Rapid synthesis of nanocrystalline ZnO by a microwave-assisted combustion method
L.C. Nehru
a
, V. Swaminathan
b
, C. Sanjeeviraja
a,
⁎
a
School of Physics, Alagappa University, Karaikudi 630 002, India
b
School of Materials Science and Engineering, Nanyang Technological University, 639798, Singapore
abstract article info
Article history:
Received 22 December 2011
Received in revised form 9 March 2012
Accepted 24 March 2012
Available online 30 March 2012
Keywords:
ZnO
Nanocrystalline
Combustion
Microwave
Synthesis
A facile and rapid microwave-assisted combustion method (MWAC) was developed to synthesis to produce
nanocrystalline ZnO powder using dissolution of zinc nitrate (as the oxidant) and urea (as fuel) as the
starting materials and water as solvent, then heating the resulting solution in a microwave oven. The study
suggested that application of microwave heating to produce the homogeneous porous ZnO was achieved in a
few minutes. The structure and morphology of the as-prepared combustion products were investigated by
means of X-ray powder diffraction (XRD), Fourier transform infrared spectra (FTIR), Raman spectra, UV–Vis
absorbance spectra and Scanning electron microscopy (SEM). The XRD, FTIR and Raman spectra confirmed
the formation of hexagonal wurtzite structural ZnO and the SEM results indicated the porous surface
characteristic of the products. The as-prepared powders have larger band gap energy (3.06 eV) and are
described here.
Crown Copyright © 2012 Published by Elsevier B.V. All rights reserved.
1. Introduction
The fabrication of transition metal oxides with nano structure has
been the target of scientific interests in recent years because of their
unique properties and fascinating applications in optoelectronics,
devices and biomedical science [1]. Among these oxides, zinc oxide
nanostructure has attracted considerable interest in many areas of
chemistry, physics and material science. It's having attracted extra
attention due to their broad range of applications in sensors [2],
catalysts [3], solar cells [4], transparent conductive oxides [5],
optoelectronic devices [6] piezoelectric devices [7] antibacterial
treatment [8] and additive in many industrial products. So the
researchers exert much effort in continuing to focus on investigating
them for technological applications due to their unusual physical and
chemical properties, which differ significantly from those of conven-
tional bulk materials from the standpoint of their extremely small
size or large specific surface area. Generally nanoscale particles
possess different physical, chemical properties, better sinter ability,
and larger catalytic activity and other unique properties may be
expected because their nano-sized crystallites are high surface area
with different surface defect properties etc. So the technological
importance of ZnO has motivated several studies on the synthesis of
this material using various methods, such as pulse laser deposition
[9], vapor phase transparent process [10], thermal evaporation [11],
aqueous solution deposition [12], template-based growth [13],
combustion synthesis [14], sol–gel [15], chemical vapor deposition
[16] and vapor transparent deposition have been developed for the
preparation of nano ZnO [17]. However, these methods require
specific apparatus, vacuum conditions and chemical costs, respec-
tively. Microwave irradiation as a heating method has found a
number of applications in chemistry. The utilization of microwave
irradiation in the preparation of nano particles has been reported in
recent years [18]. Compared to the conventional methods, the
microwave synthesis has the advantages of producing small particle
size metal oxides with high purity owing to short reaction time
[19–23].
Microwave-assisted synthesis is a novel method to produce
materials, since microwave heating is an in situ mode of energy
conversion and the microwave heating process is fundamentally
different from conventional heating processes. Heat will be generated
internally within the material, instead of originating from external
sources. By means of this method, many functional materials and
compounds with novel structures and properties have been obtained
[24]. In the recent studies, it has been shown that nanoparticles such
as Co
3
O
4
[25], LiMn
2 - x
Cr
x
O
4
[26], SnO
2
[27] Ce
1-x
Gd
x
O
2-1/2x
[28],
MgO [29], ZnO [30] and Ni
x
Co
1 - x
Fe
2
O
4
[31], can be prepared by the
microwave synthesis process.
In this paper, we report a simple method for the preparation of
hexagonal ZnO nanoparticles by using microwave-assisted combus-
tion synthesis process to fast, mild, energy-efficient and environmen-
tally friendly rout to produce ZnO nano particles using urea as fuel.
2. Experimental
All the reagents used in the experiments were analytically pure
and were purchased from MERCK Company, and were used as
Powder Technology 226 (2012) 29–33
⁎ Corresponding author.
E-mail address: sanjeeviraja@rediffmail.com (C. Sanjeeviraja).
0032-5910/$ – see front matter. Crown Copyright © 2012 Published by Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2012.03.042
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