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Epitaxial Graphene Growth by Carbon Molecular Beam
Epitaxy (CMBE)
By Jeongho Park,* William C. Mitchel, Lawrence Grazulis, Howard E. Smith,
Kurt G. Eyink, John J. Boeckl, David H. Tomich, Shanee D. Pacley, and John. E. Hoelscher
Since graphene was first prepared by simple mechanical exfo-
liation of highly ordered pyrolytic graphite (HOPG),[1] many
approaches have been studied for its growth or preparation
including annealing of silicon carbide (SiC),[2,3] exfoliation,[4]
chemical vapor deposition (CVD) on transition metals,[5,6]
and the formation and subsequent decomposition of graphite
oxide.[7] None of these approaches, however, involve direct
deposition of carbon onto the substrate of interest. Among
the above mentioned methods, the thermal decomposition of
SiC[2,3] has attracted interest due to its potential for uniform,
wafer scale growth of graphene. An advantage of this method
is that it eliminates the process of transferring the graphene
from the metal or bulk graphite to the substrate on which
the graphene will ultimately be used. In this process the SiC
decomposes at high temperatures during which Si evaporates
and carbon remains to form graphene. It is generally accepted
that a specific SiC surface reconstruction, 6√3 × 6√3 R30°, is
required for the carbon to form graphene. While great strides
have been made using this technique on both (0001) and
(0001) surfaces of SiC, it is limited by a lack of control over the
graphene growth. The only major control parameters are the
substrate temperature, growth time, and chamber pressure. A
true epitaxial growth process would provide many benefits over
simple decomposition. In addition to improved process control
through the potential to vary the carbon flux on the substrate,
it would enable innovative graphene based heterostructures
such as the BisFET proposed by Banerjee et al.[8] This device
would consist of two graphene layers separated by a thin dielec-
tric. Other novel graphene based heterostructures which could
better exploit the bandgap tunabilty of bilayer graphene[9] for
opto-electronic applications might also be possible as well.
Molecular beam epitaxy (MBE) is a well known and widely used
technique for the production of high quality and homogeneous
wafer-scale epitaxial layers. It is highly reproducible with atomic
layer control of thickness and composition. These properties
make MBE an attractive growth method for graphene films. There
have been only a few experimental attempts to grow the graphene
by the evaporation of carbon.[10–12] Logninova et al.[10] focused
[∗] Dr. J. H. Park, Dr. W. C. Mitchel, L. Grazulis, Dr. H. E. Smith,
Dr. K. G. Eyink, Dr. J. J. Boeckl, Dr. D. H. Tomich,
S. D. Pacley, J. E. Hoelscher
Air Force Research Laboratory
Materials and Manufacturing Directorate
AFRL/RXPS, Wright – Patterson Air Force Base, Ohio, 45433 (USA)
E-mail: Jeongho.Park@WPAFB.AF.MIL
DOI: 10.1002/adma.201000756
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on the nucleation and growth of graphene on a metal surface.
Al-Temimy et al.[11] demonstrated the possibility of the graphene
growth by the evaporation of carbon. Hackley et al.[12] claimed
graphitic (amorphous) carbon formation, which is not graphene,
by e-beam evaporation of carbon rod onto a Si (111) surface.
None of these experiments, however, demonstrated the growth
of high quality graphene. Further these experiments focused on
the evaporation of carbon from bulk graphite. We report here the
direct growth of epitaxial graphene on SiC substrates from C60
and bulk graphite filament carbon sources. We demonstrate that
this direct growth approach provides superior quality and homo-
geneous graphene layers. We also show that thickness, structure,
and electronic properties can be controlled by carbon flux, the
types of carbon source, and substrate temperature.
Epitaxial graphene was grown on chemical-mechanical
polished (CMP) on-axis 4H-SiC (0001) substrates by carbon
MBE (CMBE) in an EPI Model 930 MBE system modified for
high temperature growth. Prior to growth a tantalum film was
deposited on the back of all samples for thermal management.
The substrate temperature was monitored with a pyrometer.
Prior to insertion in the chamber the SiC substrates were
cleaned with acetone and methanol, followed by a 10% HF
dip to remove any native oxide. The manipulator of the MBE
system was modified to obtain a maximum temperature of
1600 °C by use of a graphite filament heater powered by a DC
power supply. The substrate holder for all experiments was
further modified by opening the back side to expose the wafer
to the heater so as to increase the maximum temperature that
could be obtained. The carbon molecular beams were obtained
from two different sources. First, C60 was used with a conven-
tional effusion cell to provide a uniform carbon flux.[13] The
carbon flux was measured with an ion gauge. For graphene
growth with C60 and for SiC thermal decomposition growth, in
situ SiC cleaning was performed by exposure to a Si flux from
a high temperature elemental source[13] at a substrate tempera-
ture of 850 °C.[14] After Si flux cleaning the shutter of the Si
effusion cell was closed and the temperature was ramped up
to desired growth temperature. The shutter of the C60 effusion
cell was then opened for the desired growth time after which
the temperature was ramped down to room temperature at a
fixed rate. For comparison, graphene was also grown by SiC
thermal decomposition. As a second carbon source, the same
pyrolytic graphite filament was used simultaneously as both
the carbon source and the substrate heater by inverting the
sample in the open back substrate holder. Graphite filaments
have been widely used as carbon sources for p-type doping
of GaAs.[15,16] Mass spectroscopy studies of the vapor from
heated filaments confirmed that the vapor consists mainly of
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C3 molecules.[17,18] The experiments with the heated graphite shown here). But, as seen in Figure 1b, a slight improvement of

filament used a different procedure from thermal decompo-
sition method and C60 CMBE growth in that the carbon flux
was controlled by changing the current through the filament
and the Si flux cleaning was not employed since the orienta-
tion of the substrate was inverted with respect to the effusion
cells to allow exposure to the carbon flux from the heater. Also,
RHEED could not be used to determine the surface recon-
struction. This does limit the control parameters but further
development could include a separate graphite filament in a
normal configuration as a source. The formation of graphene
was evidenced by a 2D peak in Raman spectra and the appro-
priate C1s peak position in X-ray photoelectron emission
measurements.
The surface morphologies of the films grown by thermal
decomposition and C60 CMBE as measured by atomic force
microscopy (AFM) are shown in Figure 1a–c. The substrate
temperature was kept at 1400 °C for 30 min.. The sample
grown by thermal decomposition shown in Figure 1a under-
goes considerable modification of the surface morphology, such
as significant roughening, the formation of many deep pits
(≥ 1 nm), and the growth of isolated graphene islands (not
Figure 1. AFM images of surface morphology for various growth methods. a) Graphene this layer. Emtsev et al.[19] claimed that the
layer grown on SiC (0001) by conventional vacuum annealing in UHV at 1400 °C for 30 min. broadening of interfacial related peaks are “a
b) Graphene grown on SiC (0001) by carbon MBE (C60 BEP : 5 × 10−8 Torr) at 1400 °C for
30 min. c) Graphene with a higher C60 flux (BEP: 8.5 × 10−8 Torr). Insert: AFM image of 5 μm ×
5 μm scan area. d) Graphene grown by carbon MBE with the graphite filament source (Average that causes inhomogeneous broadening.” The
Input current: ∼53 A) at 1200 °C for 60 min. Insert: the AFM image of graphene by vacuum FWHM in their report ranges from ∼0.85 to
annealing at 1200 °C for 30 min.
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the surface morphology was achieved after C60 CMBE growth
(BEP: 5 × 10−8 Torr). Although the surface is still covered with
pits, their depth is reduced to less than 5 Å. When the surface
was exposed to a higher carbon flux (BEP: 8.5 × 10−8 Torr) the
surface morphology improved even more as seen in Figure 1c,
where atomically flat, pit and island-free graphene terraces are
visible. Wrinkles are found in this sample along and across
the step edges (inset Figure 1c). This indicates that the graphene
film is continuous over the SiC steps. The step height at
the area having broken wrinkles is about 3.3 ± 0.1 Å, which is
the distance between graphene layers in few layer graphene.
The graphene grown by CMBE with the graphite filament
source at 1200 °C for 60 min. is shown in Figure 1d. A filament
current of ∼53 A was required to obtain this substrate tempera-
ture. The insert shows the surface morphology of graphene
grown by thermal annealing at 1200 °C for 30 min. Compared
with the graphene grown by graphite filament CMBE, the sur-
face of the graphene grown by the thermal decomposition has a
higher density of pits and is significantly rougher. Interestingly,
a higher density of wrinkles was formed on the surface. The
wrinkles are uniformly distributed and are connected to each
other to form a hexagonally shaped “wrinkle net” mesh over the
surface. This indicates that the graphene layer
is continuous over the surface.
X-ray photoelectron spectroscopy (XPS)
was used to study the chemical composition
of the layers. The XPS C1s core level spec-
trum of the graphene grown by C60 deposi-
tion (8.5 × 10−8 Torr) is shown in Figure 2a.
This spectrum contains component peaks
from graphene, SiC, interface layers, and an
addition peak located at lower binding energy
region, which is possibly associated with two
coordinated carbon atoms in the SiC sub-
strate (see Supporting Information for more
details). The graphene C1s peak is shifted
∼0.9 eV to higher binding energy than the SiC
peak. These results are in good agreement
with graphene grown by vacuum annealing[19]
and in an Ar atmosphere.[3] The FWHM of
C1s component peak of SiC, which is ∼0.8 eV,
is comparable to that (∼0.75–0.8 eV) of other
groups’ reports.[3,19] The interfacial peak, how-
ever, experiences broadening compared to
other reports[3,19] (See detail in the Supporting
information). The broadening of interfacial
peak might suggest that it contains more
than one component. The carbon atoms in
the interface layer might experience various
local environments due to the disorder prop-
erties of this layer which could result in the
multiple components in the C1s spectra of
consequences of strain in the carbon layers
∼0.9 eV. The FWHM of interfacial C1s peak of

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Figure 2. The properties of graphene grown with C60 (BEP : 8.5 × 10−8Torr) at 1400 °C during 30 min. a) XPS C1s core level spectrum of carbon MBE
grown graphene, showing contributions from the SiC substrate, the graphene layer (shifted by 1 eV from the SiC peak), and an interfacial layers.
b) Raman spectrum (λlaser = 514 nm) of epitaxial graphene grown with C60 (BEP : 8.5 × 10−8 Torr). c) 2D peak of graphene grown by thermal decomposi-
tion. d) 2D peak of graphene grown by carbon MBE with C60 (BEP : 8.5 × 10−8 Torr). e) Raman mapping of 2D peaks over a 1 mm × 1 mm area (λlaser =
514 nm, ∼1 μm spot size, 30 μm spatial resolution.

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our graphene varies from ∼1 to ∼2 eV, which is much broader.
This broadening might be due a combination of the strain
effect and the various local environments of carbon atoms in
the interface layer.
As shown in Figure 2b, the Raman spectrum shows the typ-
ical features of the graphene grown by thermal decomposition,
the 2D peak at 2750 cm−1 and the G peak at 1584 cm−1. The
quality of the film is indicated by a minimal defect related D
peak at about 1325 cm−1. The other features are due to the SiC
substrate. Figure 2c and 2d show Raman 2D peaks from UHV
graphitized and C60 CMBE grown graphene, respectively. The
number of components of the 2D spectrum is a function of the
graphene thickness and the full width at half maximum (FWHM)
of each component should be the same as that of monolayer
graphene in the case of AB or Bernal stacking.[20] Therefore,
the FWHM of the individual components of the 2D peak is
an indicator of the overall quality of the graphene film. Curve
fitting of the spectrum (solid color lines in Figure 2c) shows
that the 2D peak of the graphene grown by thermal decompo-
sition contains four Lorentzian components with FWHM of
36 cm−1, indicating bilayer graphene.[20] CMBE grown graphene
shows that the 2D spectrum is much broader than that of the
graphene grown by thermal decomposition. The fitting (solid
color lines in Figure 2d) shows that it has six components, indi-
cating the growth of trilayer graphene. The FWHM of the com-
ponents are about 31 cm−1, which indicates much improved
quality of the graphene compared to the thermally decomposed
material. Like the thermal decomposition, the 2D peak of the
CMBE grown graphene does not show the shoulder and asym-
metry observed for exfoliated graphene.[21]
With higher carbon flux, we are able to obtain thicker
graphene. The graphene layer thickness in monolayers (ML)
was estimated by using the attenuation model for carbon
photoemission lines from SiC and graphene.[22] The nominal
thickness varies from 1.8 ML to 3.7 ML for C60 fluxes in the
range between 5 × 10−8 and 3.9 × 10−7 Torr. Interestingly, the
graphene to SiC XPS C1s peak ratio (C1sG/C1sSiC) saturated at
a flux of 1.2 × 10−7 Torr which corresponds to about 3.5 ML.
The Raman 2D peaks of the graphene grown with larger carbon
flux (1.2 × 10−7 Torr) consist of only three components, indi-
cating four layer graphene[20] as well. The observed multi-peak
structure of 2D peak with increasing layer number in C60
CMBE graphene is similar to that of Bernal stacked exfoliated
graphene.[20] Therefore, it is likely that the stacking of our C60
CMBE graphene is also Bernal. The FWHMs of the individual
components of the 2D peak as a function of carbon flux show
that lower FWHMs (31 cm−1) were obtained at a flux of 8.5 ×
10−8 Torr, which gives flat, pit free graphene over the surface
(Figure 1c). As the carbon flux is increased, the FWHM experi-
ences significant broadening to 46 cm−1 and then saturates at
higher flux. The analysis of the XPS C1s and the Raman spectra
suggests that C60 CMBE graphene on SiC (0001) has a similar
electronic structure and phonon properties to graphene grown
by thermal decomposition of SiC (0001).
To evaluate the thickness uniformity of the films, we per-
formed Raman mapping as shown in Figure 2e. The meas-
ured 2D peak position depends strongly on the graphene
thickness and can indicate variations in thickness under
proper conditions. It has been shown that the 2D peak energy
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in graphene on SiC (0001) shifts to higher wave number with
increasing thickness whereas for graphene on SiC(0001) the
2D peak shifts to lower wave number with thickness. There-
fore, the mapping of the 2D peak position is a convenient
method to estimate the thickness uniformity of the film.
Figure 2e shows the peak position versus position for a 1 mm ×
1 mm area of CMBE graphene. As can be seen, most of the
material has a peak at 2750 cm−1, indicating that the uni-
formity of the graphene layer over this area is good. The large
up-shift (50 cm−1) of the 2D peak compared to reported few
layer graphene (FLG) grown by thermal decomposition might
be explained by a larger compressive strain in the MBE grown
material.[23]
The rather unorthodox use of the graphite heater as both
carbon source and substrate heater was done to help confirm
that the graphene grown by CMBE was due to carbon depo-
sition rather than SiC decomposition. For the experiment
reported here the filament current was kept at about 53 A,
which resulted in a growth temperature of 1200 °C, below the
common growth temperatures for SiC decomposition growth.
The sample was exposed to the heater for 60 min. To verify
that the graphite heater can be used as the carbon source for
graphene formation, the graphene growth on metal substrate
(4000 Å Ta) was attempted. First, Ta side was placed opposite
the filament. None of the graphene related Raman features
were present, indicating absence of carbon on the surface.
Graphene films, as demonstrated by the presence of a strong
Raman 2D band, were found on the Ta surface facing to the
graphite heater after 30 min at 1200 °C. Therefore, we can con-
clude that the graphene results from deposition of carbon from
the graphite filament
Figure 3a shows the XPS C1s spectrum for graphene grown
by heated graphite filament. The curve fitting results are sim-
ilar to those for C60 CMBE shown above and for UHV- and Ar
atmosphere grown graphene from the literature.[3,19] The C1s
peak consists of a SiC peak from the substrate, a peak due to
sp2 bonded graphene, two interface peaks, and an additional
peak at lower binding energy region (See detail in the Sup-
porting Information). The graphene peak is shifted by 1 eV
from the SiC peak. Interestingly, the C1s position (∼283.8 eV) of
SiC from graphene grown by graphite filament has a peak shift
∼0.4eV lower than that from graphene grown by C60. In addi-
tion, Si 2p3 measurement of SiC substrate showed that there
is peak shift between the two different carbon sources. Si 2p3
from graphene grown by the graphite filament has a peak shift
∼0.5 eV lower than that from graphene grown by C60. Seyller
et al.[22] reported that the change of the surface reconstruction
from 3 × 3 to 6√3 × 6√3 on the SiC surface causes the peak shift
of the SiC bulk components. They claimed the peak shift of the
SiC bulk components results from the change in surface band
bending. Our graphene shows the different doping proper-
ties. The C60 and graphite filament growth result in n-type and
p-type, respectively. Therefore, the change of the surface state
from n-type to p-type might lead to the change of Fermi level
pinning on these surfaces. These might cause the observed
peak shift of SiC bulk components on our graphene samples.
The Raman spectrum in Figure 3b shows the presence
of the 2D peak at 2676 cm−1 and the G peak at 1584 cm−1,
which is also in good agreement with results for the graphene
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Figure 3. XSP and Raman spectroscopy of graphene grown by carbon MBE from a heated graphite filament. a) C1s core level spectrum of graphene
grown at 1200 °C for 60 min. with the graphite heater source. The spectrum consists of four components due to the SiC substrate, the graphene, and
two interfacial layers. b) Raman spectrum (λlaser = 632.8 nm, ∼1 μm spot size) for this sample. c) Raman 2D peak shift as a function of graphene thick-
ness. d) Raman map (λlaser = 514 nm, ∼1 μm spot size, 30 μm spatial resolution on χ and y axes) of graphene grown at 1500 °C for 3 min (∼3.1 ML
nominal thickness). The bulk of the wafer has a 2D peak position at 2710 cm−1 with small islands at either 2705 or 2715 cm−1, indicating the epitaxial
growth of uniform thickness graphene over the large-area surface. Note that the apparent peak shift between Figure 3C and 3D is due to the different
excitation wavelength.

by thermal decomposition and C60 grown graphene. Even
though this growth is on SiC (0001), the 2D peak position
is very close to that of thermally decomposed material on
SiC (0001.[24] Interestingly, the defect-related D peak was
strongly suppressed in this sample, implying a high-quality
film. As seen in the inset of Figure 3b, the 2D peak consists
of a single Lorentzian curve with a FWHM of about 39 cm−1,
characteristic of monolayer graphene. The graphene thick-
ness in these experiments was controlled by the heater and
exposure time up to a nominal thickness of 3.1 ML. Figure 3c
shows the variation of the 2D peak position with different
graphene thicknesses. The peak position undergoes a shift to
lower wave number (about 11 cm−1) as the graphene thick-
ness increases from about 0.8 ML to a nominal thickness of
3.1 ML. Interestingly, the 2D peaks for all graphene samples
grown by the graphite filament technique are composed of a
single Lorentzian component. The single Lorentzian fits sug-
gest that these samples have non-Bernal stacking, indicating
that the graphene layers are electronically decoupled from
each other. The variation of peak position with thickness and
a single Lorentzian 2D line are very similar to the behavior of
the graphene from thermal decomposition on SiC (0001).[24]
This clearly indicates that the graphene grown here with a
graphite filament source has similar electronic structure to
the graphene on carbon face SiC. The single Lorentzian fit
also indicates that our graphene has Dirac-like electronic
states.[24] To estimate the thickness uniformity of these sam-
ples we mapped the 2D peak position of graphene grown for

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3 min at 1500 °C with a 514 nm laser for a 1 mm × 1 mm
area as for the C60 grown material. As seen in Figure 3d, most
of the area has a peak position of about 2710 cm−1 indicating
homogeneous growth over a large area.
To investigate if the structure and graphene properties are
related to the type of carbon sources, the effect of the initial
substrate condition was explored. First, the same initial SiC
substrate was prepared with Si flux cleaning and took out from
the chamber. The orientation of the substrate was inverted to
allow exposure to the carbon flux from the heater. After that,
the sample was immediately reloaded into growth chamber.
The graphene growth was followed at 1200C for 70 min.
XPS data showed that the graphene peak was shifted to
∼1 e V higher energy compare to SiC bulk component. The peak
position of graphene was also the same as that of graphene
on untreated SiC. Thickness of graphene was ∼0.85 ML.
The thickness slightly increases due to the increase the depo-
sition time. The 2D peak was confirmed by the Raman meas-
urement. The position of 2D peak was ∼2686 cm−1, which
is almost identical position to that of graphene grown on
untreated SiC by graphite filament. The surface morphology
of graphene grown on between Si flux treated and untreated
SiC has almost identical feature including hexagonal shaped
“winkle net”. These presumably suggest that the properties
difference is not related to initial surface condition but the
type of carbon sources.
In conclusion, we successfully demonstrated that the direct
deposition of carbon from solid sources, C60 and a graphite
filament, is a promising approach for graphene growth and
produces superior quality, homogeneous graphene layers in
comparison with the thermal annealing method. The direct
deposition of carbon yields atomically flat and pit-free graphene
terraces. Wrinkles along and across the step edges and map-
ping of the 2D peak position indicated homogeneous graphene
growth over the substrate. In addition, the direct deposition
of graphene gave significantly improved controllability of
the graphene growth. The thickness and electronic structure
related to the stacking order could be controlled by C60 flux and
the type of carbon source, respectively. C60 CMBE graphene has
electronic and structural characteristics similar to graphene
(Bernal Stacking) grown on SiC (0001) by decomposition but
the graphite filament CMBE graphene resembled decomposi-
tion grown graphene (Non-Bernal Stacking) on SiC (0001). This
indicates that these differences of electronic structure associ-
ated with stacking order and phonon properties of graphene
might be due to different graphene growth mechanisms asso-
ciated with different the solid carbon sources we used in the
experiment.
Supporting Information
Supporting Information is available from the Wiley Online Library or
from the author.
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Acknowledgements
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The authors wish to thank S. N. Kim for Raman measurement support.
This work was supported by the Air Force Office of Scientific Research
(Dr. Donald Silversmith and Dr. Harold Weinstock).
Received: March 1, 2010
Published online: August 20, 2010
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