Article

pubs.acs.org/JPCC

Role of Carrier Gas Flow and Species Diffusion in Nanowire Growth

from Thermal CVD
Andreas Menzel,*,† Raya Goldberg,‡ Guy Burshtein,‡ Victor Lumelsky,‡ Kittitat Subannajui,†
Margit Zacharias,† and Yeshayahu Lifshitz*,‡
†
Laboratory for Nanotechnology, Department of Microsystems Engineering, University of Freiburg, Freiburg 79110, Germany
‡
Faculty of Materials Engineering, and Russel Berrie Nanotechnology Institute Technion, Israel Institute of Technology, Haifa 32000, Israel

ABSTRACT: A variety of nanowires can be grown in a tube furnace via the transport of evaporated species by a carrier gas
toward substrates. The insufficient understanding and the resulting limited control typical for this research area motivated us to
systematically study the distribution of the growth species in such processes and evaluate its effect on the nanowire growth.
Calculations based on simple considerations as well as more sophisticated numerical (COMSOL) simulations were utilized to
follow the time evolution of the species distribution at different carrier gas pressures and flow rates. We demonstrate that the
balance between diffusion and convection must be appropriately tuned to ensure steady growth conditions (not achieved in
many of the previously reported experiments). Experimental data of Si and ZnO nanowires growth is presented and supports the
simulations. Insight into the appropriate design of nanowires growth experiments and a universal basis to compare between the
results of different laboratories are provided.

1. INTRODUCTION combines calculations with experimental data aiming at achieving

Nanowires (NWs) of different materials are considered excellent
candidate materials to serve as building blocks of future
electronic and optoelectronic devices.1−6 Realization of this
goal necessitates reproducible and controlled growth processes
capable of tailoring the structure, morphology, and size of these
NWs to meet specific demands. A common way of growing
NWs is by thermal CVD, i.e., evaporation of growth species and
their transport by a carrier gas to the substrates on which they
nucleate and grow.7−12 In spite of the huge amount of work
reporting the growth of NWs from thermal CVD the role of the
growth parameters still remains unclear. The researchers use
different system geometries8,10 (e.g., one tube, an inner tube
inside an outer tube, different tube diameters) and a variety of
growth conditions (temperature, carrier gas flow and pressure).
It is very difficult to compare between studies performed by
different groups and establish a reliable and reproducible
correlation between growth conditions and the NWs structure
and properties obtained. The present work addresses the
distribution of the growth species in the CVD chamber. It
a better insight of the role of specific parameters (e.g., geometry,
flow and pressure) on the NWs growth. It shows that frequently
used growth parameters lead to unsteady growth conditions (e.g.,
change of concentration of growth species with time). It also
indicates that procedures used to improve and stabilize the grow
conditions are based on wrong concepts. Note that the under-
standing of the transport mechanisms in NW growth is essential
for the development of controlled, reliable and reproducible large
area processes for commercial applications.
The assessment of the distribution of the growth species was
performed first by simplified calculations of the two major
processes determining the distribution of the growth species,
i.e., diffusion and convection. Such rough calculations are useful
in evaluation of the general behavior of the process under
specific conditions. In addition, a more accurate analysis was
Received: December 31, 2011
Revised: January 31, 2012
Published: February 1, 2012

© 2012 American Chemical Society 5524 dx.doi.org/10.1021/jp212635w | J. Phys. Chem. C 2012, 116, 5524−5530
The Journal of Physical Chemistry C
performed by numerical calculations using the COMSOL
software.13 Studies of NWs growth (of both Si and ZnO) by
thermal CVD at different locations were performed, varying the
carrier gas flow and pressure conditions and correlated to the
calculations to demonstrate the effect of the species distribution
on the NWs growth. Si and ZnO were chosen as very different
experimental study case systems both playing a central role in
current NWs research,1−12 allowing to check the generality of
the present work. Note that the only two previously reported
studies14,15 attempting to simulate the ZnO NW growth
process (applying COMSOL14 and ANSYS15 software) were
preliminary in their nature. The comprehensive combination of
calculations, simulations, and experimental data of the present
study provides insight and practical guidelines for future studies
of NW growth.
2. EXPERIMENTAL DETAILS
The thermal CVD system consisted (Figure 1) of a cylindrical
quartz tube (inner diameter 56 or 29 mm, 1500 mm long) in a
Figure 1. Schematic description of the thermal CVD growth system.
three zone horizontal furnace (900 mm long) pumped by
a turbo system to a base pressure better than 10−6 mbar. The
three zone furnace enabled constant temperature (±10 °C)
in the central zone and in most of the side zones (the sharp
temperature gradient between the central and side zones as
well as between the side zones and the cold edges of the
furnace depended on the rather constant temperature of each
zone). The Si NWs growth was performed by evaporation of a
SiO powder placed at the central heating zone (1100 °C)
while 5 nm thick Au deposited sapphire and Al2O3 substrates
were put in the outer zones (900 °C at downstream and
upstream positions) at different distances from the source
along the central axis of the tube. A 56 mm inner diameter
quartz tube was applied. Ar was used as a carrier gas at a
pressure of 25 mbar and a flow of 50 sccm. Similarly, ZnO
growth was performed using a mixed ZnO/C powder (1:1
weight ratio) placed at the central heating zone (950 °C), and
again, 5 nm thick Au deposited sapphire and Al2O3 substrates
were placed at different distances from the source in both the
upstream and downstream side zones (heated to 800 °C). Two
inner tube diameters were used for ZnO NW growth, 56 and
29 mm, to be able to probe the effect of the tube diameter on
the gas transport. Ar was used as a carrier gas at a pressure of
30 mbar and flows of 30−150 sccm (56 mm tube) and 9−45
sccm (29 mm tube), respectively. The morphology of the NWs
grown was investigated with a high resolution scanning
electron microscope (HRSEM).
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3. NUMERICAL MODEL
For numerical calculations (applying the COMSOL software13)
the transport of the species at laminar flow conditions (Reynolds
number ≪4000) is described by the general transport equation
∂ρc
+ ∇·(ρuc⃗ ) = ∇·(Γ∇c) + R (1)
∂t
with ρ the density of the mixture, u⃗ the velocity field, c the
concentration of the growth species, and Γ the diffusity which is
described as ρ·D of the mixture.16 The terms ∇·(ρuc⃗ ), ∇·(Γ∇c),
and ∂ρc/∂t describe the convection, diffusion, and transient
behavior, respectively, while R is the source term present.15,17
The binary system is modeled for Zn−Ar interaction for ZnO
NW growth but can be also adapted to the SiO-Ar system in case
of Si NW growth. The velocity field u⃗ of the carrier gas flow is
calculated from the Navier−Stokes equation,13,18 and the
temperature profile inside the CVD chamber is determined by
the heat convection and heat conduction equations.18,19 The
ZnO system was chosen for the simulations assuming a constant
Zn generation rate that was evaluated from the amount of Zn
source material consumed in the process.
4. RESULTS AND DISCUSSION
A conventional experimental sequence of NWs growth includes
the following steps: (1) pumping down the CVD system, (2)
introduction of the carrier gas to a specific pressure at a fixed
flow rate, (3) heating of substrates to the appropriate substrate
temperature, (4) heating of the source to the appropriate
source temperature (start of growth), (5) cooling of the source
to the substrate temperature (end of growth), and (6) cooling
of the system to room temperature. Such a process involves
uncertainties in both the start and end of the growth, since the
source evaporates at the heating and cooling stages in varying
rates and not just at the desired source temperature. This is
why some researchers now use the so-called pressure shutter
method (applying high carrier gas pressure during heating and
cooling and introducing the desired process pressure only when
the source is at the appropriate temperature), or reverse the
flow direction in the heating and cooling stages.20,21
Under stable growth conditions (source temperature, sub-
strates temperature, carrier gas flow rate and pressure), it is
obvious that the distribution of the growth species is determined
by the balance between evaporation rate, diffusion (occurring in
all directions) and the convection (occurring dominantly only in
the flow direction). Assuming that the evaporation rate at a
given temperature is constant, the typical diffusion distance is
given by z = 2(Dt)1/2 where D is the diffusion coefficient and t is
the diffusion time. D at temperature T [K] and pressure p can
be evaluated by D at normal conditions22 (Dn, 1 bar, 300 K)
since D = Dn(T/Tn)3/2/(p/pn). The subscript n denotes normal
conditions (1 bar, 300 K). The advance of the flowing front x
can be calculated by x = [f(T/Tn)t]/[(p/pn)S] where f is the
flow rate, t the advance time, and S the cross section of the
reactor cylinder. Table 1 presents a comparison between the
diffusion length z and the advance distance x at two typical
experimental conditions (p = 30 mbar or 200 mbar at T =
1173 K and f = 10−30 sccm) after 1 min (beginning of growth)
and 30 min (end of growth). It is obvious that at the beginning
of the growth process the diffusion is equally or more effective
in distributing the growth species than the convection while
the convection becomes more dominant only at the end of the
process. This result has significant implications on the CVD
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Table 1. Comparison between the Diffusion Length z and

the Advance Distance x at Two Typical Experimental
Conditions
800 °C, 200 mbar, 10−30 sccm 800 °C, 30 mbar, 10−30 sccm
1 min 30 min 1 min 30 min
z (cm) 28.5 156 73.6 402
x (cm) 8.9−26.8 268−805 59.7−179 1788−5365

growth process. The first is that an upstream distribution of

growth species and a consequent upstream growth of NWs are
possible in principle. A second is that both the pressure shutter
and the reversed flow approaches may be ineffective in
elimination of growth during the heating and cooling periods.
Another way of a crude estimation of the relative roles of
diffusion and convection is by calculation of the Peclet number
(Pe) given by Pe = L(V/D). L is the characteristic length, V the
convection front velocity and D the diffusion coefficient.
The convection is much more effective than the diffusion for
Pe ≫ 1 only. The characteristic length L for which Pe = 1 is given
by L = Dn(T/Tn)1/2/(f/S). Note that the tube is at 300 K at both
its ends (where the pressure and flow are measured) and is at the
growth temperature (say 800 °C) at the hot part of the tube, so
that under constant pressure along the entire tube the convection
velocity at the hot zone is (T/Tn) times larger than at the cold
parts. Also note that the convection velocity scales with (f/S)
and not with f. For our typical growth conditions (30 mbar,
30 sccm, 800 °C) the characteristic length L for which Pe = 1 is
9.3 cm, i.e., the convection is dominant for L ≫ 9 cm (the
convection is dominant only for L ≫ 28 cm for 10 sccm).
COMSOL13 simulations were performed using the geometry
of our CVD system and applying a variety of growth conditions
(experimental temperature profile, source evaporation rate,
different carrier gas flow rates, and different pressures) to Figure 2. (a) Time evolution of Zn species inside the three-zone
furnace from 0 to 20 min at 30 mbar and 30 sccm carrier gas flow rate
evaluate the distribution of the growth species in the reactor
and (b) time evolution of Zn species inside the three-zone furnace
versus time. Figure 2a presents the evolution of the distribution from 0 to 20 min at 30 mbar and 100 sccm carrier gas flow rate.
of the Zn species with time (up to 20 min) for typical conditions
employed by reported works (30 mbar, 30 sccm).21 The Zn
species reach both downstream and upstream regions: upstream
merely due to diffusion and downstream due to both diffu-
sion and convection. The concentration at a certain position
increases with time but does not reach saturation even after
20 min. A saturation of the concentration profile after a short time
of ∼1 min is obtained only for much higher flows (of 100 sccm
for 30 mbar, see Figure 2b) indicating that steady state
conditions (Zn evaporation rate equals Zn removal rate) are
achieved. The concentration profile along the tube axis in the
downstream direction (in both panels a and b of Figure 2)
becomes constant after some time indicating that the convection
front reached the tube end. In contrast, the concentration
profile in the upstream direction is decreasing with the distance
from the source since the convection by the flowing carrier gas
transports the diffusing Zn species backward toward the
downstream direction. Figure 3 presents the distribution after
10 min for a fixed pressure (30 mbar) but using different flow Figure 3. Zn species distribution inside the three-zone furnace depending
on several carrier gas flow rates ranging between 1 and 100 sccm at
rates. The concentration at a certain point in the downstream 30 mbar after 10 min.
direction decreases with increasing flow. This results from the
raise of the flow front velocity with the increase of the flow rate concentration does reach saturation after a short time of ∼1 min
so that the Zn species are transported faster from the CVD (Figure 2b).
system. In the upstream direction the Zn species reach shorter Figure 4 shows the effect of the pressure on the species
distances upon increasing flow rate since the diffusing species distribution for a fixed flow (30 sccm). At low pressures both
are removed faster by the carrier gas flow. Note, that at the diffusion and the flow front velocity are large, thus the
sufficiently high flow rates (e.g., 100 sccm for 30 mbar) the concentration is constant with the distance from the source in
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Figure 4. Zn species distribution inside the three-zone furnace depending
on several pressures ranging between 1 mbar and 1000 mbar at 30 sccm
carrier gas flow rate after 10 min.
both (downstream and upstream) directions. As the pressure
increases both the diffusion and the flow front velocity become
smaller, resulting in a large concentration gradient in both
directions. While the pressure increases the Zn species spend
more time in the system before being pumped so that the Zn
concentration (at a fixed time) increases with increasing pressure.
When the pressure shutter approach20,21 is used and the pressure
is increased to say 1 bar, the Zn species are accumulated near the
source (though some diffuse in both downstream and upstream
directions and some convection in downstream directions also
exists). The reduction of the pressure to start growth (which is
the second stage of the pressure shutter approach) increases the
diffusion (in both the upstream and downstream directions) and
the convection (in the downstream direction only) so that
nonsteady conditions (Zn concentration first increasing with
time then decreasing with time at a fixed point) occur.
We conclude from the above analysis that under experi-
mental conditions where diffusion and convection are domi-
nant the NW growth should occur in upstream and down-
stream directions simultaneously. This was indeed observed for
both the ZnO and the Si NWs growth (HRSEM micrographs in
Figure 5). The Si NWs growth from SiO9,11,12 and the ZnO NWs
Figure 5. ZnO and Si NWs grown at 190 mm from the source both
downstream and upstream. No change of the morphology or density is
observed, indicating the dominant role of diffusion with respect to
convection.
growth from a ZnO:C mixture7−9,15,21,23 are completely
different processes. In the first, SiO vapor is generated and
disproportionates on the Au catalyst SiO → Si + SiO2. The Si is
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dissolved in the catalyst and upon the increase of its
concentration in the catalyst droplet it precipitates below the
droplet to form a Si NW nucleus which is embedded in a SiO2
sheath. The growth is thus via a vapor liquid solid (VLS)
process in which the growth species transported in the gas
phase are SiO species.12 The heating of the ZnO/C powder in
the second system applied7−9,15,21,23 (in addition to the Si
system), however, initiates carbothermal reactions which can
be described as ZnO + C → Zn + CO and ZnO + CO → Zn +
CO2 . Zn is carried to the Au catalyst onto which it reacts with
either O2 or CO or CO2 to form ZnO. The formation of ZnO
NWs may be purely catalyst free due to the anisotropy of
the ZnO crystal (catalyst free vapor solid (VS) growth9,23). The
nucleation of the ZnO NW may also be catalyst assisted with a
catalyst free VS growth driven again by the ZnO anisotropy.23
The catalyst assisted growth of ZnO NWs via a classical vapor
liquid solid mechanism (VLS)9 however is most unlikely. Such
a mechanism requires Zn dissolution in the catalyst, its
precipitation at the interface between the catalyst and the
substrate/growing NW (when the Zn concentration exceeds the
solubility limit), and its oxidation to form a ZnO NW. No solid
phase however exists for the Au−Zn system at the temperatures
of 800−900 °C as applied by us.23 It was suggested23 that the
ZnO NW growth may be catalyst assisted nucleation and catalyst
assisted growth in a vapor solid solid (VSS) process in which
ZnO molecules diffuse on the catalyst surface and incorporate in
the interface between the substrate and the catalyst reducing the
surface energy.23 The growth species for ZnO NWs evolution via
carbothermal reactions are thus a complex mixture of Zn, ZnO,
CO, CO2, and O2, very different from the single component SiO
vapor involved in the present SiNW growth. The similar
downstream and upstream distributions of the Si and ZnO NWs
observed (for an identical reactor and similar flow and pressure
conditions) support the validity of our simulations in assessing
NW growth by thermal CVD.
We further studied the ZnO NWs distribution under different
flow conditions and different tube diameters. The data obtained
using a tube diameter of 56 mm shows that an increasing flow
(100 and 150 sccm) shortened the distance in the upstream
direction in which ZnO NWs were grown (compared to
30 sccm), but does not affect the distance in which NWs were
detected in the downstream direction (HRSEM micrographs in
Figures 6 and 7). Similarly, the distance in which NWs were
grown in the upstream direction was reduced upon increasing
the carrier gas pressure (not shown here) as previously antic-
ipated by the calculations. In the third stage of our experiments
we checked the distribution of the ZnO NWs in a 29 mm ID
tube in three different flows (9, 30, 45 sccm) keeping the f/S
values applied for the experiments with the 56 mm ID tube
(30, 100, and 150 sccm, respectively). Note (Figures 8 and 9)
that the morphologies and distributions of the ZnO NWs in both
downstream and upstream directions are indeed similar for
different tube diameters once the f/S values are preserved. A full
description of the Si and ZnO NWs growth is beyond the scope
of the here presented publication.
The calculations and simulations presented in this work are
a first order simplification of the actual processes taking place
in the CVD reactor. They assume that the growth species
concentration is not affected by the deposition on the system
surfaces (leading to the NWs growth). Such a deposition might
lead to a decrease of the growth species concentration with
increasing distance from the source. The simulations indicate
that the vapor species velocities near the reactor system surfaces
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Figure 6. HRSEM micrographs of Al2O3 substrates arranged in different locations from the source downstream (indicated on the left side of the
figures), with ZnO NWs grown at temperatures of 950 (source) and 800 °C (substrates) at 30 mbar for 60 min at Ar flow rates of 30, 100, and
150 sccm. The tube diameter was 56 mm.

Figure 7. HRSEM micrographs of Al2O3 substrates arranged in different locations from the source upstream (indicated on the left side of the
figures), with ZnO NWs grown at temperatures of 950 (source) and 800 °C (substrates) at 30 mbar for 60 min at Ar flow rates of 30, 100, and
150 sccm. The tube diameter was 56 mm.

(walls, substrates) are significantly lower than along the center of
the tube, and the angle of incidence on the substrates also vary.
The possible effects of the species velocities and angle of
incidence on the deposition efficiency were neglected as well (a
previous work20 claims that NW growth is enhanced when the
5528
substrate is perpendicular to the carrier gas flow direction). The
ZnO NW growth via carbothermal reactions involves a complex
mixture of species which may differ in different locations of the
system. An indication of such an effect is the growth of longer and
more aligned NWs in the upstream direction (Figures 5−9 and ref 15).
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The Journal of Physical Chemistry C Article

Figure 8. HRSEM micrographs of Al2O3 substrates arranged in different locations from the source downstream (indicated on the left side of the
figures), with ZnO NWs grown at temperatures of 950 (source) and 800 °C (substrates) at 30 mbar for 60 min at Ar flow rates of 9, 30, and
45 sccm. The tube diameter was 29 mm.

Figure 9. HRSEM micrographs of Al2O3 substrates arranged in different locations from the source upstream (indicated on the left side of the
figures), with ZnO NWs grown at temperatures of 950 (source) and 800 °C (substrates) at 30 mbar for 60 min at Ar flow rates of 9, 30, and
45 sccm. The tube diameter was 29 mm.

The preferred growth of ZnO NWs in the upstream direction
was attributed in a previous report to an optimized
concentration of O2 in the upstream direction, while its con-
centration in the downstream direction was either too low or
too large.15 By controlling the O2 concentration, the growth
5529
can be either in upstream or in downstream position.9,15 A
detailed and accurate analysis of all processes occurring in a
thermal CVD NW growth system is very complicated and
needs much more significant efforts in future studies. Note that
this work focused on the understanding of the species
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The Journal of Physical Chemistry C Article

distribution in CVD systems and did not treat the issue of the
optimal species concentration needed for the growth of a certain
nanomorphology (nanowires, nanorods, nanobelts, tripods etc.).
The actual morphology obtained would depend on a variety of
parameters (nanomaterial grown, substrate type, substrate
temperature, growth species used) dictating a different
optimal concentration for each set of parameters.
The present (simplified) work nevertheless demonstrates that
an analysis of the species distribution in the CVD reactor is
most helpful in understanding the NW growth at different
locations of the CVD system, and the effect of carrier gas flow,
pressure and evaporation time. The experimental conditions
(flow rate, pressure, and systems diameter) can be tuned to
balance between the effects of diffusion and convection. This
provides control and enables the determination of the con-
centration profile inside the tube furnace. The time for steady
growth conditions (i.e., species saturation) can be estimated.
It is obvious that under experimental conditions used by many
groups (e.g., 30 mbar, 30 sccm)21,23 the concentration of the
growth species significantly varies with time (Figure 2a). Hence
it does not allow a controlled growth sequence under steady
conditions (as seen in figure 1b for 30 mbar, 100 sccm). The
analysis of the growth species distribution enables an evaluation
on how effective an approach is in terms of stabilizing growth
conditions (e.g., pressure shutter or the change of flow direction).
The analysis is also essential for a meaningful comparison
between experiments of different groups, conducted using
different geometries and experimental conditions.
5. CONCLUSIONS
In summary, the distribution of growth species in thermal CVD
systems used to grow NWs was assessed using simplified
calculations and numerical (COMSOL) simulations. It was
shown that the balance between diffusion and convection of
the growth species is governed by the carrier gas flow. The
investigation indicates that both upstream and downstream
growths of NWs are possible as indeed experimentally observed.
The role of carrier gas flow rate and pressure was evaluated in
terms of determining the species distribution and confirmed by
experimental data. The here suggested approach is helpful for
designing growth experiments and achieving a better control
over the NW growth process.
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■ AUTHOR INFORMATION
Corresponding Author
*E-mail: shayli@tx.technion.ac.il (Y.L.); andreas.menzel@
imtek.uni-freiburg.de (A.M.).
Notes
The authors declare no competing financial interest.

■ ACKNOWLEDGMENTS
The authors acknowledge the German Research Society (DFG)
for the project funding (ZA 191/28-1, Ll 1832/1-1) within the
DIP (German Israel Cooperation Program), and the partial
support of the Russel Berrie Nanotechnology Institute at
Technion.

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