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Synthesis and Characterization of Zinc Oxide Nanoparticles using Zinc Acetate

Dihydrate and Sodium Hydroxide

Article · December 2015

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Industrial Research and Consultancy Centre University of Khartoum
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Journal of Nanoscience and Nanoengineering
Vol. 1, No. 4, 2015, pp. 248-251
http://www.aiscience.org/journal/jnn

Synthesis and Characterization of Zinc Oxide

Nanoparticles using Zinc Acetate Dihydrate and
Sodium Hydroxide
Dalia Ahmed Mohammed Osman1, Mustafa Abbas Mustafa2, *
1
Department of Chemical Industries Research, Industrial Research and Consultancy Centre, Khartoum, Sudan
2
Department of Chemical Engineering, Faculty of Engineering, University of Khartoum, Khartoum, Sudan

Abstract
Low-temperature aqueous chemical growth methods have shown great potential in the synthesis of ZnO nanostructures.
Hexamethylenetetramine (HMTA) is the most common chemical substance used in the hydrothermal synthesis. In this study
zinc oxide nanoparticles were prepared via hydrothermal growth using zinc acetate dihydrate and sodium hydroxide, as
precursors instead of HMTA, as it is commercially available and cheap. Crystal structure and grain size of the obtained
nanoparticles were characterized by X-ray diffractometer. Scanning electron microscopy (SEM) has been used to study the
morphological features of the ZnO nanopowder. The results obtained show that this hydrothermal synthetic method can
produce good quality ZnO nanoparticles.

Keywords
Zinc Oxide, Nanostructures, Hydrothermal Synthesis, Morphological Effect

Received: September 17, 2015 / Accepted: December 17, 2015 / Published online: December 29, 2015
@ 2015 The Authors. Published by American Institute of Science. This Open Access article is under the CC BY-NC license.
http://creativecommons.org/licenses/by-nc/4.0/

the compound. Low-temperature aqueous chemical growth

1. Introduction
Nanotechnology can be understood as a technology of
design, fabrication and applications of nanostructures and
nanomaterials, as well as fundamental understanding of
physical properties and phenomena of nanomaterials and
nanostructures [1-2]. Metal oxides nanostructures play
crucial role in many areas of chemistry, physics and materials
science [3]. The different properties of oxides enable the
numerous applications in the fabrication of microelectronic
circuits, sensors, piezoelectric devices, fuel cells, coatings
against corrosion and as catalysts (most catalysts involve an
oxide as active phase).
ZnO is an important metal oxides that could be easily grown,
environmental friendly and of interest to many applications.
It is suitable for industrial, technical and medical applications
due to its diverse properties which have been found to
strongly depend on their morphology [4] and thus has been
the subject of study by many researchers. This has led to the
development of a great variety of techniques for synthesizing
method has been shown to be a high performance growth
technique for ZnO nanostructures, due to its excellent
advantages such as low cost, low temperature, non-toxic
operation and environmental friendliness. Although there are
already a number of researches on the preparation of ZnO
nanostructures via aqueous techniques which include micro
emulsion hydrothermal synthesis [5], direct deposition in
aqueous solution [6], surfactant assisted hydrothermal
orientation growth [7], alcohol solution refluxing [8] and
simple chemical sol–gel process [9].
Low temperature hydrothermal synthesis
The low temperature hydrothermal synthesis is one of the
excellent processes for nanocrystalline state synthesis [10]. It
has been widely used for the growth of ZnO nanostructures
mainly because have unique advantages over other methods
in many ways. The growth is carried out under relatively
lower temperatures ranges from 70°C to 90°C. The cost of
production is minimal due to the use of simpler equipment
and cheaper chemicals. It uses more environmental and less

* Corresponding author
E-mail address: dr.mustafa.abbas@gmail.com (M. A. Mustafa)
 Journal of Nanoscience and Nanoengineering Vol. 1, No. 4, 2015, pp. 248-251 249

hazardous materials. In the hydrothermal synthesis, different

parameters such as the type of the precursor, the additives,
the solvents and the pH of the growth medium all play an
important role in the growth of ZnO nanostructures [11]. It is
considered that molecular structure-directing agents play a
significant role in the kinetic control of the nanocrystal
growth by preferentially adsorbing onto specific crystal
faces, thus impeding growth of that surface. Organic and
inorganic additives have been widely added to the wet
chemical nanosynthesis for designed morphology [12]. Zinc
salt precursor has been reported to play effective role on the
surface morphology and properties of zinc oxide [12]. In this
paper ZnO nanopowder was prepared via a hydrothermal
technique with prime focus on the growth in alkaline
solutions (NaOH) and its effect on the size and morphology
of the particles.
[Zn(OH)4]2– ↔ ZnO 2
-2
+2H2O (3)
ZnO2-2 +2H2 O ↔ZnO + 2OH −
(4)
The formation mechanism of the ZnO nanostructures is a
complex process and mostly considered to include two main
steps: the generation of a ZnO nuclei, and subsequent ZnO
crystal growth, the Zn(OH)42- complexes serve as basic
growth units for the preparation of ZnO nanostructures [13-
14].The zinc acetate may convert into Zn(OH)2 colloids
firstly under alkali solution, as shown in reaction 1. During
the process, part of the Zn(OH)2 colloids dissolves into Zn2+
and OH− according to reaction no 2. When the concentration
of Zn2+ and OH− reaches the supersaturation degree of ZnO,
ZnO nuclei will form according to reaction no 4.

2.4. Characterization of ZnO Nanopowder

2. Materials and Methods X-ray diffraction analysis of the ZnO samples was carried
2.1. Reactants out by use of a Phillips (X’Pert Pro software) powder
diffractometer operating with Cu-Ka radiation working at 40
Zinc acetate dihydrate Zn(CH3COO)2.2H2O (as a zinc mA and 45 kV. and SEM (MIRA3 TESCAN), at an
source) and sodium hydroxide (NaOH) were used as accelerating voltage of 15 kV.
precursors for the formation of the zinc oxide nanopowder.
Deionized water was used for dilution.
3. Results and Discussions
2.2. Synthesis of Zinc Oxide Nanopowder
3.1. XRD Analysis of Zinc Oxide
Zinc acetate dihydrate Zn(CH3COO)2.2H2O and sodium Nanopowder
hydroxide NaOH were each dissolved separately in deionized
X-ray Powder Diffraction (XRD) studies were carried using
water to form the liquid media of the desired concentrations
X-ray diffractometer with cu kα radiation (λ = 1.5418 Å) in
of 0.05M and 0.1M for sample A and B respectively the ratio
the range of 10–80° to determine their crystal structure and
of the concentrations was 1:1 (Zn(CH3COO)2.2H2O: NaOH).
phase. Figures 1 illustrates a typical XRD spectrum of ZnO
The Zinc acetate dihydrate was slowly added drop- wise to
nanopowder prepared by aqueous chemical growth (ACG)
NaOH solutions under vigorous stirring at room temperature,
method. X-ray diffraction patterns indicate that the obtained
forming transparent white solutions, then inserted into an
ultra-fine particles are in good crystallinity. The XRD spectra
electrical oven at 90°C for 2 hours. These solutions were
indicate that the ZnO crystal has a hexagonal structure, with
reacted to produce zinc oxide precipitates.
space group P63mc (ICSD collection code: 065119).
Following the precipitation, the solution was centrifuged at
3000 rpm for 30 minutes. The supernatant was then removed,
and the precipitation which contains nano ZnO was obtained.
Finally, nano ZnO was grinded with mortar to be shaped into
powder. This experiment was repeated eight times under the
same conditions for each concentration. Then the total
powder obtained was mixed to provide sample A (0.05M)
and sample B (0.1M).

2.3. The Growth Mechanism of the Zinc

Oxide Nanopowder
The growth process of ZnO nanopowder can be controlled
through the following listed chemical reactions:

Zn.(CH3COO)2.2H2O + 2NaOH → Zn(OH)2+2CH3COONa +2H2O (1)

Figure 1. XRD pattern of ZnO powder for sample (A) prepared using a
2+ -
Zn(OH)2 (gel) + 2H2O = Zn + 2OH + 2H2O = [Zn(OH)4] (2) 2 concentration of 0.05M sodium hydroxide.
250 Dalia Ahmed Mohammed Osman and Mustafa Abbas Mustafa: Synthesis and Characterization of Zinc
Oxide Nanoparticles using Zinc Acetate Dihydrate and Sodium Hydroxide

a. Magnification 9.32kx

Figure 2. XRD pattern of ZnO powder for sample (B) prepared using a
concentration of 0.1M sodium hydroxide.

Diffraction peaks related to impurities were observed in the

XRD pattern in the first sample. It could be seen that the
diffraction peaks shown in Figure 2 (sample B) were more
intense and narrower than that of Figure 1 (sample A),
implying the good crystalline nature of the synthesized ZnO b. Magnification 38.2 kx
nano powder and that the products have a high-purity ZnO
wurtzite phase. The average crystallite sizes (D) of samples
A and B were estimated to be about 75 and 54 nm
respectively according to the Debye- Scherrer formula [15].
. λ
D (5)

Where
λ is wave length of X-Ray (0.1541 nm),
βi is FWHM (full width at half maximum)in radians c. Magnification 76 kx

θ is the diffraction angle (18.267° and 18.240° for sample A Figure 3. SEM image of zinc oxide nanopowder for sample A.
and B respectively)
D is particle diameter size.
The detailed analysis of the XRD and the assignments of
various reflections are given in Table (1).
Table 1. Analysis of XRD and the assignments of various reflections of
ZnO.

Sample d-spacing FWHM Estimated crystallite size (nm)

A 2.44834 0.11808 75
B 2.46312 0.1771 54

These results indicate that the higher the concentration of a. Magnification 11.3 kx

precursor, the smaller the average crystallite size of ZnO

nanopowder

3.2. SEM Analysis of Zinc Oxide

Nanopowder
SEM studies were conducted in order to examine the
morphology of the prepared nanopowder. The SEM images
of the obtained ZnO-nanopowder are shown in Figure 3 and
4.

b. Magnification 38.2 kx
 Journal of Nanoscience and Nanoengineering Vol. 1, No. 4, 2015, pp. 248-251
c. Magnification 77.6 kx
Figure 4. SEM image of zinc oxide nanopowder for sample B.
The SEM images present the particles of sample A with a
very wide particle size distribution and different
morphologies of platelets and flaky particles while that of
sample B were nanotubes, spherical and nanorods were the
predominate particles.
4. Conclusions
The ZnO nanopowder was successfully prepared via low
temperature chemical growth through hydrothermal
technique using zinc acetate dihydrate as a zinc source and
sodium hydroxide. A high production yield was obtained by
using sodium hydroxide instead of hexamethylenetetramine
(HMTA). The method used is a simple and cheap method
which does not require a solvent or calcination after drying.
Deferent morphologies could be obtained from the growth in
alkaline solutions using NaOH. Furthermore, the method can
be scaled-uphowever requires considerable amounts of water.
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