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 Nanotechnology

Nanotechnology 27 (2016) 155701 (8pp) doi:10.1088/0957-4484/27/15/155701

Tuning the mechanical properties of vertical

graphene sheets through atomic layer
deposition
Keivan Davami1,2, Yijie Jiang1, John Cortes1, Chen Lin1,
Mehrdad Shaygan3, Kevin T Turner1 and Igor Bargatin1
1
Department of Mechanical Engineering and Applied Mechanics, University of Pennsylvania,
Philadelphia, PA 19104, USA
2
Department of Mechanical Engineering, Widener University, One University Place, Chester,
PA 19013, USA
3
Advanced Microelectronic Center Aachen (AMICA), AMO GmbH, Otto-Blumenthalstraße 25, D-52074
Aachen, Germany

E-mail: kdavami@seas.upenn.edu and bargatin@seas.upenn.edu

Received 25 November 2015, revised 22 January 2016

Accepted for publication 4 February 2016
Published 29 February 2016

Abstract
We report the fabrication and characterization of graphene nanostructures with mechanical
properties that are tuned by conformal deposition of alumina. Vertical graphene (VG) sheets,
also called carbon nanowalls (CNWs), were grown on copper foil substrates using a radio-
frequency plasma-enhanced chemical vapor deposition (RF-PECVD) technique and conformally
coated with different thicknesses of alumina (Al2O3) using atomic layer deposition (ALD).
Nanoindentation was used to characterize the mechanical properties of pristine and alumina-
coated VG sheets. Results show a significant increase in the effective Young’s modulus of the
VG sheets with increasing thickness of deposited alumina. Deposition of only a 5 nm thick
alumina layer on the VG sheets nearly triples the effective Young’s modulus of the VG
structures. Both energy absorption and strain recovery were lower in VG sheets coated with
alumina than in pure VG sheets (for the same peak force). This may be attributed to the increase
in bending stiffness of the VG sheets and the creation of connections between the sheets after
ALD deposition. These results demonstrate that the mechanical properties of VG sheets can be
tuned over a wide range through conformal atomic layer deposition, facilitating the use of VG
sheets in applications where specific mechanical properties are needed.
Keywords: vertical graphene sheets, atomic layer deposition, mechanical properties

(Some figures may appear in colour only in the online journal)

1. Introduction soaking in a solvent [6]. In addition to manipulating their

There is an ongoing effort to tailor the mechanical properties
of one and 2D nanostructures to accommodate the demands
of diverse applications. Various techniques have been repor-
ted for altering the mechanical properties of 2D nanos-
tructures, including alloying [1], addition of a continuous or
non-continuous layer of another material onto the surface of
the nanostructures [2, 3], thermal treatment and annealing [4],
mechanical compression to achieve densification [5], and
mechanical properties, such modifications may also simulta-
neously tune other properties (e.g., electrical and thermal
conductivities), unveiling the connections between the var-
ious characteristics of these low-dimensional materials.
Carbon-based materials, such as carbon nanotubes
(CNTs) and graphene, are among the most studied nanos-
tructures. Due to their unique properties, a significant amount
of research has been devoted to their synthesis, character-
ization, and applications [7–10]. In particular, the mechanical

0957-4484/16/155701+08$33.00 1 © 2016 IOP Publishing Ltd Printed in the UK

Nanotechnology 27 (2016) 155701
properties of CNTs, and their modification, have been the
subject of numerous research studies [11–15]. For instance,
Brieland-Shoultz et al [2] showed that the effective Young’s
modulus of CNT micropillars increased from 14.5 MPa for
uncoated CNTs to 24.5 GPa with 51 nm Al2O3 coating.
Graphene, with its high Young’s modulus, large surface
area per mass, high electrical and thermal conductivity is also
an attractive material for various applications [16]. Although
past research has focused on horizontal graphene, the lesser-
known vertical graphene (VG) structures also have many of
the same desirable properties. VG sheets are nanoscale flakes
of 1–20 layers of graphene that grow almost perpendicular to
a substrate. VG sheets can be inexpensively synthesized
without catalysts on a wide variety of substrates, making them
attractive for many applications. For instance, in the energy
storage field, the unique properties of MnO2/CNW/Ni
hybrid electrode make it an interesting material to be used in
environment friendly, inexpensive and high-performance
electrical energy storage devices [17]. It was also shown that
by depositing silicon on CNWs, their electrochemical per-
formance is significantly enhanced, which makes them a
potential candidate for lithium-ion batteries’ 3D anode mat-
erial [18]. This 3D silicon-decorated nanowall framework can
minimize the lithium diffusion length and more effectively
collect charge, leading to better cycling performance at high
rates [18]. CNWs can also be employed in fuel cells since
Pt(Cu)st/CNW catalyst has low Pt content and high specific
surface [19]. In the chemical and biological area, CNWs
improve surface enhanced Raman scattering (SERS), which is
a powerful surface analysis tool for chemical and biological
single-molecule detection and molecular diagnosis [20, 21]. It
was reported that ultrasensitive SERS substrates can be fab-
ricated by decorating silver nanoparticles on thin CNWs or
coating CNWs with thin silver film [20, 21]. Seo et al [22]
demonstrated that gold- and palladium-decorated honey-VG
sheets offer reliable sensing performance for Au tagged
antibodies as well as H2. In the optical domain, the ultra-low
reflectance, superior light absorption and high specific
absorption optical properties of VG sheets grown on silicon
and copper make them potential candidates for outstanding
lightweight light absorbers for solar concentrators, or as a
coating for bolometers [23, 24]. In addition, a novel approach
was introduced by Davami et al [25] to manufacture VG-
based nanocomposite thin films with uniform dispersion and
improved mechanical properties.
The behavior of VG sheets under mechanical loading has
not been studied so far. Herein, we study their mechanical
behavior using instrumented indentation and investigate how
conformal coating with Al2O3 can be used to tune their
mechanical response. Al2O3 was chosen as the coating mat-
erial since it can be uniformly coated on the VG sheets with a
precisely controlled thickness. Additionally, it also features a
high stiffness, chemical and high-temperature resistance, as
well as a remarkably conformal and pinhole-free properties
when it is deposited through the atomic layer deposition
(ALD) method [26].
2
K Davami et al
2. Experimental method
An RF-PECVD technique was used to grow VG sheets [27].
The copper substrates were cut into small pieces and after
cleaning with acetone, IPA, and DI water were dried with N2.
Copper was chosen as the substrate since VG sheets grow on
copper more uniformly and with a smaller variation in heights
and angles compared to other substrates (Si, Si covered with
Au, etc). In order to clean the chamber before the VG
synthesis, an oxygen plasma cleaning process for a period of
90 min was conducted. The copper pieces with an approx-
imate dimension of 1 cm×1 cm were placed on a stage
inside the chamber. The pressure of the chamber and the stage
temperature were set to be 680 °C and 1 Torr, respectively,
while the RF power was maintained at 900 W. Hydrogen and
methane with a 1:1 ratio were introduced into the chamber to
ignite the plasma. The growth process was continued for
40 min and at the end of the process, the samples were cooled
down in vacuum to room temperature to avoid their oxidation.
ALD deposition of Al2O3 was performed using a Cambridge
NanoTech Savannah tool. The two precursors used were tri-
methylaluminum (TMA), which serves as the source of alu-
minum, and water, which serves as the source of oxygen. The
deposition was performed at a relatively low temperature of
80 °C in order to assure that the mechanical and chemical
properties of the carbon nanowalls remained unchanged
during the process. Each cycle consisted of a 0.015 s exposure
of water, a 30 s chamber evacuation, a 0.015 s exposure of
TMA and finally, another 30 s evacuation of the chamber.
Using this recipe, each cycle deposited approximately 0.1 nm
of aluminum oxide on the substrate. This deposition rate was
confirmed by measuring the thickness of deposited aluminum
oxide on a flat piece of silicon with a Filmetrics F50 thin-film
thickness mapping tool. Films with thicknesses of 5.0, 7.5 and
10.0 nm were made using this method.
Indentation tests were conducted with a Hysitron TI-950
TriboIndenter® using a spherical diamond indenter with a
radius of ∼59.5 μm. This large-radius indenter was used in
order to measure the average mechanical response of the
surface over many VG nanowalls. The indentation experi-
ments were performed under load control. The load function
included ten cycles of loading and unloading at each location.
In each unloading segment (except for the final one, which
was unloaded completely) the sample was unloaded to 5% of
the peak load that was applied in the previous loading seg-
ment. The peak load was increased by 16 μN in each load–
unload cycle; the peak load in the first cycle was 16 μN and
the peak load in tenth cycle was 160 μN. Each loading and
unloading segment had duration of 2 s. On each sample, the
ten-cycle indentation test was repeated at 25 different loca-
tions. The locations were separated by 80 μm and arranged on
a 5×5 grid.
3. Results and discussion
A scanning electron microscope (SEM—JEOL 7500
HRSEM), working at 5.00 kV, was used to image and study
Nanotechnology 27 (2016) 155701
Figure 1. Top view (a) and cross section (b) SEM images of pure VG sheets as well as top view of VG sheets with a 5 nm (c) and 10 nm (d)
thick Al2O3 coating. The scale bars in all images are 200 nm.
the morphology of the VG sheets before and after deposition
(figures 1(a)–(d)). VG sheets have a wavy geometry due to
the stress induced during the growth process (figure 1(a))
[27]. As can be seen in the cross-section image in figure 1(b),
most of the sheets had a leaf shape morphology and were
nearly perpendicular to the Cu substrate with a height of
around 400–500 nm. Figures 1(c) and (d) show top-view
SEM images of VG sheets coated with Al2O3 with a thickness
of 5 nm and 10 nm, respectively. As can be seen here, a 5 nm
thick ALD layer does not significantly change the morph-
ology of the VG sheets, while a 10 nm thick coating makes
the VG array more similar to cellular foam. For ALD layers
thicker than ∼15 nm, the precursors could no longer effec-
tively penetrate between the sheets, as the ALD layer on top
thickened and closed off entry points to the precursors,
forming a non-uniform ‘crust’ on top of the sheets. For this
reason, we limited the mechanical measurements to the VG
samples with coatings that were 10 nm in thicknesses or less.
The Raman spectra of pristine VG sheets was measured
using an NT-MDT NTEGRA system with an excitation
3
K Davami et al
wavelength of 532 nm, an exposure time of 10 s, and a laser
power of 0.2 mW. As can be seen in figure 2, four main peaks
were observed: D (∼1330 cm−1), G (∼1580 cm−1), D′
(∼1620 cm−1) and 2D (∼2660 cm−1). It should be noticed
that the D peak in VG sheets usually has a high intensity due
to the significant number of the edges [27].
Figure 3(a) shows force–displacement plots for an
uncoated specimen as well as a specimen coated with a 5 nm
thick alumina layer. After ALD coating, the VG sheets
became stiffer, and a higher load was required to induce the
same deformation (figure 3(b)). For example, a 2, 4.5, and
10 μN force was required to achieve a 5 nm displacement in
pure, 5 nm thick, and 10 nm thick samples, respectively.
The contact stiffness was calculated from force–dis-
placement curves based on the slope of the unloading seg-
ment [28]. Figure 4(a) shows the contact stiffness of the ALD
coated and bare samples change with the peak load and alu-
mina thickness. The contact stiffness is expected to increase
with increasing load as the contact area between the sample
and the spherical indenter increases with indentation depth. At
Nanotechnology 27 (2016) 155701 K Davami et al

Figure 2. Raman spectra of pristine vertical graphene sheets.

Figure 3. (a) A comparison of force–displacement curves for a bare VG surface and a VG surface coated with a 5 nm thick alumina layer. (b)
Force–displacement curves of bare and coated samples with different thicknesses of alumina.

the lowest load of 16 μN, the stiffness of the bare samples
(∼2 μN nm−1) was smaller than that of the ALD coated ones
(∼3 μN nm−1), but the error bars of all measurements overlap
significantly. Over the full range of loads, the ALD coated
samples clearly have a higher stiffness than the bare samples
and a trend of increasing stiffness with increasing alumina
thickness is also observed. The enhancement in stiffness and
modulus may be explained by stronger interlocking and
coupling of VG sheets due to the alumina coating as well as
an increase in the bending stiffness of individual VG sheets
due to the coating, similar to what has been observed for
CNTs [2].
The effective Young’s modulus of the VG structured
surfaces can be extracted from the nanoindentation mea-
surements. In order to do this, a mechanics model, which
relates the indentation force and depth to one another as a
function of the indenter geometry and specimen modulus, is
required. Classical nanoindentation analyses, which assume
that the specimen being indented is a homogenous elastic
half-space, are not appropriate here as the surface being
indented consists of VG flakes that are only weakly connected
in-plane. As a result, the effective elastic modulus was cal-
culated based on an assumption that the sample acts as an
array of vertical springs that is being compressed axially
under the indenter. The effective Young’s modulus is the
normal stress in the material under the indenter divided by the
effective normal strain. The stress and strain in the contact
vary radially because of the spherical geometry of the tip, thus
in this analysis the area beneath the indenter is divided up into
ring-shape differential areas (figure 5). The stress on this ring
of material is defined as the force on the material, dF, divided
by the area of the ring, dA. The strain on this ring of material

4
Nanotechnology 27 (2016) 155701 K Davami et al

Figure 4. (a) Contact stiffness as a function of nanoindentation load for samples with different ALD thicknesses and (b) Effective Young’s
modulus as a function of peak load for samples of varying thickness of ALD.

test (i.e., the total force over the contact area) is:
a2 d (r )
F= ò dF = ò0 E
h (r )
2pr dr

⎡ 0 (d2 - d1) r dr
= 2pE ⎢ò
⎢⎣ a1 h 0 + R - d1 - R 2 - r 2

a1 R 2 - r 2 - (R - d 2 ) ⎤
+ ò r dr ⎥ , (2 )
a2 h0 ⎥⎦

where R is the tip radius, h0 is the original height of sample,

Figure 5. A schematic showing the model used for determination of
Young’s modulus from the measured force–displacement curves.
is defined as the vertical deformation of the material d, divi-
ded by the height of the VG film, h. The effective elastic
modulus is thus:
dF dA
E= . (1 )
d h
Assuming that the effective Young’s modulus is the same
for all differential areas, the force measured in the indentation
a1 and a2 are the contact radius after and before an unloading
segment, and d1 and d2 are the contact depth after and before
unloading (figure 5).
The ALD-coated VG sheets form a complex composite-
like structure. As the VG sheets deform via bending when
indented, coating with an alumina layer with a high Young’s
modulus (∼130 GPa), substantially increases the bending
stiffness of the VG sheets, which scales with thickness cubed,
and leads to a significant increase in the effective Young’s
modulus of the structure. Figure 4(b) shows the effective
Young’s modulus as a function of the applied load for both
pure and ALD alumina-coated samples. For all four samples,
the effective Young’s modulus reduces with increasing load.
This can be attributed to local buckling of the thin graphene
sheets during compression. Buckling is commonly observed
in in situ compression tests of CNTs [29]. In contrast to flat
indenters typically used in previously reported CNT tests, the
spherical indenter in our tests will gradually cause more and
more sheets to buckle with increasing load. Thus, a plateau in
the force–displacement curve is generally not seen in our
data; instead, buckling manifests itself as a gradual decrease
of effective Young’s modulus with increasing peak load. For
the smallest peak loads (∼16 μN), pure VG samples displayed
an effective Young’s modulus of just above 100 MPa. In

5
Nanotechnology 27 (2016) 155701
Figure 6. (a) Energy absorbed and (b) strain recovery versus the applied load for pure and coated samples. The error bars were calculated
based on the standard deviation of the 25 measurements on the sample at each load.
contrast, coated samples featured a Young’s modulus on the
order of 260 MPa (an almost threefold increase) under the
same loading conditions. The Young’s modulus depends on
the coating thickness. For example, at a peak load of 16 μN,
the sample with a 10 nm thick ALD coating has a Young’s
modulus that is ∼20 MPa larger than that of the sample with
an alumina thickness of 7.5 nm (270 MPa versus 250 MPa).
At a peak load of 160 μN load, the difference in modulus
between the 7.5 and 10 nm thick coating was about ∼15 MPa
(95 MPa compared to 80 MPa). On average for all loads, the
Young’s modulus increased by 25 MPa as the ALD coating
thickness was increased from 5 to 7.5 nm, and by 45 MPa
when the coating thickness went from 5 to 10 nm.
Figure 6(a) shows the energy absorption per unit volume
for pristine and coated samples. The energy absorbed was
estimated as the area of the hysteresis loop divided by the
volume of material under the indenter (the compressed
volume). As can be seen here, the energy absorption
decreases with increasing thickness of the alumina coating,
but increases with increasing applied load. Similar to the
mechanical deformation of arrays of CNTs, the hysteresis can
be attributed to the energy absorbed as a result of the inter-
action of VG sheets with each other and the friction between
them as well as viscous dissipation attributed to the airflow
during unloading [3]. The coating is believed to decrease the
energy absorption because it increases the stiffness of the VG
sheets and roughens the surface of the VG sheets, which
prevents adhesion.
Finally, figure 6(b) shows the strain recovery for the pure
and coated samples. The strain recovery was defined as the
fraction of the recovered displacement in the unloading seg-
ment to the displacement in the corresponding loading
segment. The strain recovery was calculated for each
6
K Davami et al
load–unload cycle. In all of the samples, the strain recovery
increased with an increase in the applied load, but was typi-
cally smaller in coated VG sheets than in pristine VG sheets.
This is in contrast to previously reported measurements of
CNTs, where graphene petals as well as ALD alumina coating
enhanced the strain recovery [2, 3]. The opposite behavior
observed here can be attributed to the differences between an
array of CNTs and VG sheets. When CNTs are compressed,
they bend, buckle, and adhere to each other during densifi-
cation, resulting in a small strain recovery. ALD coatings can
reduce the adhesion between individual CNTs and therefore
enhance the strain recovery [2]. Likewise, adding spring-like
petals between neighboring CNTs results in a bigger strain
recovery of the array [3]. In contrast, pristine VG sheets
buckle and interact with each other much less under a load
due to larger spacing between the sheets. Thus, coated VG
sheets do not show enhanced strain recovery. Instead, adding
a brittle material such as alumina to the VG sheets make them
more brittle. In addition, ALD deposition might lead to ‘spot
welded’ points between the sheets that cannot accommodate
large strains and thus fracture when indented.
We note that according to our previous TEM study of the
VG sheets [27], VG sheets typically consist of 10–20 layers,
with the spacing between the layers equal to 3.5±0.05 Å.
Thus, the thickness of the VG sheets and ALD coating is in
the same range. On the other hand, the spacing between the
sheets is much larger than the thickness of the ALD coating.
Therefore, the ALD coating does not form a continuous bulk
material. The fact that the measured mechanical properties of
the samples continue to change with the thickness of the ALD
layer, even for the thickest coatings, also confirms that our
measurements are not dictated by the properties of just
alumina.
Nanotechnology 27 (2016) 155701
4. Conclusion
Tailoring the properties of nanostructures through coating
creates opportunities to expand their applications. Tuning the
mechanical properties of VG sheets may lead to lightweight
bulk materials with enhanced mechanical behavior. In this
research, VG sheets were synthesized using an RF-PECVD
method and coated with different thicknesses of atomically
deposited alumina. The mechanical properties of pristine and
coated samples were studied using nanoindentation. The
deposition of a 5 nm thick alumina layer results in nearly a
three-fold increase in the effective Young’s modulus com-
pared to the pristine samples. In contrast to CNTs, the
deposition decreased the strain recovery of the VG sheets.
This is attributed to the significant differences in morphology
between arrays of CNTs and VG sheets. Overall, the results
here show how the mechanical properties of VG sheets may
be tuned using conformal coating with nanoscale layers.
Acknowledgments
This work was supported, in part, by the School of Engineering
and Applied Science at the University of Pennsylvania and a
seed grant of the Center of Excellence for Materials Research
and Innovation (CEMRI), NSF grant DMR11-20901.
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