPs (P25) were mixed with Nafion-coated graphene to fab-
ricate dye-sensitized solar cells, where the Nafion served as a network. Consequently, the anode made from the graphene–
“glue” to tightly bind graphene sheets and NPs.[379] In another Co3O4 NP composites showed a very high reversible capacity
example, after the pre-synthesized CdS NPs were functional- of 1100 mA h g−1 in the first 10 cycles, and over 1000 mA h g−1
ized with benzyl mercaptan molecules and then mixed with after 130 cycles (Figure 4C).
rGO sheets, the benzyl mercaptan-capped CdS NPs absorbed Thin-film-based applications require postsynthetic depo-
on rGO surfaces through π–π interactions.[423] However, in sition of the composite materials on substrates by techniques
some cases the pre-synthesized NPs from an organic synthetic such as spin-coating, drop casting, and transfer printing.
route are not compatible with the aqueous dispersion of GO Therefore, the direct electrochemical deposition of NPs on
sheets. In order to solve this problem, a two-phase approach graphene-based substrates is an attractive approach to pre-
was developed to prepare graphene–TiO2 composites. For pare certain types of graphene–semiconductor nanomaterial
example, after a solution of oleic acid-capped TiO2 nanorods hybrid films, for example, ZnO, Cu2O, and CdSe.[78,80,429] For
in toluene was mixed with GO water suspension and stirred instance, ZnO nanorods were deposited on spin-coated rGO
for 24 h, the TiO2 nanorods were able to assemble on the GO thin films on quartz, using an oxygen-saturated aqueous solu-
surface at the water/toluene interface.[256] tion of ZnCl2 and KCl as the electrolyte.[80] It is found that
Very recently, a novel strategy used to prepare graphene- the crystal quality of the deposited ZnO nanorods depends
encapsulated metal oxides hybrids has been developed. In on the thickness of the rGO thin films. For example, the thick
this work, after the negatively charged GO sheets wrapped rGO film electrode with low resistivity gives better quality
around the positively charged Co3O4 NPs (modified by ami- of the deposited ZnO nanorods. This method has also been
nopropyltrimethoxysilane, APS) through the electrostatic applied to deposit Cu2O nanostructures on rGO films, spin-
interaction, GO was chemically reduced to rGO. The obtained coated on flexible polyethylene terephthalate (PET) sub-
composites were successfully used for the Li ion battery strates.[78] Different from the random deposition of ZnO
application (Figure 4A–C).[404] This approach is essentially and Cu2O on rGO films, the ordered CdSe NP patterns on
important for the preparation of graphene–metal oxide NP graphene films were realized through a templated electro-
composites as anode materials for lithium ion storage due to chemical process.[429] In this work, after graphene was epitax-
the following reasons. First, the graphene encapsulation can ially grown on Ni film, a layer of mesoporous silica film was
suppress the aggregation of oxide NPs during the charge– formed on the graphene sheets via a sol–gel process. Then
discharge process. Second, it gives rise to high oxide content CdSe NPs were electrochemically deposited on the graphene
in the composites (∼91.5 wt%). Third, an overall high electro- surface through the precoated porous silica film. This work
conductivity of the composite is maintained by the graphene demonstrates a ligand-free process for the pattern formation

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Graphene-Based Materials
of NPs on graphene sheets, without affecting the combined
electronic properties of the semiconductor NPs and the
graphene layers.
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, PDI–GO
core–shell wires were formed through π–π interactions.[242]
The obtained organic hybrid structure outperformed its
individual components in donor–acceptor-type solar cells.
Graphene–peptide 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 core–shell structures
were subsequently calcinated to remove the peptide cores,
and gave rise to hollow graphene shells, which could be
applied as supercapacitor electrodes.
Moreover, graphene–carbon nanotube (CNT) compos-
ites have been prepared and applied in transparent con-
ductors,[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 elec-
tronic properties compared to pristine graphene. Hence,
the combination of rGO and CNT in a transparent con-
ductor has shown the expected enhancement in film conduc-
tivity.[435] Another advantage of graphene–CNT 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 pil-
lars 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 g−1 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 cata-
lyst 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 charge–discharge processes.
Third, the interconnection of CNTs with graphene main-
tains 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, 1876–1902 © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
3. Applications of Graphene and
Graphene-Based Materials
3.1. Field-Effect Transistors
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 μm was obtained by mechanical exfoliation of
highly oriented pyrolytic graphite (HOPG). 2D FLG behaves
with metallic characteristics and exhibits a strong ambi-
polar electric field effect. The pristine graphene could not
be used for the fabrication of effective FET devices because
the on–off 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 character-
istics were observed.[188] The saturation velocity depends on
the charge-carrier concentration which is attributed to scat-
tering by interfacial phonons in the SiO2 layer which sup-
ports the graphene channel. The electrostatic modulation of
the channel through an efficiently coupled top-gate yields the
transconductance as high as 150 μS μm−1. These results dem-
onstrate the feasibility of such graphene devices for analogue
and radio-frequency circuit applications where bandgap engi-
neering/opening is unnecessary.
In order to improve the on–off 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.[5,169–172,177,439–440] 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 thin-
nest 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 reduc-
tion 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 on–off ratio from the corre-
sponding 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 well-
defined zigzag or armchair-edged structures. Electrical trans-
port experiments showed that all of the sub-10-nm GNRs
were semiconductors and afforded graphene FETs with
on–off ratio of ∼107 at room temperature.[5]
Although GNRs have shown semiconductor proper-
ties due to the bandgap opening of graphene, the practical
devices and circuits often require high driving current or
www.small-journal.com 1885
 reviews X. Huang et al.

Table 1. Comparison of methods used for generation of GNRs and the resulting on–off graphene oxide (GO),[223,441] graphene–
current ratio obtained from the GNR-based FETs. Au hybrid systems,[104] graphene–polymer
composites,[218] and rGO-electrodes.[219,220]
Methods for Methods for Width of graphene Maximum Current References In the graphene-based nonvola-
preparation generation of nanoribbons bandgap opening on–off
tile memory device with ferroelectric
of graphene graphene nanoribbons [nm] [meV] ratio
gating,[217] the binary information, i.e., high
Mechanically Oxygen plasma with 15 200 N.A. [170]
and low resistance states of the graphene
peeled from e-beam lithography
working channel, can be switched by con-
graphite generated resist
crystals pattern as etch mask trolling the polarization of the ferroelec-
tric thin film induced by the electrostatic
Mechanically Oxygen plasma with ∼15 N.A. ∼12 [169]
peeled from dielectric nanowire as
doping of graphene. In the case of GO-
graphite crystals etch mask based memory devices, the properties of
Exfoliation plus Chemical ∼2 ∼400 10 7
[5]
desorption/absorption of oxygenated func-
ultrasonication derivation tional groups on the GO sheets[441] and
based on the unique charge trapping properties of
expandable graphite GO[223] have enabled the switching effect
Unzipping multiwall Plasma etching ∼6 N.A. >100 [177] with the threshold voltage of 1 and 1.4 V,
carbon nanotubes respectively.[223,441]
Thanks to the feasibility of large-area
production of rGO films, the fabrication
transconductance. Therefore, a dense array of ordered nanori- of both conductivity- and type-switching memory devices
bbons is desirable, which, however, remains a significant has been successfully demonstrated in a rGO/Au NP hybrid
challenge. Alternatively, another type of graphene nanostruc- system (Figure 6).[104] The real-time type-switching of the car-
tures, called graphene nanomesh (GNM)[182,183] or nanoper- rier types in the rGO-FETs can be controlled by applying a
forated graphene,[184] was developed, which not only opens gate bias to adjust the charges in the Au NPs, thus in turn
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 fabri-
cated with GNM as the channel material,
referred to as GNM-FETs, can support
currents ∼100 times greater than individual
GNR devices, while the on–off ratio, which
can be tuned by varying the neck width,
is comparable with that achieved in indi-
vidual GNR devices (Figure 5). Addition-
ally, 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 theo-
retically by Gunlycke et al. that when
the graphene nanostrips are under a
non-equilibrium state, e.g., in the pres-
ence of a ballistic current, both spin-
polarized 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 graphene-
related memory devices were carried
out, based on pristine graphene,[217]
Figure 5. A) Schematic of a GNM-FET. B) Drain current (Id) versus drain–source 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 μm and length 3.6 μm), ∼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.

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Graphene-Based Materials

memory device exhibits a high on–off ratio

(104–105) and low switching threshold
voltage (0.5–1.2 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 fab-
ricate highly reduced GO films by chem-
ical 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 ≈160–500 Ω sq−1. By using
them as the electrodes in memory devices
with a configuration of rGO/P3HT:PCBM/
Al, a high on–off current ratio of up to106
is achieved.

3.3. Photovoltaic Devices

Figure 6. A) Operation principle of type-switching memory device. B) Typical hysteresis Owing to its good electronic con-
curve of type-switching memory device based on GO and NPs. It exhibited both n-type and ductivity, optical transparency, and large
p-type characteristics near zero gate bias voltage. C) Real-time switching of the reduced GO specific surface area, graphene-based
channel type. After applying a large positive (or negative) top-gate bias, a small back-gate materials have been extensively explored
bias was used to confirm the p-type (or n-type) behavior of the channel. D) Switching the in the field of photovoltaics. Until now,
inverter functionality by using a transistor that consisted of graphene and NPs. Reproduced
lots of studies on graphene-based photo-
with permission.[104]
voltaic applications have been reported, in
which graphene-based materials are used
affecting the charges in the FET channel. Importantly, such as the transparent electrodes,[23,80,105,234,244,248,435,442] electron
type-switching behavior of the rGO-based devices is success- acceptor,[161,237–238,246,376,378–379] and light absorber.[161]
fully applied to build the reconfigurable inverter logic gates
by controlling the charges in the Au NPs.[104]
3.3.1. Transparent Electrodes
Graphene–polymer composites have been investigated
in memory devices as well, through a reliable and low-cost Graphene-based transparent electrodes are mainly employed
synthetic route.[218] As reported, GO was modified by a in three types of photovoltaic devices: organic,[23,105,244,435,442]
conjugated-polymer of triphenylamine-based polyazome- inorganic–organic hybrid,[80] and dye-sensitized solar cells.[234]
thine (TPAPAM), and then incorporated into a nonvola- In the organic photovoltaic (OPV) solar cells, the highest
tile memory device. This device exhibits a typically bistable power conversion efficiency (PCE, η) of 1.71% has been
electrical switching and nonvolatile rewritable memory reported based on the use of large-area, continuous, trans-
effect. An on–off current ratio of more than 103 is achieved. parent, and highly conducting few-layer graphene films
Under application of a constant voltage stress, both deposited by the CVD process.[244] The good performance is
the on and off states from such TPAPAM–GO-based attributed to the noncovalent modification of the graphene
memory device are stable up to 108 read cycles at a read films with pyrene buanoic acid succidymidyl ester. In another
voltage of –1.0 V. report, CVD-deposited-graphene is successfully transferred
The use of indium tin oxide (ITO) and some metal onto a flexible PET substrate for fabrication of OPV devices.
materials as electrodes in memory devices has been limited It is worth noting that the graphene/PET-based and ITO/PET-
because of their brittle nature, high cost, and insufficient ele- based OPV devices showed comparable performances with an
ment resources. Consequently, the memory device based on η of 1.18 and 1.27%, respectively.[23] Importantly, the CVD-
polymer composites of poly(3-hexyl thiophene) (P3HT) and grown graphene-based solar cells show outstanding capability
methanofullerene [6,6]-phenyl C61-butyric acid methyl ester to be operated under bending conditions with bending angles
(PCBM) bulk-heterojunction (BHJ) on rGO film electrode up to 138°, while the ITO-based devices display cracks and
has been developed in our group.[86] The current–voltage irreversible failure under bending of only 60°. Therefore, the
(I–V) curves from this rGO/P3HT:PCBM/Al memory show epitaxially grown graphene used as a highly flexible, transparent,
the electrical bistable behavior, a write-once-read-many- and continuous electrodes for OPVs presents itself as a poten-
times (WORM) memory effect. The carrier transport mecha- tial replacement for ITO in flexible photovoltaic applications.
nism related to the conductivity-switching is affected by the As an alternative to CVD-grown graphene, rGO film has
polarization of PCBM domains and the formation of a local- been used as transparent electrode as well.[80] In this study,
ized internal electrical field among the adjacent domains. The ZnO film is electrochemically deposited on the rGO electrode

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 reviews X. Huang et al.

and subsequently incorporated to a hybrid solar cell based on a
ZnO–P3HT system. The PCE of the inorganic–organic 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 flex-
ible 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 per-
formance 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 1000–3000 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-p-
methoxyphenilamine)-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 mate-
rial 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 graphene–TiO2 composite,[376]
and a layered graphene–quantum 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 functional-
ized graphene (SPFGraphene) was then mixed with poly(3-
octylthiophene) (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 sug-
gests the promises of SPFGraphene materials to serve as a
competitive alternative to PCBM as the electron acceptor for
high-performance OPV devices.
The graphene–TiO2 composite, as another type of effec-
tive 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 pre-
vent the charge recombination and increase the light collec-
tion efficiency, thus improving the photoelectrical conversion
efficiency of DSSCs. Compared with pure TiO2 photoanode-
based DSSCs, the short-circuit current density for the
graphene–TiO2 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 signifi-
cantly 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

The tunable bandgap and large optical
absorptivity of graphene are appealing
characteristics for the efficient light har-
vesting. By using small organic compounds,
graphene QDs that contain 168 conju-
Figure 7. A) Under simulated globe sun illumination, the obtained I–V curves for ZnO/P3HT gated carbon atoms have been synthesized
hybrid solar cells by using I) one-step and II) two step reduced GO films as electrodes. Inset: via a stepwise solution-based chemical
schematic illustration of the fabricated solar cell. Reproduced with permission.[80] B) Top: route.[161] The uniform-sized graphene
illustration of dye-sensitized solar cell using graphene film as electrode. The four layers
QDs are made highly soluble after their
from bottom to top are Au, dye-sensitized heterojunction, compact TiO2, and graphene film.
Bottom: I–V curve of graphene-based cell (black) and the FTO-based cell (grey), illuminated edges are covalently reacted with 1,3,5-
under AM solar light (1 sun). Reproduced with permission.[234] Copyright 2008, American trialkyl phenyl moieties. This novel solu-
Chemical Society. bilization strategy enables the QDs to act

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Graphene-Based Materials
as light absorbers (sensitizers) and to replace the tradition-
ally used ruthenium complexes in nanocrystalline TiO2 solar
cells. However, the resulting energy conversion perform-
ance is not high, which requires improvement by covalently
binding functional groups to the QDs for higher charge injec-
tion, or optimizing the preparation procedure for the elec-
trode. 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 sensi-
tivity,[258] low noise,[19,20,258] facile fabrication, and biocompat-
ible 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 detec-
tion 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 con-
ducting 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 mol-
ecules 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.
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.
small 2011, 7, No. 14, 1876–1902 © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
Such excellent performance is attributed to the high carrier
mobility of graphene[18–19] and the resulting extremely low
noise.[19–20]
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 perform-
ance 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 prom-
ising 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 pro-
teins.[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 secre-
tion of catecholamine molecules by PC12 cells in the high K+
solution.[75a]
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 reviews
A hybrid material of rGO and Au NP–antibody conju-
gates 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-nanomaterial-
based sensors.
3.4.2. Electrochemical Sensors
Graphene-based materials possess large specific sur-
face area, excellent conductivity, and availability for sur-
face functionalization, which are important characteristics
in the electrochemical applications.[449] Until now, many
graphene-based electrochemical sensors have been reported
to detect glucose,[119,265,344,348,371,450–460] ascorbic acid,[461–463]
dopamine,[462–470] H2O2,[343,372] DNA,[257] DNA bases,[259] and
antigen.[471] It has been shown that graphene and graphene-
based materials are promising supplements or replacements
for conventional carbon materials, such as carbon nanotubes
and graphite.[472] Even superior performance of graphene-
based electrochemical sensors compared to carbon nano-
tubes 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 differen-
tiate 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 sub-
strates, which are used to simultaneously detect dopamine,
ascorbic acide, and uric acide. The graphene flakes process
abundant graphitic edge planes and defects, which are essen-
tially responsible for the fast electron transfer and good elec-
trocatalytic 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 elec-
trode[119,257,265,451,465] and Au electrode.[259] The glassy carbon
electrode is usually functionalized with APTES, which con-
tains 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 methicillin-
resistant 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 sur-
face.[265] In the latter case, the rGO is further treated with
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X. Huang et al.
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 alter-
natively with poly(ethyleneimine) (PEI) on a glassy carbon
electrode via an LbL assembly approach.[452] The obtained
multilayer graphene–polymer films display enhanced elec-
tron 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, graphene–NP composites have been
applied in electrochemical sensing.[343,372,471,473] In one of the
attempts, a graphene–Au NP composite is mixed with chi-
tosan 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, graphene–Pt NP is used
to modify glassy carbon electrode, which exhibits superior
detection performance compared to the electrode only modi-
fied by graphene, with a wide linear range and low detec-
tion limit for H2O2 and trinitrotoluene (TNT).[372] In these
reports, the enhanced performance of graphene–metal 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 graphene–NP composites to
modify the electrode, nanogold enwrapped graphene nano-
composites (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-anti-
CEA-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, selec-
tive, 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,[261,262,264,474–476] induced by the fluo-
rescence 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
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Graphene-Based Materials

the detection process, a target molecule (i.e., the complemen-
tary 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 sen-
sitivity 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 mag-
nitude lower than that detected by CNT-based florescent
sensors.[264]
In a different approach, GO is complexed with a water-
soluble and positively charged organic dye, 4-(1-pyrenyl-
vinyl)-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 sur-
face 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.[478–479]
As reported recently, GO exhibits the near-UV to blue fluo-
rescence,[149,480] which originates from the recombination
of electron–hole pairs, localized within the small sp2 carbon
domains embedded in the carbon–oxygen sp3 matrix.[149]
Based on this feature of GO, an immune-biosensor system
has been developed. In this work, after GO sheets are pat-
terned 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 9A–C). Once the binding
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,
which were synthesized with Au NP/Ab molar ratios of 1:150, 10:150, and 30:150. C) Relative
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 ioniza-
efficiencies 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]
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 plat-
form 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 clus-
ters.[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 low-
mass 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 characteri-
zation of small molecules. Hence, many substances have been
tested as a matrix to eliminate matrix–ion 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., α-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 pol-
lutant. A detection weight of as low as 500 pg is achieved,
whereas conventional organic matrices of 2,5-dihydroxyben-
zoic 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 π-conjugated networks of rGO for energy
absorption and electron transfer, and the presence of oxygen-
containing functional groups for interac-
tion with the released radicals.[82]
Surface-enhanced laser desorptio/
ionization time-of-flight mass spectrom-
etry (SELDI-TOF-MS) is another type of
LDI-MS. Instead of using a matrix such as
in MALDI-TOF MS, SELDI-TOF-MS uti-
lizes 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 π–π interactions,
graphene flakes are able to disperse in
water. The binding force between DNA and
100 fm toward ssDNA is obtained.[488]

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 reviews
3.5. Patterning of Graphene-Based Materials
There is increasing demand on the fabrication of pat-
terned graphene thin films with well-controlled feature size
and periodicity, and tunable electronic properties, such as
patterned graphene electrodes, arrays of graphene nanori-
bons (GNRs), and nanomeshes (GNMs). Various methods
have been developed to generate graphene-based patterns,
which include the conventional photolithography,[200,489–491]
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] tip-
based thermal chemical reduction,[499] dip-pen nanolitho-
graphy (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.[24,505–506]
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 con-
trol. 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., functional-
ized perfluorophenylazide (PFPA) such as PFPA-silane for
a silicon or glass substrate or PFPA–disulfide for gold films.
Then a suspension of graphene flakes is spin-coated onto the
modified substrate, which is, after drying, subjected to UV-
irradiation through a photomask. Upon light irradiation, the
azido group on PFPA is converted to the highly reactive sin-
glet perfluorophenylnitrene that can undergo C=C addition
reactions with the adjacent graphene. The subsequent ultra-
sonication and rinsing processes result in the removal of non-
reacted 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 epitaxi-
ally 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 sub-
strates 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 pat-
terns[502] or dot arrays[501] of GO sheets. Recently, by using
dip-pen nanolithography (DPN), an AFM-based lithography
method,[507–516] 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 pat-
terned graphene films,[24,505,506] which offers better electrical
properties compared to those films made from chemically
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X. Huang et al.
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 pat-
terned 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 pris-
tine graphene sheets, such as focused ion beam lithography
(FIB)[166] and e-beam lithography (EBL),[494] which can pro-
vide much smaller sized graphene patterns compared to con-
ventional photolithography. GNR arrays that are 20–30 nm
wide are fabricated by using EBL to deposit Al lines on
large-area pristine graphene and then etching the unpro-
tected 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
on–off 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 on–off
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 envi-
ronment. 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 on–off 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 arrange-
ment 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.
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Graphene-Based Materials

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 nano-
disk 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 27–39 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
several micrometers and a neck width of nanostructures patterned by STM lithography. An 8-nm-wide 30° GNR bent junction connecting
[493] an armchair and a zigzag ribbon. Reproduced with permission.[167] Copyright 2008, Nature
less than 20 nm.
Publishing Group.
Since the aforementioned litho-
graphic 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 magni-
the graphene films. The generated rectangular rGO patterns tude in conductivity compared to that of GO.
(Figure 11A) are successfully used as electrodes in electronic By using STM lithography, smaller features in graphene,
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 elec-
various 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
(Figure 11B).[504] energy gaps, STM can generate more complicated archi-
Another type of patterning methods is the local anodic tectures as well, such as a GNR bent junction which con-
oxidation 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 hydrogen-
can 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

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,
Figure 11. A) SEM image of patterned rGO electrodes generated by the “scratching” method.
and device integration.
Reproduced with permission.[76] B) SEM image of fabricated GO patterns by AFM lithography. A great number of materials have been
Inset: enlarged AFM image. Reproduced with permission.[504] Copyright 2010, American composited with graphene derivatives—
Chemical Society. namely,polymers,metal NPs,semiconductor

small 2011, 7, No. 14, 1876–1902 © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim www.small-journal.com 1893
 reviews
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 arrange-
ment 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 graphene–CNT 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, graphene-
based materials may serve as templates for the growth of
both inorganic and organic crystals with unusual morpholo-
gies and properties.
Graphene-based applications in FETs, memory, photo-
voltaic devices, and sensing platforms have been summarized.
The on–off 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 trans-
parent 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 optoelec-
tronic 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 applica-
tions, graphene-based materials, featured with good conduc-
tivity, 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 versa-
tile 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 on–off current
ratio only relies on e-beam lithography, and has not been real-
ized 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
1894 www.small-journal.com © 2011 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
X. Huang et al.
and rapid device integration, and to prepare molecular pat-
terns on large-area graphene films in order to partially func-
tionalize 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-T2–1-060) from MOE, CRP
(NRF-CRP2–2007-01) from NRF, A∗STAR SERC Grants (No. 092
101 0064) from A∗STAR, 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 influential research at Northwestern
University.
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