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Hydrothermal Zinc Oxide Nanowire Growth Using Zinc Acetate Dihydrate Salt

Article  in  Journal of Materials Research · June 2012

DOI: 10.1557/jmr.2012.92

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 Hydrothermal zinc oxide nanowire growth using zinc acetate
dihydrate salt
Mehmet Can Akgun
Department of Micro and Nanotechnology, Middle East Technical University, Ankara, Turkey
Yunus Eren Kalay
Department of Metallurgical and Materials Engineering, Middle East Technical University, Ankara, Turkey
Husnu Emrah Unalana)
Department of Micro and Nanotechnology, Middle East Technical University, Ankara, Turkey; and
Department of Metallurgical and Materials Engineering, Middle East Technical University, Ankara, Turkey

(Received 24 November 2011; accepted 13 March 2012)

Hydrothermal approach is widely used for the synthesis of zinc oxide (ZnO) nanowires. Zinc nitrate
hexahydrate, zinc acetate and zinc chloride are three common salts that are used for synthesis.
Among these, zinc nitrate hexahydrate is primarily used in many studies and zinc chloride is
preferred for electrodeposition. In this work, zinc acetate dihydrate salt is used for the growth of ZnO
nanowires and the effects of time, temperature, solution concentration and concentration ratios of the
precursor chemicals are investigated. It is found that the growth time and solution concentration
control the lengths of the nanowires, whereas the precursor concentration ratio and solution
concentration control their diameter. High solution concentrations and high zinc acetate dihydrate
concentrations lead to the development of thin film morphology. Optimum growth parameters are
obtained and suggested for the use of zinc acetate dihydrate as a zinc source for growing ZnO
nanowires with high aspect ratio (AR). The use of zinc acetate dihydrate leads to the formation of
ZnO nanowires without impurities and eliminates the need for using extra capping agents.

I. INTRODUCTION methods. Hydrothermal synthesis is a robust and economic

Electronic devices utilizing nanowires and nanorods are
subject of great interest since they promise to have novel
properties and be a substitute for devices made of
conventional semiconducting thin film or bulk materials.
ZnO, with its wide direct band gap (3.37 eV) and large
exciton binding energy (60 meV), is a promising material
for various applications. Nanostructures offer grain-
boundary and mostly defect-free single crystalline nature
over their bulk counterparts, which could be beneficial for
electronic and optoelectronic applications. Therefore, ZnO
nanorods and nanowires have been a subject of intense
study in recent years for their implementation in ultraviolet
(UV) lasers,1 field emission devices,2,3 sensors,4,5 transis-
tors,6 solar cells,7–9 piezo-nanogenerators,10,11 light emitting
diodes.12 Several methods have been utilized for the
synthesis of ZnO nanowires. Vapor phase transport,13,14
metal-organic chemical vapor deposition (MOCVD),15,16
and low temperature approaches17–34 are among a few
of these methods. Low temperature growth methods for
ZnO nanostructures include but not limited to sol-gel
method,35,36 chemical bath deposition37 and hydrothermal
a)
Address all correspondence to this author.
e-mail: unalan@metu.edu.tr
DOI: 10.1557/jmr.2012.92
method for the growth ZnO nanowires that can be carried
out with simple equipment unlike the other methods
mentioned. Hydrothermal method was first introduced by
Vaysseries et al.30 for the growth of ZnO nanowires on
substrates. This has been followed by seeding and anneal-
ing the substrates17 to obtain aligned nanowires. Sub-
sequently, it has been shown that ZnO nanowires can be
patterned,29 can be doped with transition metals31 and their
growth direction can be controlled.32 Formation of ZnO
nanotubes by a two-step hydrothermal process has also been
demonstrated, in which previously grown nanowires were
preferentially etched within the same solution, but at a lower
temperature to form nanotubes.34 One of the problems
associated with the hydrothermal synthesis of the ZnO
nanowires was the time required, which spanned from
several hours to days. It has been resolved through heating
the growth solution through a tip sonicator33 or a micro-
wave23 oven under ambient conditions. This allowed syn-
thesis of high AR ZnO nanowires in matter of minutes.
Researchers use capping agents20 or strong bases21,27 to
synthesize ZnO nanowires with high AR; however, these
substances may introduce unwanted impurities into ZnO
nanowires, which could limit their use in certain applica-
tions. In almost all of the previously mentioned studies,
zinc nitrate hexahydrate has been used as the zinc source
and the effects of different growth parameters on the final

J. Mater. Res., Vol. 27, No. 11, Jun 14, 2012 Ó Materials Research Society 2012 1445
 M.C. Akgun et al.: Hydrothermal zinc oxide nanowire growth using zinc acetate dihydrate salt
product have been reported using this salt.19 Zinc chloride,
on the other hand, is mainly preferred for electrochemical
ZnO nanowire growth.38 A third alternative, zinc acetate
dihydrate, which is commonly used for seeding the ZnO
nanowire growth, is rarely used as a zinc source involving
the hydrothermal method. Because of this, no parametric
study taking into account the growth parameters using zinc
acetate dihydrate salt has been ascertainable in the literature.
In this work, we report on the effect of parameters for
growing ZnO nanowires via hydrothermal method using
zinc acetate dihydrate as a zinc source. The effects of growth
time, temperature, solution concentration and concentration
ratio are investigated. Our results present a roadmap for the
synthesis of ZnO nanowires with desired diameter and
length using zinc acetate dihydrate as the zinc source,
without any extra additives.
II. EXPERIMENTAL DETAILS
In this work, silicon (001) substrates were used to grow
ZnO nanowires. All chemicals were purchased from Sigma-
Aldrich and Merck Chemicals and used without further
purification. Before growth process, pieces of silicon sub-
strates were first ultrasonically cleaned, in consecutive
acetone (99.8%), isopropanol (99.8%) and deionized (DI)
water baths (18.3 MX) for 10 min. Substrates were then
dried with nitrogen gas. A 5 mM solution of zinc acetate
dihydrate in 1-propanol was prepared and used for the
deposition of seed layer through spin coating. Right after
spin coating, substrates were annealed at 350 °C for 20 min
to obtain aligned ZnO nanowires. Seeded substrates were
then dipped into aqueous solutions of zinc acetate dihydrate
[Zn(O2CCH3)2(H2O)2, 99.0%] and hexamethylenetetra-
mine [HMTA, (CH2)6N4, 99.0 %] at the set temperature
and kept for the desired duration of time for growth.
Solution concentrations (0.01–0.1 M) with zinc acetate
dihydrate/HMTA concentration ratios of 3:1, 2:1, 1:1, 1:2
and 1:3 were investigated. Growth times up to 3 h at growth
temperatures in the range of (50–100 °C) were elaborated.
At the end of the growth process, substrates were taken out
of the solution, rinsed with DI water to remove any residual
salts and organic material and finally dried with nitrogen gas.
The crystal structure of the nanowires was investigated
by x-ray diffraction (XRD) using a vertical goniometer axis
Rigaku Cu Ka x-ray diffractometer (Rigaku Corporation,
Tokyo, Japan) with the Bragg-Brentano focusing geometry.
Optical absorption measurements via ultraviolet visible
spectroscopy (UV-VIS) were taken using VARIAN CARY
100 BIO UV-Visible Spectrometer (Agilent Technologies
Pty Ltd., Mulgrave, Victoria, Australia) in normal incidence
mode from ZnO nanowires grown on quartz substrates.
Conventional and high-resolution transmission electron
microscopy (HRTEM) analyses were conducted using
a JEOL JEM 2100F scanning/transmission electron micro-
scope (S/TEM; JEOL Ltd., Tokyo, Japan) operated at
1446 J. Mater. Res., Vol. 27, No. 11, Jun 14, 2012
200 kV. Specimens for TEM analyses were prepared by
drop-casting of methanolic solution of nanowires onto lacey
carbon coated copper grids. Photoluminescence measure-
ments were performed using HORIBA Jobin Yvon PL
system (HORIBA Ltd., Irvine, CA) at an excitation wave
length of 325 nm. The morphology and size of the ZnO
nanowires were investigated by a FEI Nova Nano SEM 430
Field Emission Scanning Electron Microscope (FESEM;
FEI, Eindhoven, Netherlands) at 10 kV. ZnO nanowires
grown on silicon substrates were analyzed without any
coating. Cross-sectional SEM analyses were conducted from
the cleaved surfaces of the specimens. Length and diameter
of the more than 100 individual nanowires were measured
using ImageJ software from the obtained SEM images and
then the average length and diameter of the nanowires were
calculated and reported with their error bars.
III. RESULTS AND DISCUSSION
XRD spectrum from ZnO nanowires grown at 85 °C, for
3 h at an equimolar zinc acetate dihydrate and HTMA
concentration of 0.02 M is shown in Fig. 1(a). The strong
peak at 34.8° (2h) corresponding to (002) spacing of the
wurtzite structure [Joint Committee on Powder Diffraction
Standards (JCPDS) Card No: 36–1451] revealed a preferen-
tial alignment of the nanowires on the substrate in their
c-axis direction. Figure 1(b) shows the transmittance of the
ZnO nanowires grown under the same conditions. Within
the 3.17–6.2 eV photon energy range, almost constant and
high transparency in the visible portion and a sharp absorp-
tion onset at 374 nm is observed. The band gap of the ZnO
nanowires is estimated to be 3.27 eV from the Tauc plot
considering the direct band gap, as shown at the inset of the
graph in Fig. 1(b). Photoluminescence measurement shown
in Fig. 1(c) revealed strong band edge emission at 3.3 eV
without any detectable defect related emission. TEM anal-
ysis revealed further structural information. Figure 1(d) and
1(e) show bright-field (BF) images and the corresponding
selected area electron diffraction (SAED) pattern [Fig. 1(e)
inset] of ZnO nanowires grown using the same growth
conditions at relatively low magnifications. SAED pattern
from a single nanowire reveals the single crystalline nature
of the ZnO with (0002) crystal planes extending along the
growth direction. Further HRTEM analyses, Fig. 1(f), from
the same single crystals, clearly indicates the growth of ZnO
nanowire in [0001] direction. The lattice spacing along
[0001] was measured as 0.52 nm and matches up with the
lattice parameter of wurtzite structure across the c-axis.
A. Effect of the time on the growth process
Figures 2(a)–2(d) shows the cross-sectional SEM
images of ZnO nanowires that are grown at 85 °C for
40, 80, 160 and 180 min, respectively. Plot in Fig. 2(e), on
the other hand shows the change in diameter and length
 M.C. Akgun et al.: Hydrothermal zinc oxide nanowire growth using zinc acetate dihydrate salt
FIG. 1. (a) X-Ray diffraction pattern for ZnO nanowires grown on
silicon substrates in an equimolar 0.02 M solution of zinc acetate
dihydrate and HMTA for 180 min (b) UV-VIS transmission pattern of
ZnO nanowires grown on quartz substrates under the same conditions.
Inset shows the Tauc plot showing the change in (ahv)2 with respect to
energy. (c) Photoluminescence spectra from ZnO nanowires grown on
silicon substrates. (d) BF TEM image showing a group of ZnO
nanowires at relatively low magnification. (e) BF TEM image and
corresponding SAED pattern (inset) taken from single crystal ZnO.
(f) HRTEM image of a single ZnO nanowire showing the lattice fringes
along the [0001] growth direction.
of the nanowires with time. The graph at the inset of the
plot in Fig. 2(e) reveals the change in AR of the nanowires
with time. An equimolar solution of 0.02 M zinc acetate
dihydrate and HMTA was used to determine the effect
of growth time. As shown in Fig. 2(e), lengths of the
nanowires increase steadily during the reaction period,
whereas their diameters remain almost constant. At the end
of 180 min, perpendicularly aligned nanowires with
high AR (up to 35) were obtained. It was reported by Xu
et al.20 that adding acetate ions to a solution of zinc nitrate
hexahydrate and HMTA lead to highly responsive capping
effect for growing nanowires with high AR compared with
other capping agents, such as sodium dodecyl sulfate and
ethylenediamine. Therefore, we attribute constancy of nano-
wire diameter during growth process to the capping effect of
the acetate ions. Furthermore, Zhang et al.21 have reported
that low Zn12/OH
concentration ratio is necessary for the
growth of ZnO nanowires with high AR. We believe this
condition also plays an important role in this study.
J. Mater. Res., Vol. 27, No. 11, Jun 14, 2012
FIG. 2. Cross-sectional SEM images of ZnO nanowires that are grown for
(a) 40, (b) 80, (c) 160 and (d) 180 min. All scales are the same. (e) Variation
of nanowire diameter and length with reaction time. Inset shows the
variation of AR of the samples. Lines are for visual aid.
B. Effect of temperature on the growth process
Temperature of the growth solution is another factor that
has a direct influence on nanowire length and diameter.
Figures 3(a)–3(f) show the cross-sectional SEM images of
ZnO nanowires that are grown at 50, 60, 70, 80, 90 and
100 °C, respectively. These nanowires were grown for 3 h.
Plot in Fig. 3(g) shows the change in the diameters and
lengths of ZnO nanowires as a function of temperature.
Lengths of the nanowires increase steadily with temper-
ature, whereas their diameters are found to be almost con-
stant around 80 nm. Nanowire growth was not observed for
the sample kept at 50 °C. Short and stubby ZnO nanowires
were observed when growth process was conducted at 60 °C.
This indicates that a temperature in between 50 and 60 °C
initiates the growth of ZnO nanowires in this method. It is
evident that higher temperatures increase the kinetics of the
reaction favoring the quick precipitation of ZnO; therefore,
resulting in longer and high AR (up to 55 for the growth
1447
 M.C. Akgun et al.: Hydrothermal zinc oxide nanowire growth using zinc acetate dihydrate salt

at 100 °C for 180 min) nanowires. This means that as
the temperature of the reaction increases, the capping effect
of acetate ions is getting more prominent. In addition, the
resulting decrease in the concentration of Zn12 and the
Zn12/OH
ratio in the solution due to increase in reaction
kinetics may also contribute to keep the diameters of the
nanowires constant.
C. Effect of the concentration ratios on the growth
process
Figures 4(a)–4(e) show the cross-sectional SEM images
of ZnO nanowires that are grown at HMTA and zinc ace-
tate dihydrate solution concentration ratios of 3:1, 2:1, 1:1,
1:2 and 1:3, respectively. Nanowires were grown at 85 °C
for 3 h. The effect of different concentration ratios on the

FIG. 3. Cross-sectional SEM images of ZnO nanowires that are grown
at (a) 50 °C, (b) 60 °C, (c) 70 °C, (d) 80 °C, (e) 90 °C and (f) 100 °C.
All scales are the same. Insets in (d) and (e) show the top view SEM
images of the nanowires. (f) Variation in the diameter and length of ZnO
nanowires with temperature. Inset shows the variation of AR of the same
samples. Lines are for visual aid.
FIG. 4. Cross-sectional SEM images of ZnO nanowires that are grown
with solution concentration ratios of ([HMTA]/[zinc acetate dihydrate:
(ZAD)]) (a) 3:1, (b) 2:1, (c) 1:1, (d) 1:2 and (e) 1:3. All scales are the
same. (f) Graph showing the effect of different solution concentration
ratios of HMTA and zinc acetate dihydrate on the diameter and length of
ZnO nanowires. Lines are for visual aid.

1448 J. Mater. Res., Vol. 27, No. 11, Jun 14, 2012
 M.C. Akgun et al.: Hydrothermal zinc oxide nanowire growth using zinc acetate dihydrate salt

diameters and lengths of ZnO nanowires as a function of

concentration ratios of HMTA and zinc acetate dihydrate
is plotted at in Fig. 4(f). The reactions that are taking place
during the ZnO nanowire growth are20:

ðCH2 Þ6 N4 þ 6H2 O ! 6HCHO þ 4NH3

NH3 þ H2 O ! NHþ
4 þ OH

2OH
þ Zn2þ ! ZnðOHÞ2 ðsÞ ! ZnOðsÞ þ H2 O

From these reactions, it appears that the formation of

1 mol of ZnO product requires one-half mol of (CH2)6N4
and 1 mol of Zn(O2CCH3)2(H2O)2 which is equivalent to
[(CH2)6N4]/[(Zn(O2CCH3)2(H2O)2] ratio of 1/2. So, one
may expect to obtain longest ZnO nanowires using this
ratio. However in our study, longest ZnO nanowires were
obtained at a HMTA/zinc acetate dihydrate ratio of 1.
Excess amount of (CH2)6N4 provides sufficient amount of
OH
ions for the growth of ZnO nanowires in the solution,
where actual concentration of NH3 is less than the nominal
concentration. In this respect, our results are similar to the
ones obtained during ZnO nanowire growth using zinc
nitrate hexahydrate.19 On the contrary to nitrate growth, we
have not observed a change in the alignment and nucleation
density of the nanowires with HMTA/zinc acetate dihydrate
ratio at least for the nanowire morphology.19 When the ratio
of the concentration of zinc acetate dihydrate is higher, the
structure of ZnO deviates from nanowires to a thin film-like
form. This condition is related to an increase in Zn12/OH

concentration ratio, which in turn decreases the length and
AR of ZnO nanowires yet increases their diameter. On the
other hand, higher HMTA ratios in comparison with zinc
acetate dihydrate led to an increase in the AR of ZnO
nanowires. This is due to the higher availability of OH

ions that leads to the precipitation of more ZnO compared
with other concentration ratios. FIG. 5. Cross-sectional SEM images of ZnO nanowires grown in
solutions for 180 min containing equimolar (a) 0.01 M, (b) 0.02 M,
(c) 0.03 M, (d) 0.04 M, (e) 0.05 and (f) 0.1 M zinc acetate dihydrate
D. Effect of solution concentration on (ZAD) and HMTA. All scales are the same. Inset shows top view SEM
the growth process images of the samples grown at indicated concentrations. (g) Graph
Figures 5(a)–5(f) shows the cross-sectional SEM images showing the effect of different equimolar solution concentrations of
HMTA and zinc acetate hexahydrate on the diameter and length of ZnO
of ZnO nanowires grown in an equimolar ratio of zinc ace- nanowires. Lines are for visual aid.
tate dihydrate and HMTA solution which has zinc acetate
dihydrate and HMTA concentrations of 0.01 M, 0.02 M,
0.03 M, 0.04 M, 0.05 M and 0.1 M, respectively. The effect during precipitation. Thin and long nanowires were ob-
of different concentrations on the diameters and lengths of served for a solution concentration of 0.02 M. With the
ZnO nanowires as a function of equimolar concentrations of increase in solution concentration to 0.05 M, an evident
HMTA and zinc acetate dihydrate is plotted in Fig. 5(g). increase in the nanowire diameter was observed. This is a
Nanowires were grown at 85 °C. Only a few nanowires are result of existence of more Zn12 ions compared with OH

observed on the silicon substrates for the samples grown at ions in the growth solution which influences the growth of
a solution concentration of 0.01 M. It is clear that the growth the nanowires from the side planes. A film-like morphology
of these nanowires was not originated from the seeds on was observed for the nanowires grown at a solution concen-
the silicon substrates and they get attached to the substrate tration of 0.1 M. Nanowire features and more prominently

J. Mater. Res., Vol. 27, No. 11, Jun 14, 2012 1449
 M.C. Akgun et al.: Hydrothermal zinc oxide nanowire growth using zinc acetate dihydrate salt
hexagonal facets of ZnO can still be seen within the thin
film morphology, which clearly indicates that the capping
effect of acetate ions have been impeded. Optimum con-
centration was then determined to be 0.02 M leading to the
growth of high AR ZnO nanowires.
Although using highly basic growth solutions with
sodium hydroxide (NaOH) and zinc nitrate hexahydrate
yields high AR nanowires (AR of 15 within 60 min),27
this may introduce impurities to nanowires. Capping agents
like acetate ions or sodium oxalate can be used for the growth
of high AR ZnO nanowires, but similarly, they could intro-
duce impurities. In addition, longer reaction times were found
to be necessary for the growth of the ZnO nanowires with
capping agents. For instance, an AR of 20 was obtained in
36 h when acetate ions were added to the growth solution,20
whereas an AR of 120 in 24 h were obtained through the
addition of sodium oxalate (Na2C2O4).22 On the contrary, the
use of zinc acetate dihydrate, as described in this paper, leads
to the formation of ZnO nanowires in short reaction times
without impurities and eliminating the need for using extra
capping agents. This is evident with the obtained AR of 55
for the growth conducted at 100 °C for 180 min. Full
control over the lengths and diameters of the nanowires
with the synthesis parameters provided herein would facil-
itate the realization of ZnO nanowire-based electronic and
optoelectronic devices in short reaction times without
impurities.
IV. CONCLUSIONS
To conclude, ZnO nanowires have been grown using zinc
acetate dihydrate as the zinc salt and the effect of growth
parameters such as time, temperature, solution concentration
and concentration ratios of the precursor chemicals have
been determined. The use of zinc acetate dihydrate, which
has acetate ions, enhances the capping effect and leads to the
growth of high AR ZnO nanowires. The lengths of the
nanowires were found to be controlled through the growth
time and solution concentration. On the other hand, the
diameters of the nanowires were found to be controlled by
the precursor concentration ratio and solution concentration.
Thin film morphology was obtained through the growth
conducted with a high zinc acetate dihydrate concentra-
tion as compared with HMTA and at high solution concen-
trations. The results reported in this article establishes the
basis for the growth ZnO nanowires via hydrothermal
growth using zinc acetate dihydrate as the zinc source.
ACKNOWLEDGMENTS
This work was supported by the Scientific and
Technological Research Council of Turkey (TUBITAK)
under Grant No. 109M084 and 109M487 and the Distin-
guished Young Scientist Award of the Turkish Academy
of Sciences (TUBA).
1450 J. Mater. Res., Vol. 27, No. 11, Jun 14, 2012
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