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RESEARCH PAPER
Phase transition in a single VO2 nano-crystal: potentialfemtosecond tunable opto-electronic nano-gating
M. Maaza • A. Simo • B. M. Itani •
J. B. Kana Kana • S. El Harthi • K. Bouziane •
M. L. Saboungi • T. B. Doyle • I. Luk’yanchuk
Received: 10 October 2013 / Accepted: 1 April 2014 / Published online: 1 May 2014
� Springer Science+Business Media Dordrecht 2014
Abstract The first-order semiconductor–metal Mott
transition in single nano-crystal of VO2 has been
observed using scanning tunneling spectroscopy. The
variation of the band gap Eg with an external thermal
stimulus on a single VO2 nano-crystal in the temper-
ature range of 293.5–361.0 K is reported for the first
time. The corresponding tuneable I–V characteristics
versus temperature could be applied in thermally or
optically tunable electronic nano-gating in the femto-
second regime in view of the ultrafast dynamic in VO2.
Keywords VO2 � Mott transition � Single
nano-crystal � Band gap � Scanning tunneling
spectroscopy � Opto-electronic nano-gating �Instrumentation
Introduction
Vanadium dioxide (VO2) manifests an ultrafast fem-
tosecond first-order semiconductor/metal (SM) phase
transition at the vicinity of TC * 340.8 K. Below TC,
the band gap Eg is approximately 0.70 eV. Above TC, it
closes (Eg = 0 eV) inducing a considerable reduction
in the electrical resistivity by several orders of
magnitude ‘‘larger than 107 for the bulk material’’
(Morin 1959; Mott 1968; Zylberstejn and Mott 1975;
Adler 1966; Goodenough 1971). This electronic phase
transition is related to a reversible sharp crystallo-
graphic modification: monoclinic and tetragonal below
and above TC (Felde et al. 1997; Eyert 2002). The
tetragonal rutile (P42/mnm) structure has chains of
M. Maaza (&) � A. Simo � B. M. Itani �J. B. Kana Kana � S. El Harthi � K. Bouziane �M. L. Saboungi � T. B. Doyle � I. Luk’yanchuk
College for Graduate Studies, University of South Africa,
Muckleneuk Ridge, P O Box 392, Pretoria, South Africa
e-mail: [email protected]
M. Maaza � A. Simo � B. M. Itani � S. El Harthi �K. Bouziane � M. L. Saboungi � T. B. Doyle �I. Luk’yanchuk
Nanosciences African Network (NANOAFNET),
iThemba LABS-National Research Foundation of South
Africa, 1 Old Faure Road, Somerset West,
Western Cape 7129, South Africa
J. B. Kana Kana
Department of Materials Science & Engineering,
University of Arizona, Tucson, AZ 85721, USA
S. El Harthi
Department of Physics, College of Sciences, Sultan
Qaboos University, Muscat Masqat, Oman
M. L. Saboungi
Centre de Recherche sur la Matiere Ultradivisee, CNRS,
Orleans, France
T. B. Doyle
School of Chemistry and Physics, University of KwaZulu-
Natal, Durban 4001, South Africa
I. Luk’yanchuk
LPMC, Universite de Picardie Jules Verne, 33, rue St Leu,
80039 Amiens, France
123
J Nanopart Res (2014) 16:2397
DOI 10.1007/s11051-014-2397-z
edge-shared VO6 octahedra along the c-axis and the V–
V distance along the chains is 0.2851 nm, while in the
monoclinic (P21/c) crystal structure, the dimerized
vanadium atoms have alternate V–V distances of
*0.2619 and *0.312 nm.
From a theoretical point of view, this SM phase
transition has been interpreted initially in terms of
Mott–Hubbard transition as well as electrons trapping
in homopolar bonds (Goodenough 1971; Eyert 2002).
The recent laser ultrafast spectroscopy investigations
shed lighted on the dynamic of such a phase transition
(Cavalleri et al. 2004; Lysenko et al. 2006). Using a
femtosecond laser pump-probe geometry, the relaxa-
tion processes in VO2 indicated that the light-induced
SM phase transition was as fast as the laser pulse
duration itself (*100 fs). As reported in Fig. 1, the
possible mechanism in relation to the phase transition
may be due to changes in the 3d band configuration
associated with the crystal structure variation. The
upper d||, unoccupied in the semiconductor phase is
within the empty broad p*-band, while strongly
hybridized with oxygen 2p-orbitals and lying above
the Fermi level EF. In the metallic phase, however, all
3d-bands are close to the Fermi level. Upon the laser
pump excitation, the main transitions are from the
occupied d||-valence band to the unoccupied d||–p*
mixed conduction band followed by resonant transi-
tions to unoccupied excited states of the metallic phase.
As a result, the screening of the charge transfer by the
conduction electrons in the metallic phase takes place
by ultrafast laser excitation. The complementary recent
work of Lysenko et al. (2006) indicated that upon an
ultrafast laser excitation, an instantaneous response in
the transient reflectivity and transmission is induced
followed by a relatively longer relaxation process. The
observed phase transition has been associated with the
optical interband transition in VO2. As a consequence
of such a femtosecond reversible MS phase transition,
the optical dielectric constant and thus the refractive
index of VO2 exhibit a temperature modulation which
translates in a large reversible optical modulation in the
infrared spectral region specifically. This singular and
unique property of VO2 makes it a candidate of choice
for smart windows applications, thermal sensors,
optical switching devices, field effect transistors and
electro-optical gates as well as ultrafast tunable nano-
plasmonics, and optical limiting nano-scaled opto-elec-
tronic devices among others (Fan et al. 1977; Gal’perin
et al. 1998; Klimov et al. 2002; Rivera et al. 2009; Maaza
et al. 2000, 2005a, b, 2012; Chen et al. 2004; Balberg and
Trokman 1975; Sella et al. 1998; Wang et al. 2005a, b;
Tsai et al. 2006; Bouchiat et al. 2009).
While extensive studies were conducted on VO2 in
terms of synthesis and investigations of its physical
properties as well as its potential opto-electronic
technological applications, very limited studies were
performed on the variation of its electronic bandgap
Eg(T) in its nano-structured form (Yin et al. 2011;
Adler et al. 1967; Neuman et al. 1964; Kosuge 1967;
Appel 1968; Bongers 1965; Koide and Takei 1967;
Goodenough 1960, 1965; Ladd and Paul 1969; Adler
1966; Sasaki and Watanabe 1964; Zylberstejn and
Mott 1975). For our best knowledge and relatively to
the published literature including the recent work of
Yin et al. (2011), this contribution reports the first
experimental results of the thermal variation of the
Eg(T) of a single VO2 nano-crystal. Likewise, it
demonstrates the possibility to engineer ultrafast and
tunable VO2-based opto-electronic nano-gates.
Experiments and discussion
To perform the intended transport investigations in
single nano-crystals of VO2, it is necessary to engineer
Fig. 1 Reversible opening/closing of the VO2 bandgap versus
external thermal stimuli such as temperature according to Adler
et al. (1967). The phase transition involves mainly d|| and p*
electronic orbitals
2397 Page 2 of 8 J Nanopart Res (2014) 16:2397
123
crystalline VO2 films below the coalescence threshold
i.e., consisting of crystallographically textured isolated
nano-particles. Hence pulsed laser deposition was
considered as the technique of choice (Maaza et al.
2000). The target was a pressed powder pellet
(*15 mm in Ø and *2-mm thick) of pure VO2
(Johnson–Matthey 99.99 %). Laser ablation was carried
out in vacuum at a base pressure of*7.5 9 10-8 mbar
with the target rotating at *225 rpm under the XeCl
excimer fundamental laser radiation. F:SnO2-coated
float-glass substrates (5 9 5 9 1 mm3) were used as
transparent electrodes. The coated substrates were
rotated at the same speed as the target, while heated to
a temperature of *674 K. The laser ablation fluence
was adjusted using a quartz lens. The depositions were
carried out at a repetition rate of *10 Hz for a total
number of cycles ranging from 300 to 6,000 in the
fluence range of 0.7–3.2 J/cm2 (Maaza et al. 2000,
2012). The optimal fluence of*1.32 J/cm2 allows high
quality stoichiometric single-phase thermochromic
VO2 nano-crystals. Using the optimal conditions, five
samples of VO2 thin films on F:SnO substrates with
thicknesses of *27 ± 5 nm, 64, 151, 409, and
1,218 ± 2 nm were prepared. This thickness range
which was based on a previous study was considered to
obtain discontinuous and continuous films below and
above the percolation threshold of the VO2 nano-
crystals.
Then, VO2 films surface topology was investigated
using atomic force microscopy (AFM) in the contact
mode. With the exception of the thinnest film
(*27 ± 5 nm in thickness), the other samples (64,
151, 409, and 1,218 ± 2 nm in thickness) showed
almost identical surface morphology as reported in
Fig. 2a which indicates a continuous network of quasi-
spherical nano-crystals with a polydisperse diameter
distribution. Figure 2b reports the surface morphology
of the thinnest VO2 film (*27 ± 5 nm). It indicates a
system of quasi-isolated nano-crystals with an obloid-
like shape anisotropy. The statistical scans provide
average dimensions of *469 ± 12 9 103 ± 9 9
29 ± 7 nm. More accurately, the average height value
of *29 ± 7 nm was obtained from additional statis-
tical measurements over about 30 horizontally posi-
tioned VO2 nano-crystals. One could notice that it is
comparable to the average thickness of the thinnest
film itself (i.e., 27 ± 5 nm), and hence could be
considered as a discontinuous film of single grains.
This thin film sample will be used for the measurement
of the temperature dependence of the I–V characteris-
tics of individual/single VO2 nano-crystals, and hence
the change in the band gap Eg(T) through the SM
transition is as described below.
Fig. 2 AFM surface topography of the thickest (1,218 ± 2 nm,
continuous film) and thinnest (the *27 ± 5 nm, discontinuous,
below percolation threshold) VO2 films in tapping mode
J Nanopart Res (2014) 16:2397 Page 3 of 8 2397
123
To make certain that all films consist of pure VO2,
X-rays diffraction (XRD) and resistivity (R(T)) inves-
tigations were performed on all films. Figure 3a, b
reports the typical XRD and R(T) profiles of the
thickest VO2 films (in this case VO2 film with thickness
of *1,218 ± 2 nm), respectively. These results are
representative of all five samples including the thinnest
discontinuous film. For this latter (i.e., 27 ± 5 nm), as
it was expected, the XRD Bragg peaks and the
resistance/cm2 were broader and larger, respectively.
From the XRD spectra, the room temperature mono-
clinic M1 VO2 phase is confirmed via the presence of
the distinctive (110) Bragg diffraction peak located at
approximately 27.8� corresponding to an average
lattice parameter values of a & 0.5791 nm,
b & 0.4531 nm, and c & 0.5486 nm. From the
R(T) transport perspective, the two orders of magnitude
decrease in the electrical resistance at T & 335 K
(from about 5 9 105 to 7 9 103 X) indicates a (but
incomplete) semiconductor (M1 VO2 phase) to metal
(tetragonal rutile-type structure) phase transition.
Likewise, the stoichiometry of the VO2 films was
further investigated by means of Rutherford Backscat-
tering experiments which gave a ration of vanadium/
oxygen in the range 0.48–0.51 range (±5 %) which
concurs with the stoichiometric value of 0.5.
Scanning tunneling spectroscopy (STS) measure-
ments were performed on the various VO2 film
samples using a Brucker unit equipped with an in-
situ heating stage in the range of 298–573 K with an
accuracy of 0.1 K. The experimental set-up is illus-
trated in Fig. 4 for the thinnest discontinuous film.
STS scans over a representative area of about 1 mm 9
1 mm at temperatures below and above the SM
transition temperature Tc, more precisely at about
338.7 and 361.0 K, respectively, for the thickest VO2
film (1,218 ± 2 nm) are shown in Fig. 5a, b, respec-
tively. Spatial drift due to thermal effects has been
eliminated so that the two figures report the same area/
group of nano-crystals. The surface density of states
(SDS) of Fig. 5 and their spatial distribution were
studied by measuring the I–V characteristics in the
voltage interval from -1 to 1 V by single-point STS
averaging over *15 times of I–V scans in each spot
and grid measurements. The grid for which the
measurements were carried out consisted of a matrix
of 445 9 445 pixels (surface 1.5 9 1.5 nm2). The I–
V curves were taken at each pixel with a bias voltage of
*0.207 V. The results from this time intensive
measurements are illustrated in Fig. 5. Areas where
the occupied electronic states are close to the Fermi
energy, in particular, areas in the metallic state, have
higher tunneling currents and show as dark regions
(gray to black color).Predominantly insulating to a
metallic surface is clearly seen in the evolution of the
images of Fig. 5 as observed by Qazilbash et al. (2007)
by SNOM on thick VO2 films. The white areas
correspond to the semiconducting phases, while the
gray–black regions match up with the metallic VO2
phases. As it can be observed, the cover surface of the
gray–black regions is somehow equivalent to the
white ones at 338.7 K just at the vicinity of TC. This
seems indicating that the Mott phase transition, yet
incomplete, takes place at slightly lower temperatures
20 30 40 50 60 700.0
2.0k
4.0k
6.0k
8.0k
10.0k (33
4)
(60
0)
(52
2)
(43
2)
(22
4)
(51
0)
(42
1)
(42
0)
(00
4)
(41
1)
(40
0)
(31
1)
(31
0)
(22
0)
(10
2)
(21
1)
(11
0)
Inte
nsi
ty (
cps)
2Θ (Deg)
+++: VO2(A)
(a)
(b)
Fig. 3 Typical a XRD and b transport R(T) profiles of the
pulsed laser deposited VO2 thin films onto F:SnO2-coated float-
glass substrate
2397 Page 4 of 8 J Nanopart Res (2014) 16:2397
123
than the bulk value of TC * 341.5 K. Above TC i.e.,
361 K, while almost all of the scanned surfaces are
conducting (gray–black regions), one could notice that
there are still semiconducting domains (white
regions). This could be due either to the amorphous
nature of the surface layer surrounding some of the
VO2 nano-crystals or their oxygen sub-stoichiometry
or to their surface strain/stress. In all three cases, this
surface layer would act as a resistive component and
hence would affect the effective value of the bandgap
Eg(T) of the single VO2 nano-crystals. As it was
evidenced by Wei et al. (2009), the surface strain
phenomenon affects significantly the metal–semicon-
ductor phase transition of VO2. Theoretically, this was
sustained previously by Luk’yanchuk et al. (2009),
while investigating the origin of ferroelastic domains
in free-standing single crystal ferroelectric films. The
near field scanning microwave microscopy investiga-
tions in strained quasi 2-D VO2 nano-platelets by
Tselev et al. (2010a, b) have evidenced the interplay
between ferroelasticity and the SM phase transition as
well as the strain-induced transition between the
insulating M1 and M2 and metallic R phases of VO2.
More precisely, it was demonstrated that the compe-
tition between several phases is purely driven by the
lattice symmetry. Considering the XRD results of
Fig. 3a, it is worth to point to the possibility of co-
existence of both M1 and M2 VO2 phases with the M1
and M2 nano-crystals being crystalline and amor-
phous, respectively. If so, the semiconducting (white)
domains observed at 361 K could be due to the M2
VO2 nano-scaled domains that would not transit
electronically.
In terms of bandgap Eg of a single VO2 (M1) nano-
crystal and its temperature dependence, which is the
cornerstone of this communication, quantitative
assessments by STS have been conducted via I–
V single point measurements in the discontinuous i.e.,
thinnest VO2 film on single isolated nano-crystals of
Fig. 4 The STS configuration to be used to conduct the single
particle I–V measurements on single VO2 nano-crystals in
granular film far from the percolation threshold
Fig. 5 STS of the percolated VO2 film (here the thickest film,
1,218 ± 2 nm in thickness): a just below TC (338.5 K) and
b above TC (358.5 K)
J Nanopart Res (2014) 16:2397 Page 5 of 8 2397
123
VO2. The bandgap Eg is determined from the exten-
sion of the flat section at the center of the dI/dV STS
characteristics, while the spatial distribution of band-
gaps can be visualized by setting a threshold tunneling
current at a set voltage in the dI/dV curves from the
grid measurement. One should mention that Eg values
determined from the flat section are systematically
smaller by 0.1–0.3 eV than if one uses the inflection
point method (Yin et al. 2011). The tunneling thresh-
old current at a set voltage is linked to Eg, which has
been confirmed in a large number of I–V characteristics
of several semiconductors. Figure 6 reports the mea-
sured I–V characteristics for a single isolated single
nano-crystal of VO2 in the thinnest discontinuous film
of 27 ± 5 nm as shown in the inset figure. The I–
V profiles of Fig. 6 have been measured at 298.5,
323.5, 338.5, and 358.5 K. The used tunneling current
was in the range of 0–15 nA for an applied DC voltage
varying from 0 to 2.5 V. At T = 358.5 K i.e., above
Tc, the I–V characteristic is approximately linear, i.e.,
ohmic, pointing to a metallic behavior. At T \ Tc
(298.5, 323.5, and 338.5), the I–V characteristics
exhibit a semiconductor behavior of the investigated
isolated nano-crystal with the width of the ‘‘plateau’’
region being approximately equal to 2 9 Eg(T). As it
can be noticed, width of the plateau and the band gap
Eg(T) vary rapidly at the vicinity of TC. This temper-
ature variation of Eg(T), derived from the standard
derivative dI/dV for various temperatures for the
thinnest discontinuous film, is distinctly illustrated in
Fig. 7. Eg(T) temperature evolution can be splitted in 3
different regions. In region I, Eg(T) decreases almost
linearly, while in region III, its evolution in nearly
inverse exponential with temperature reaches zero
value close to 358.5 K. In region II (temperature range
of 330–340 K), i.e., in the vicinity of TC, it decays
sharply. This trend of Eg(T) in region II could certainly
be correlated to the singular 1st order phase transition
of VO2. However, one should point out 2 major
concerns: (i) the value of Eg(T) in the room temper-
ature range and (ii) the observed temperature variation
of Eg(T) itself. Concerning the values of Eg(T) within
the room temperature range, even with the experi-
mental bar error of ±10 %, the experimentally derived
values of Eg at 298.5 K and at 323.5 K are about
*0.93 and *0.81 eV, respectively, i.e., quite larger
than the bulk value of about 0.7 eV. This difference
could be due to the STS approach itself [23] or/and
either to 3 other major causes. As it was mentioned
previously, the bandgap value Eg deduced from the I–
V flat section is analytically different by 0.1–0.3 eV
than if one uses the inflection point method. This first
source of error has been minimized as the deduced
Eg(T) values were averaged using in fact both I–V and
dI/dV derived values. The 3 additional causes are as
follows: (i) the amorphous nature of the surface layer
surrounding the investigated VO2 single nano-crys-
tals, (ii) its oxygen sub-stoichiometry due to surface
effects such as breakdown of the 3-D symmetry and
atomic coordination, and (iii) its oxygen sub-stoichi-
ometry due to their the strain/stress. In all three cases,
this surface layer would act as a resistive component
and hence would affect the effective value of the
bandgap of the single VO2 nano-crystals. This surface
layer seems to exist in view of the inset zoom of the I–
V curve at 358.5 K. Indeed, the zoom shows clearly
that the I–V evolution is not a complete ohmic type. In
addition, in regard to the recent studies on VO2, the
surface strain hypothesis should be considered too. As
it was evidenced by Wei et al. (2009), the surface
Fig. 6 a Typical I–V curves on a single VO2 nano-crystal in the
non-percolated/discontinuous film at various temperatures:
298.5, 323.5, 338.5, and 358.5 K, b the isolated nano-crystal
on which the measurements were carried out
2397 Page 6 of 8 J Nanopart Res (2014) 16:2397
123
strain phenomenon affects significantly the metal–
semiconductor phase transition of VO2. This was
sustained theoretically by Luk’yanchuk et al. (2009)
while investigating the origin of ferroelastic domains
in free-standing single crystal ferroelectric films. The
near field scanning microwave microscopy investiga-
tions in strained quasi 2-D VO2 nano-platelets by
Tselev et al. (2010a, b) have evidenced the interplay
between ferroelasticity and the metal–semiconductor
phase transition symmetry relationship as well as the
strain-induced transition between the semiconducting
M1 and M2 and metallic R phases of VO2.
From technological applications point of view,
Fig. 6 supports confidently the possibility of using
such a device for ultrafast tunable opto-electronic
gating as the SM reversible transition of the VO2 nano-
crystals can be induced optically in the femtosecond
regime (Cavalleri et al. 2004; Lysenko et al. 2006;
Maaza et al. 2012). Likewise, such an applied aspect is
being extended to engineer tunable ultrafast devices for
surface-enhanced Raman spectroscopy via bang gap
engineering of core shell oxide/VO2 nano-structures
(Balakumar and Ajay Rakkesh 2013; Durgalakshmi
and Balakumar 2013; Parthiban et al. 2013; Ajay
Rakkesh and Balakumar 2013).
Conclusion
The contribution reported on the thermal variation of
the bandgap Eg(T) of VO2(M1) single nano-crystals
synthesized by pulsed laser deposition in a tempera-
ture range below and above the Mott phase transition
taking place at TC * 340.8 K, more precisely in the
range of 298.5–358.5 K. Such a bandgap Eg(T) vari-
ation was deduced from STS via I–V and dI/dV profiles
on single VO2(M1) crystalline nano-particle in a
discontinuous VO2(M1) thin film below the percola-
tion threshold. The variation of Eg(T) at the vicinity of
TC seems to concur with Adler’s crystalline distortion
model. From the technological application perspec-
tive, this contribution has demonstrated the possibility
to engineer reversible and tunable VO2 nano-scaled
femtosecond opto-electronic gates.
Acknowledgments This research program was generously
supported by grants from the National Research Foundation of
South Africa (NRF), the French Centre National pour la
Recherche Scientifique, iThemba LABS, the UNESCO-
UNISA Africa Chair in Nanosciences & Nanotechnology, the
Organization of Women in Science for the Developing World
(OWSDW) and the Abdus Salam ICTP via the Nanosciences
African Network (NANOAFNET) as well as the African Laser
Centre (ALC) to whom we are grateful.
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