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Colloids and Surfaces A: Physicochem. Eng. Aspects 319 (2008) 130–135

A simple preparation technique for shape-controlled zinc oxide

nanoparticles: Formation of narrow size-distributed
nanorods using seeds in aqueous solutions
Tetsuo Kawano, Hiroaki Imai ∗
Department of Applied Chemistry, Faculty of Science and Technology, Keio University 3-14-1 Hiyoshi, Kohoku-ku, Yokohama 223-8522, Japan
Received 14 September 2006; received in revised form 8 May 2007; accepted 14 May 2007
Available online 18 May 2007

Abstract
Various shapes of wurtzite-type ZnO nanoparticles were selectively produced in a simple aqueous system prepared by mixing ZnSO4 and NaOH
solutions. Ellipsoidal nanoparticles were obtained by the addition of an alkaline agent into an acidic zinc solution (acidic route), while nanorods
were grown by mixing a zinc precursor into an alkaline solution (basic route). The aspect ratio and size distribution of the nanorods grown through
the basic routes were controlled by the addition of nanoparticles prepared by the acidic route as seeds. On the other hand, micrometric branching
rods were obtained by dilution of the reaction solution in the basic routes. The morphological variation of ZnO particles is ascribed to the balance
of the nucleation and crystal growth depending on the degree of the supersaturation. We successfully prepared narrow size-distributed rods with
a nanometric width and a submicrometric length using the seed particles, because the presence of the seeds suppressed additional nucleation and
then controlled the degree of the supersaturation for steady growth of the crystalline particles.
© 2007 Elsevier B.V. All rights reserved.

Keywords: Zinc oxide; Nanoparticle; Nanorod; Crystal growth; Seed

1. Introduction including surfactants [21,22], amine [23], solvents [24,25] and

Wurtzite-type zinc oxide (ZnO), a wide band-gap (3.37 eV)
semiconductor with a large exciton-binding energy, is an attrac-
tive material because of its unique properties, such as optical
transparency, electric conductivity, piezoelectricity and near-UV
emission [1–4]. The size and morphology are important param-
eters to determine the physical and physicochemical properties
of ZnO crystals. Various kinds of nanoscale morphologies, such
as spherical particles [5], rods [6–9], whiskers [10], columns
[11–13], wires [14], tubes [15], rings [16], disks [17] and
other characteristic shapes [18–20], were fabricated. Wet chem-
ical methods using aqueous solution-based systems have been
widely applied for the preparation of the ZnO crystals with var-
ious morphologies. The size and shape of ZnO crystals grown
in the solutions were controlled by the reaction conditions [21],
selection of precursors [22] and addition of organic molecules
∗ Corresponding author. Tel.: +81 45 566 1556; fax: +81 45 566 1551.
E-mail address: hiroaki@applc.keio.ac.jp (H. Imai).
polymers [26,27].
One-dimensional (1D) ZnO materials were prepared using
various methods [6–10,14,15,28–33]. In particular, nanorods
have been produced in basic solution systems at low temper-
atures [6–9,33] and under hydrothermal conditions [7]. The
submicrometric control of the length of the nanorods in a
range smaller than the wavelength of visible light is essen-
tial for applications to optically transparent materials, such as
ZnO–polymer composite films for a component of recording
media [4]. Although the aspect ratio varied in the range of
50–100 with a width of 10–30 nm by changing [OH− ]/[Zn2+ ]
[6], preparation techniques for nanorods with submicrometric
lengths have not been established.
We selectively produced nanoparticles and nanorods of ZnO
crystals using a simple mixing technique of ZnSO4 and NaOH
solutions without any organic additives [9]. However, the size
distribution of the nanorods broadened because the nucleation
was not controlled in the mixtures. In the present study, we per-
formed further control of nanometric shapes and size distribution
of ZnO particles by addition of seeds into the simple system. The

0927-7757/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.colsurfa.2007.05.019
 T. Kawano, H. Imai / Colloids and Surfaces A: Physicochem. Eng. Aspects 319 (2008) 130–135 131

mechanism of morphological variation is discussed on the basis
of the balance of the nucleation and crystal growth at a certain
degree of supersaturation. This work would provide not only a
simple method for selected fabrication of 1D ZnO particles with
a nanometric width and a submicrometric length, but also funda-
mental information for shape control of nanoparticles prepared
through the crystal growth in aqueous solutions.
2. Experimental
A stock solution (pH 5.3) of 0.2 M zinc sulfate (ZnSO4 )
and an alkali solution (pH 13.8) of 4.0 M sodium hydroxide
(NaOH) were prepared by dissolution of zinc sulfate hep-
tahydrate (ZnSO4 ·7H2 O, 99.5%; Kanto Chemical) and NaOH
(Junsei Chemical) into purified water, respectively. The reac-
tions were fundamentally performed with stirring by mixing the
stock solution of ZnSO4 , the alkali solution of NaOH and a cer-
tain amount of purified water. The final pH of the mixture was
fixed to ca. 13 because a highly basic condition is suitable for the
direct preparation of wurtzite-type ZnO crystals [12]. Precipita-
tion occurred at 60 ◦ C for 2 h after the mixing of the solutions.
The products obtained by centrifugation were washed with puri-
fied water and then dried at 60 ◦ C in air. However, the shape and
size of resultant particles depended on the mixing procedure of
the solutions.
As an acidic route, 25.0 cm3 of the alkali solution (4.0 M
NaOH) was dropped at an approximate rate of 5 cm3 /min into
an acidic mother solution (pH 5.6) prepared from 25.0 cm3 of
the stock solution (0.2 M ZnSO4 ) and 50.0 cm3 of purified water.
As a basic route, 25.0 cm3 of the stock solution (0.2 M ZnSO4 )
was dropped at an approximate rate of 5 cm3 /min into a basic
mother solution (pH 13.6) obtained by mixing the alkali solution
(4.0 M NaOH) and purified water. Typically, 25.0 cm3 of the
stock solution was added into a mixture of 25.0 cm3 of the alkali
solution and 50.0 cm3 of purified water (basic route 1). The final
concentrations of ZnSO4 and NaOH for the acidic route and
basic route 1 were 0.050 and 1.0 M, respectively.
Seed-mediated crystal growth was performed using the basic
route to modify the morphology of resultant ZnO crystals. Ini-
tially, seed particles of ZnO crystals were prepared via the
above-mentioned acidic route and washed with abundant puri-
fied water. Then, 12.5 cm3 of the stock solution (0.2 M ZnSO4 )
was dropped at an approximate rate of 5 cm3 /min into a seeded
mother solution produced from 12.5 cm3 of the alkali solution
(4.0 M NaOH), 25.0 cm3 of purified water and 50.0 cm3 of a
seed suspension (basic route 2). The amount of seeds varied
from 0 to 0.077 g in 100 cm3 of the final solution by changing
the concentration of the seed suspension. The degree of super-
saturation was lowered during the formation of ZnO crystals by
subsequent dilution (basic route 3). A mother solution for basic
route 1 was initially prepared by mixing 12.5 cm3 of the stock
solution, 12.5 cm3 of the alkali solution and 25.0 cm3 of puri-
fied water. After being stirred for 5 min, the reaction solution
was diluted by addition of an excessive amount of water with a
volume of 50.0 cm3 . The concentrations of ZnSO4 and NaOH
in the resultant solution for basic routes 2 and 3 were 0.025
and 0.5 M, respectively. The preparation conditions are listed in
Table 1.
The precipitated particles were characterized by θ/2θ X-ray
diffractometry (XRD; Rigaku RAD-C and Bruker D8 Advance)
using Cu K␣ radiation. The morphologies of the particles were
observed with a field-emission scanning electron microscope
(FESEM, Hitachi S-4700) at 5 kV accelerating voltage and
a field-emission transmission electron microscope (FETEM,
Philips TECNAI F20). The size of the ZnO particles was esti-
mated from the FESEM images.
3. Results
According to the XRD patterns (Fig. 1), the precipitates
were assigned to wurtzite-type ZnO regardless of the prepa-
ration routes. However, the shape of the products was obviously
influenced by the preparation route as shown in Figs. 2 and 3,
and listed in Table 2. Ellipsoidal nanoparticles with an aver-
age width of 32 nm and a length of 44 nm were grown at pH
12.8 through the acidic route (Fig. 2(a) and (b)). On the other
hand, ZnO nanorods with a high aspect ratio were obtained
at pH 12.8 through basic route 1 (Fig. 2(c) and (d)). The lat-
tice image indicates that the ZnO rods were single-crystalline
and were elongated along c axis (Fig. 4). Fig. 5 shows cumu-
lative undersize distribution of ZnO particles estimated from
FESEM images. The median width and length of the rods pre-

Table 1
Conditions for the preparation of wurtzite-type ZnO particles
Route Mother solution Additional solution Final concentrations

ZnSO4 (M) NaOH (M) Seed (g/100 cm3 )

Acidic 0.2 M ZnSO4 25.0 cm3 ; H2 O 50.0 cm3 4.0 M NaOH 25.0 cm3 0.050 1.0 0
Basic 1 4.0 M NaOH 25.0 cm3 ; H2 O 50.0 cm3 0.2 M ZnSO4 25.0 cm3 0.050 1.0 0
Basic 2–1 4.0 M NaOH 12.5 cm3 ; H2 O 75.0 cm3 0.2 M ZnSO4 12.5 cm3 0.025 0.5 0
Basic 2–2 4.0 M NaOH 12.5 cm3 ; H2 O with seeds 75.0 cm3 0.2 M ZnSO4 12.5 cm3 0.025 0.5 0.019
Basic 2–3 4.0 M NaOH 12.5 cm3 ; H2 O with seeds 75.0 cm3 0.2 M ZnSO4 12.5 cm3 0.025 0.5 0.077
Basic 3 4.0 M NaOH 12.5 cm3 ; H2 O 25.0 cm3 First 0.2 M ZnSO4 12.5 cm3 ; 0.025 0.5 0
second H2 O 50.0 cm3

Stock solution: 0.2 M ZnSO4 , Alkali solution: 4.0 M NaOH.

132 T. Kawano, H. Imai / Colloids and Surfaces A: Physicochem. Eng. Aspects 319 (2008) 130–135

In order to control the morphology, ellipsoidal nanoparticles

were added as seeds into a diluted mother solution (0.025 M
ZnSO4 and 0.5 M NaOH) for the basic route. No precipita-
tion was observed without the seed particles (basic route 2–1),
because the final concentration of Zn2+ was lower than the typ-
ical condition of basic route 1 (0.050 M). In this case, the final
pH of the resultant solution was slightly changed by the dilution
(pH 12.9). This fact indicates that the nucleation did not occur
practically at a relatively low concentration whereas the basic
solution was supersaturated. Here, the addition of seed particles
could mediate the precipitation accompanied with the growth of
ZnO crystals. As shown in Fig. 3, nanorods were obtained by
seed-mediated crystal growth (basic routes 2–2 and 2–3). Since
the aspect ratio of the seed-mediated products was higher than
that of the original seed (Table 2), the ZnO particles were pref-
erentially grown in c axis. The aspect ratio increased through
promotion of the axial growth by decreasing the amount of the
seeds in the mother solution. Moreover, these nanorods exhib-
ited a narrow size-distribution in comparison with those prepared
without the seeds (Fig. 5). Regarding to the product yield, it was
not sufficient without using seed particles (acidic route: 11.4%;
basic 1: 7.0%). However, the yield was found to be drastically
increased to 73.0% by introduction of the seed particles (basic
2–3).
A typical reaction solution was diluted with an excessive
amount of water to lower the degree of supersaturation during the
precipitation (basic route 3). As shown in Fig. 2(e) and (f), micro-
metric branching rods with hexagonal habits were obtained in
the solution. The definite hexagonal features were not observed
on the nanoparticles (Fig. 2(b)) and nanorods (Fig. 2(d)). In the
Fig. 1. Typical X-ray diffraction patterns of the precipitates obtained through diluted solution, considerably large ZnO crystals were gradually
(a) acidic route, (b) basic route 1, and (c) basic route 3.
grown at a relatively low degree of supersaturation. Interestingly,
the tilted angle of most branches on a basal rod was observed to
pared through basic route 1 were estimated to be 53 and 624 nm, be around 90◦ . Similar structures of wurtzite ZnO rods having
respectively, whereas the length ranged widely from 230 to oriented branches with a tilted angle of 80 ± 3◦ were reported
1310 nm. The broadened diffraction peaks observed in profile as a secondary branch crystal [34]. Therefore, the branching
(a) in Fig. 1 reveal that particles grown in the acidic route were rods are suggested to be twinned crystals rather than random
smaller than those formed via the basic routes. The grain sizes aggregates of independently grown rods.
evaluated form FESEM images for the nanoparticles grown in
the acidic route are consistent with the crystallite sizes (34 nm in 4. Discussion
a axis and 56 nm in c axis) estimated from the (1 0 0) and (0 0 2)
diffraction peaks in profile (a) using Scherrer’s formula. Wurtzite-type ZnO crystals were directly grown in a basic
solution containing Zn2+ ions at pH ∼13 [9]. Crystalline
Table 2 particles were gradually formed in a suitable degree of supersatu-
Shapes of wurtzite-type ZnO particles ration for crystal growth at pH ∼13 as shown in Fig. 6. However,
Route Shape Sizesa (nm) Aspect ratio the morphology of the resultant ZnO particles depended on the
(=length/width) condition during the precipitation. A large amount of nuclei of
Length Width
ZnO were generated through the acidic route, because the degree
Acidic Ellipsoid 44 32 1.4 of supersaturation on the initial stage was extremely high due to
Basic 1 Rod 624 53 12 the low solubility of ZnO under the acidic condition (acidic route
Basic 2–1 No precipitation – – –
Basic 2–2 Rod 539 98 5.5
in Fig. 6). Further crystal growth was then suppressed because
Basic 2–3 Rod 208 49 4.2 most of the Zn2+ ions were consumed for the initial nucleation.
Basic 3 Flower-like 4200 320 13 Finally, the resultant particles were nanometric grains with an
a The length and width of ZnO particles were fundamentally obtained from ellipsoidal shape. On the other hand, the nucleation was lim-
the median values of the cumulative undersize distributions of the particles. The ited on the initial stage of the basic route because of the low
values for basic route 3 were estimated from typical several products shown in degree of supersaturation in the mother solution at pH 13.6
Fig. 2(e). (basic route 1 in Fig. 6). Thus, subsequent crystal growth was
 T. Kawano, H. Imai / Colloids and Surfaces A: Physicochem. Eng. Aspects 319 (2008) 130–135
Fig. 2. FESEM images of ZnO particles prepared through (a and b) acidic route, (c and d) basic route 1, and (e and f) basic route 3.
promoted on the next stage in the solution containing abun-
dant Zn2+ ions. The formation of nanorods elongated along c
axis indicated that preferential growth occurred in the c direc-
tion of the wurtzite structure in the basic route. Since anionic
zinc species, Zn(OH)4 2− , dominantly exist under a highly basic
condition, the growth in the c direction could be initiated with
preferential adsorption of the anionic precursor on the positively
charged (0 0 1) face.
The length of nanorods prepared through basic route 1 exhib-
ited a wide distribution (Fig. 5). However, monodispersion is
generally required for homogeneous functionality of colloidal
and composite materials. The wide distribution of the nanorods
is attributable to the time variance of the nucleation during the
precipitation reaction. In the present study, seed-mediated crys-
tal growth was found to be effective for the control of the shape of
the nanoparticles. In a mother solution at relatively low degree of
supersaturation (0.025 M ZnSO4 and 0.5 M NaOH), the nucle-
ation of ZnO crystal could not occur, but the crystal growth
could be induced around the seed particles added into a mother
solution (basic route 2 in Fig. 6). Then, narrow size-distribution
of the ZnO rods was achieved by homogeneous crystal growth
133
of the seed particles. The length of the rods increased primarily
by decreasing the number of seeds. Here, the separation of the
nucleation and the crystal growth is essential for the morpho-
logical control.
As shown in Fig. 2(e) and (f), micrometric ZnO rods hav-
ing a branching morphology were obtained by dilution of the
reaction solution (basic route 3). In this case, a small number
of nanoparticles could be generated on the initial stage before
the dilution (basic route 3 in Fig. 6). The considerably large rods
having hexagonal habits would be grown form the nanoparticles
at a low degree of supersaturation. Since the rod size obtained
in the diluted solution was larger than that using seed parti-
cles, the amount of the nanoparticles prepared on the initial
stage was smaller than that of the seeds. Interestingly, branch-
ing, thick rods were obtained through basic route 3, although
longer nanofibers would be formed with a smaller amount of
seeds with basic route 2. These facts suggest that the growth
condition on the later stage in basic route 3 was slight different
from that in basic route 2 using seeds. Similar branching mor-
phologies were obtained by hydrothermal treatment at 150 ◦ C
in systems containing Zn(NO3 )2 –NaOH (or KOH) [28] or zinc
134 T. Kawano, H. Imai / Colloids and Surfaces A: Physicochem. Eng. Aspects 319 (2008) 130–135

Fig. 5. Cumulative undersize distribution (width and length) of ZnO particles

prepared through the basic routes. The plots were shown with the following
symbols: () basic 1; () basic 2–2; () basic 2–3.

salt–ethylenediamine (or triethanolamine) [32]. A certain angle

of branching indicates the formation of twinned crystals under
a relatively high degree of supersatruration. Thus, the degree
of supersaturation on the later stage in basic route 3 is tenta-
tively estimated to be larger than that in basic route 2, whereas
the final concentrations of ZnSO4 and NaOH were the same
for both routes. The concentration of zinc ions and the degree
of supersaturation were lowered with the crystal growth of the
seeds. On the other hand, a decrease in the concentration of
zinc ions is assumed to be very slow due to a small amount of

Fig. 3. FESEM images of ZnO particles prepared with seeds through basic
routes 2–2 (a) and 2–3 (b).

Fig. 6. Phase stability diagrams for crystalline ZnO–H2 O [9,12,35]. Arrows

Fig. 4. (a and b) FETEM images of the ZnO nanorods prepared through basic demonstrate variations of pH and zinc concentration through acidic, basic 1,
route 1. basic 2, and basic 3 routes, respectively.
 T. Kawano, H. Imai / Colloids and Surfaces A: Physicochem. Eng. Aspects 319 (2008) 130–135
nanoparticles as seeds in basic route 3. Therefore, the branching
would occur on the basal rods. However, further investigation
is required to clarify the details of the formation mechanism for
the complicated morphologies.
5. Conclusions
Various shapes of wurtzite-type ZnO crystals including
nanomeric ellipsoids, nanorods and micrometric branching rods
were prepared by a simple aqueous system using ZnSO4 and
NaOH solutions. The morphology of ZnO particles would be
governed by the balance of the nucleation and crystal growth
determined by the reaction route. The aspect ratio and size
distribution of the nanorods were successfully controlled by
seed-mediated crystal growth in basic solutions.
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