International Journal of Materials Science ISSN 0973-4589 Volume 12, Number 1 (2017)
© Research India Publications http://www.ripublication.com
One step and facile hydrothermal synthesis of hexagonal molybdenum
trioxide nanorods and its photo response
Himanshu Mishra
Department of Physics, Institute of Science,
Banaras Hindu University,
Varanasi, Uttar Pradesh, India.
Anchal Srivastava
*
Department of Physics, Institute of Science,
Banaras Hindu University,
Varanasi, Uttar Pradesh, India.
*
Corresponding author
Email: anchalbhu@gmail.com
Abstract
Present study reports the one pot facile synthesis of metastable
hexagonal phase of molybdenum trioxide (h-MoO
3
) using
ammonium heptamolybdate (AHM) as starting material and
HNO
3
as reducing agent. The synthesized nanostructures are
nanorods in shape having length ~ 50 μm and diameter ~ 200
nm. The samples have been characterized by using X-ray
diffractometer (XRD), scanning electron microscopy (SEM),
transmission electron microscopy (TEM) and Raman
spectroscopy. The photoresponse of micrometer thick h-MoO
3
film on glass substrate also have been studied. It was found
that the amount of photocurrent increases with increase in the
frequency of the incident radiation.
Keywords: MoO
3
, nanorods, photocurrent.
Introduction
Since last few decades, nanostructures have gained much
attention in the field of energy, electronics, optical and
sensing applications [1, 2]. Various transition metal oxides
have been extensively studied in this regards [3, 4]. Among
various transition metal oxides molybdenum oxide (MoO
3
) is
one of the most studied materials. As we know, MoO
3
exists
in three different phases, orthorhombic (α-MoO
3
), hexagonal
(h-MoO
3
) and monoclinic (β-MoO
3
). Among these three, α-
MoO
3
is the most studied as it is thermodynamically stable
phase and exhibits a unique layered structure which permits it
to be cleaved easily along their basal planes [5-7]. h-MoO
3
is
a metastable phase whose basic building unit is a distorted
MoO
6
octahedron to form layered structure through corner-
sharing mode. Two adjacent layers of h-MoO
3
are joined
together with weak Vander Waals forces [6]. Sometimes
metastable phases provide much novel and enhanced results in
comparison to their thermodynamically stable structures but
their synthesis is usually difficult. Till date, several methods
for the synthesis of h-MoO
3
have been reported [8-10]. But
there are very few reports about its photoresponsivity. So, a
facile and fast synthesis route and its photoresponsivity need
further investigation.
Present study focuses the one pot, facile and fast synthesis of
h-MoO
3
using hydrothermal method. A micrometer thick film
of h-MoO
3
have been prepared onto a glass substrate using
nebulizer coating method and photoresponse of the h-MoO
3
film have been studied.
Methods
Ammonium heptamolybdate ( (NH
4
)
6
Mo
7
O
24
, AHM) and
nitric acid (HNO
3
) have procured from Hi-Media, India. All
the chemicals were of analytical grade and used without any
further purifications. Throughout the experiment de-ionized
(DI) water has been used for the solution preparation. Ethanol
has been used for the dispersion of h-MoO
3
for thin film
deposition.
In a typical hydrothermal synthesis route of h-MoO
3
, 4.8 g of
AHM is dissolved in 68.8 ml of DI and stirred for 10 min. at
40ᴼC to make a transparent solution. After that 11.2 ml of
HNO
3
has been added to this transparent solution and again
stirred for 10 min. at 40ᴼC. After that the solution is
transferred into a stainless steel lined Teflon autoclave having
capacity 100 ml and put for the hydrothermal reaction for 8
hrs. at 180ᴼC (figure 1). After the completion of th e reaction
the light white precipitate has been filtered and washed thrice
with DI and ethanol. The filtered and washed precipitate has
been dried for 8 hrs. at 60ᴼC. Finally the dried sample has
been crushed into tiny powder form.
67