Int. J. Electrochem. Sci.

, 7 (2012) 2077 - 2090

International Journal of
ELECTROCHEMICAL
SCIENCE
www.electrochemsci.org

Pulsed- Electrochemical Synthesis and Characterizations of

Magnetite Nanorods
Hassan Karami1,2*, Elham Chidar1
1
Department of Chemistry, Payame Noor University, P. O. Box 19395-3697, Tehran, Iran
2
Nano Research Laboratory, Department of Chemistry, Payame Noor University, Abhar, Iran
*
E-mail: karami_h@yahoo.com

Received: 28 December 2011 / Accepted: 7 February 2012 / Published: 1 March 2012

Magnetite nanorods are synthesized by exerting pulsed current in potassium hydroxide solution for the
direct oxidation of iron electrode. The prepared samples are characterized by X-ray diffraction (XRD),
scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive
X-ray (EDX). The effects of synthesis parameters such as pulse height (current amplitude or current
density), pulse frequency, solution temperature, potassium hydroxide concentration and type and
concentration of synthesis additives on the morphology and particles sizes are investigated by the “one
at a time” method. The optimized conditions are 2 M potassium hydroxide, 45°C solution temperature,
18 mA.cm-2 pulse height, 8 Hz pulse frequency, and 1 g.L-1 cetyltrimethyl ammonium bromide
(CTAB) as synthesis director additive conditions to synthesize nanostructured magnetite. In the
optimized conditions, nanomagnetite is synthesized in nanorod form with 67 nm average diameter and
900 nm average lengths.

Keywords: Nanomagnetite; Nanorods; Pulsed current, Electrosynthesis

1. INTRODUCTION

Physical and chemical properties of nanoscale particles are very different from the bulk
materials [1-3]. This change of behavior is the same for iron oxide [4]. Among the numerous metal
oxides, iron oxide (Fe3O4; Magnetite) nanoparticles are of intense interest and have been extensively
investigated for their applications. Magnetite has been attracting attention in the biomedical
applications because of its biocompatibility and low toxicity in the human body [5, 6]. Also magnetite
has been used as a catalyst for many reactions of important industrial productions [7-10] such as the
Int. J. Electrochem. Sci., Vol. 7, 2012 2078

NH3 production, alcohol oxidation, and Fisher-Tropsch synthesis for hydrocarbons and it can catalyze
oxidation/reduction reactions [11]. On the other hand, magnetite was used in pigment and related
industries [12]. Iron oxide (magnetite) can also be used in wastewater purification [13]. It can be an
absorbent for heavy metal from water [14] .The synthesis of iron oxide nanoparticles of controlled
shapes has attracted much attention because the physical and chemical properties depend strongly on
particles size and morphology.
During the past several years, the development of reliable, simple and efficient methods for
synthesizing large amounts of uniformly sized and novel structured iron oxide nanoparticles has been
one of the main goals in chemistry research. Recently several chemical methods are employed to
synthesize iron oxide nanoparticles such as sol-gel [15], hydrothermal [16, 17], solid state [18, 19], wet
milling [20], pyrrolysis [21], and microemulsion [22]. The synthesis method plays a key role in
determining the morphology, particles sizes, and shape. On the other hand, the electrochemical
methods were used to synthesize different nanostructured materials, such as Palladium [23], SnO2 [24]
and super-hydrophilic polypyrrole [25]. Cyclic voltammetry [26], potentiostatic [27, 28], galvanostatic
[29, 30] and pulsed current [31-36] as different electrochemical techniques were used to synthesize
nanoparticles. Many reports that show pulsed current routes present a simple, quick, and economical
method for the preparation of various types of nanoparticles.
In previous studies, we successfully applied the pulsed current technique to synthesize lead
dioxide nanoparticles [32, 33], cadmium sulfide nanofibers [34], cobalt nanorods [35], iron
nanoclusters [36], and nickel nanoclusters [37].
In this work, we synthesized iron oxide nanoparticles by the pulsed current electrochemical
method on the surfaces of iron-based electrodes immersed in alkaline solution. The pulsed current
technique has some advantages such as being nonhazardous and, inexpensive and it is a method
considered proper for use in laboratory and industrial applications alike. Nanomagnetite is produced in
this method with high purity. The effects of experimental parameters of the synthesis, such as pulse
current, pulse frequency, solution temperature, potassium hydroxide concentration and synthesis
additives have been studied. The amounts of synthesis parameters were varied to find the optimum
conditions to synthesize magnetite nanorods. The techniques of SEM, TEM, EDX, and XRD were
used to investigate the morphology, the particles sizes, and the composition of the prepared iron oxide
samples.

2. EXPERIMENTAL

2.1. Materials

Potassium hydroxide (KOH) was purchased from Merck and used without any purification.
Sodium dodecyle sulfate (SDS), triton X-100, cetyle trimethyl ammonium bromide (CTAB), polyvinyl
pyrrolidone (PVA), saccharine and glycerol with high purity were obtained from Loba Chimie (India).
Double-distilled water was used in all experiments.
Int. J. Electrochem. Sci., Vol. 7, 2012 2079

2.2. Instrumentals

The morphology and the particles sizes of the iron oxide samples were studied by a Philips
scanning electron microscopy (XL30 model). A Philips X´Pert diffractometer with Cu (Kα) radiation
(λ = 0.15418 nm) was used to study the phase composition and the particles sizes of iron oxide
samples. The constant current was supplied by an MPS-3010L model of power source (Taiwan Matrix
Co.). A home-made electrical pulse apparatus was used to create the consistently current pulses. The
temperature of the synthesis solutions was kept constant by a water bath (Pars Azma Co., Iran).

2.3. Procedure

First, the iron electrodes were put in concentrated nitric acid for 1 min, then twice rinsed with
distilled water to clean any surface pollutant. An electrochemical cell containing three iron electrodes
(two cathodes and one anode) was immersed in potassium hydroxide solution. The different amounts
of pulse currents were exerted into this cell to oxidize iron anode into iron oxide nanoparticles for 24 h.
The prepared particles were then collected by a paper filter and dried at 400º C for 2 h. The effects of
different parameters, such as reaction temperature, pulse current, pulse frequency, potassium
hydroxide concentration and type and concentration of different additives, were optimized by the "one
at a time” method to obtain uniform nanorods.

3. RESULT AND DISCUSSION

Iron substrate was used as the initial material to be converted into iron oxide. First, the used
iron electrode was analyzed by Energy Dispersive X-ray (EDX) to verify its acceptable purity. Figure
1 shows the EDX patterns.

Figure 1. EDX patterns for the iron oxide sample that synthesized at a pulse height of 3mA.cm-2, pulse
frequency of 8 Hz, solution temperature of 25ºC and 4 M potassium hydroxide concentration
Int. J. Electrochem. Sci., Vol. 7, 2012 2080

Based on the data shown in Fig. 1, the iron substrate has only Mn (1.86 %wt) and Cr (1.49
%wt) as impurities. Chemical specifications of Mn, Cr and Fe reveal that Fe is oxidized before Cr and
Mn. Therefore, during controlled oxidation of iron, Mn and Cr have no interference.
During the synthesis process, direct current with stable amplitude was provided by a common
power supply instrument. The output of power the supply system was connected to the home-made
pulse maker. The output current of the pulse system is a dc pulse. In the present method, each pulse
cycle contains one pulse time (Ton) and one relaxation time (Toff). Pulse frequency is the number of
pulse cycles applied in a time unit (1 s). Figure 2 shows the used pulse diagram and its parameters.

Figure 2. Pulse diagram used for synthesizing iron oxide nanostructures

The pulsed current technique has four instrumental variables including pulse time (ton),
relaxation time (toff), pulse height and pulse frequency. Based on previous studies [32-37], the toff/ton
ratio of 3 is suitable to synthesize metal oxide nanoparticles. Therefore in this study, we used this ratio,
but the other pulse parameters including pulse height, pulse frequency and pulse time were optimized
in this work. Besides pulse parameters, the effects of chemical parameters, including concentrations of
potassium hydroxide and synthesis additives and synthesis temperatures were studied on the
morphology, the particles sizes and the composition of the samples. In the following sections, the
optimization experiments and the obtained results will be discussed.

3.1. Effect of pulse height

In the present method, pulsed current with constant amount of current during exerting the pulse
into the electrochemical cell is used to direct oxidation of iron substrate. During exerting the current
pulse into the system, cell voltage can increase from zero up to a final value. The cell voltage depends
on three factors including cell temperature, solution conductivity and the distance between anode and
cathode. In a typical experiment according to the section 2.3, the cell voltage can increase from zero up
to 12 V.
Int. J. Electrochem. Sci., Vol. 7, 2012 2081

In the first experiment, the effects of pulse height were evaluated on the synthesis of iron oxide
nanoparticles. The amount of height varied from 3 to 200 mA.cm-2, but the amounts of other
parameters were constant (temperature 25ºC, pulse frequency 8 Hz and potassium hydroxide
concentration 4M). Figure 3 shows the morphology and particles sizes of the synthesized samples.

Figure 3. SEM images of the iron oxide samples that synthesized at different current densities,
namely, 3 mA.cm-2 (a), 18 mA.cm-2 (b), 100 mA.cm-2 (c), 150 mA.cm-2 (d) and 200 mA.cm-2
(e).

Figure 3 shows that, the pulse current of 18 mA.cm -2 causes the formation of uniform and
organized particles with respect to the other currents. In pulse current of 3 mA.cm-2, the synthesis rate
was very slow; thus the total time of synthesis was very long. By using 3 mA.cm-2, we synthesized an
Int. J. Electrochem. Sci., Vol. 7, 2012 2082

amorphous sample with low porosity. The porosity of samples is increased by increasing pulsed-
current density (pulse height) of up to 18 mA.cm-2. At this density, magnetite nanorods start to form.
Because of greater nucleation rate at higher currents, all nanoparticles were agglomerated. Also, no
nanorods appeared in the samples that synthesized at higher current densities. Therefore 18 mA.cm -2
was selected as the optimum current density (pulse height) for further studies.
There are many reports about the growth mechanisms of magnetite nanorods that synthesized
by the non-electrochemical methods [38-41]. The growth mechanism of magnetite nanorods in
pulsed-electrochemical synthesis is probable different than those of previous reported methods such as
anisotropic growth. In the pulsed current synthesis, particle growth is slow so that magnetic properties
of an initial magnetite seed formed on the surface of the electrode induce a controlled direction to joint
the next produced magnetite species (iron and oxygen ions) until formation of a nanorod.

3.2. Effect of pulse frequency

Figure 4. SEM images of the samples that synthesized at different pulse frequencies; (a) simple
constant current, (b) 6 Hz, (c) 8 Hz, (d) 14 Hz, and (e) 16 Hz.

The effects of pulse frequency were studied on the morphology and the particles sizes of iron
oxide nanoparticles. The amount of pulse frequency varied from 0 to 16 Hz, but the other parameters
Int. J. Electrochem. Sci., Vol. 7, 2012 2083

were constant (temperature 25 ºC, pulse height 18 mA.cm2-, and potassium hydroxide concentration
4M). Figure 4 shows the SEM images of iron oxide (magnetite) samples that synthesized at different
pulse frequencies.
It is obvious from Fig 4a that constant current (pulse frequency of 0) is not suitable to
synthesize iron oxide nanostructures. By using pulsed current, we converted the amorphous and
agglomerated samples to the nanostructured sample (Fig. 4b and 4c). At frequency of 8 Hz, the
agglomeration of iron oxide particles was decreased and the particles changed to needle shape
nanorods. At the higher frequencies (12 Hz: Fig. 4d; 16 Hz: Fig. 4e), the iron oxide particles are
transferred to agglomerated and amorphous powder because the relaxation time between two
consequent pulses is very low; thus before the particle formation in the first pulse is compeleted, the
next pulse will be applied. This phenomenon causes large agglomerated particles to form.
The obtained results showed that the pulsed-current technique can control the morphology of
the sample. The frequency of 8 Hz was chosen as an optimum pulse frequency for the electrosynthesis
of iron oxide nanoparticles.

3.3. Electrosynthesis temperature

Figure 5. SEM images of the iron oxide samples synthesized at different temperatures; (a) 0°C, (b)
25°C, (c) 45°C and (d) 75°C. Nanomagnetite and nanohematite peaks were marked by 1 and 2,
respectively.

Based on our previous studies [32-37], the temperature of electrosynthesis solution is an

important parameter that can affect the morphology, the particles sizes, and the composition of the
Int. J. Electrochem. Sci., Vol. 7, 2012 2084

final yield. The synthesized samples at different temperatures were characterized by SEM and XRD.
The SEM images shown in Fig. 5 present the effects of synthesis temperature on the morphology and
particles sizes of magnetite samples.

Figure 6. XRD patterns of the iron oxide samples synthesized at different temperatures; (a) 0°C, (b)
25°C, (c) 45°C and (d) 75°C. Nanomagnetite and nanohematite peaks were marked by 1 and 2,
respectively.

Based on the SEM images shown in Fig. 5, the sample morphology was converted from
agglomerated spherical nanoparticles into nanorods when the synthesis temperature was increased to
46°C, from 0°C. The effects of temperature can be related to rate constants of two nucleation and
particle growth processes. At higher temperatures (>45°C), agglomeration and changing of
morphology into spherical nanoparticles were observed. By comparing the SEM images, the synthesis
temperature of 45 °C makes the most uniform and smallest nanorods. Therefore this temperature can
be selected for further studies, but the XRD patterns of the synthesized samples at different
temperatures make it necessary to change this selection.
Int. J. Electrochem. Sci., Vol. 7, 2012 2085

Figure 6 shows the effect of synthesis temperature on the XRD patterns. Based on the XRD
results, the sample synthesized at 25°C or lower contains only Fe3O4 (magnetite). At higher
temperatures, it contains Fe3O4 (magnetite) and α-Fe2O3 (hematite). The oxidation state of iron
increases when the synthesis temperature is increased so that at a higher temperature, iron can oxidize
to Fe3+ to form hematite. With respect to SEM images and XRD patterns, 25°C is suitable to
synthesize pure nanomagnetite.
The effect of temperature can be explained by considering the following reactions:

Eq. (1) Anodic oxidation at the surface of iron electrode: 3Fe  Fe 2  2Fe 3  8e

Eq. (2) Magnetite formation: 2Fe 3  Fe 2  8OH   Fe3O4  4H 2 O

Eq. (3) Hematite formation (at high temperature): 2Fe 3  6OH   Fe 2 O3  3H 2 O

At low temperatures (below 45°C), iron substrate is oxidized to Fe3+ and Fe2+ with ratio 2:1
(Eq. 1). Fe3+ and Fe2+ ions converted into nanomagnetite according to Eq. 2. At higher temperatures
(above 45°C), the Fe3+ content exceeds the 2:1 ratio. The Fe3+ excess is converted into nanohematite
(Fe2O3). Therefore the synthesized samples at higher temperatures (45°C and more) include a mixture
of nanomagnetite and nanohematite.

3.4. Effects of potassium hydroxide concentration

Potassium hydroxide concentration is a most- important factor in the proposed synthesis. Six
samples were synthesized in the solution containing 0.5, 1, 2, 3, 4 and 5 M potassium hydroxide to
evaluate the effect of this factor on the morphology and particles sizes of magnetite samples. The
synthesized samples were studied by SEM.
Figure 7 shows the SEM images of the samples. It can be seen in Fig. 7 that the morphologies
of samples change from irregular nanoparticles into uniform nanorods, when the hydroxide
concentration increases to 2 M from 0.5 M. At higher concentrations (more than 2 M), the samples are
strongly agglomerated and changed to amorphous sample.
The formation reactions for nanomagnetite and nanohematite have been presented in Eqs 2 and
3. At higher concentrations of hydroxide ion, the following reaction is carried out:

Eq. (4) Fe 3  Fe 2  5OH   Fe(OH ) 3  Fe(OH ) 2

Iron hydroxide species are seen as amorphous form in Figs 7e and 7f. Based on the presented
results, the 2 M potassium hydroxide solution is the best electrolyte to synthesize nanostructured
magnetite.
Int. J. Electrochem. Sci., Vol. 7, 2012 2086

Figure 7. SEM images of the samples synthesized at different hydroxide concentrations; 0.5 M (a), 1
M (b), 2 M (c), 3 M (d), 4 M (e), and 5 M (f).

3.5. Effects of synthesis additives

Surfactants are used as director agents to control the mechanism and kinetics of the reactions in
synthesis processes of nanomaterials. These additives can affect the morphology and particles sizes of
the final product [42]. The sizes distribution of the nanoparticles can be controlled by adding a
surfactant [43]. Different surfactants have been employed in the synthesizing of nanoparticles such as
bis(2-ethylhexyl) sulfosuccinate (AOT), sodium dodecyl sulfate (SDS), cetyltrimethyl ammonium
bromide (CTAB), polyvinyl pyrrolidone (PVP) and diethyl sulfosuccinate (DES) [44-46]. In this study,
the effect of PVP, saccharin, SDS, glycerol, CTAB and triton X-114 was investigated on the
morphology and particles sizes of iron oxide nanoparticles.
For a selection of suitable additives, several synthesizes were carried out in the presence of
different additives with the same concentration (5 g.L-1). Initial experiments showed that PVP, SDS
Int. J. Electrochem. Sci., Vol. 7, 2012 2087

and glycerol are not suitable as additives in magnetite electrosynthesis. These additives are made to
extremely decrease the rate of nanomagnetite synthesis. Figure 8 shows the SEM images of the
samples synthesized in the presence of saccharin, CTAB, and triton X-114 as synthesis additives.

Figure 8. Effects of saccharin (a), CTAB (b) and triton X-114 (c) on the morphology of nanomagnetite
samples. Each additive has been used in 5 g.L-1.

As Fig. 8 shows, CTAB acts better than the others. In the presence of CTAB, the sample
includes uniform nanorods. At the next step, the effects of CTAB concentration were studied on the
sample morphology (Fig. 9).
As Fig. 9 shows, by using 1 g.L-1 CTAB in 2 M potassium hydroxide solution, a sample
containing uniform nanorods can be synthesized. Therefore 1 g.L-1 CTAB is suitable to control the
formation of magnetite nanorods. CTAB in 2 M potassium hydroxide solution converts
homogeneously into cetyltrimethyl amine and potassium chloride. The formed cetyltrimethyl amine
acts as a suitable complex agent to stabilize iron ions (Fe2+ and Fe3+). The complex formation can
change kinetics and the mechanism of a magnetite formation.
Based on the results, optimized conditions to synthesize magnetite nanorods follow:
Potassium hydroxide: 2 M
Pulsed current amplitude: 18 mA.cm-2
Pulse frequency: 8 Hz
CTAB concentration as synthesis director (additive): 1 g.L-1
Int. J. Electrochem. Sci., Vol. 7, 2012 2088

Figure 10 shows the SEM image and TEM images of the magnetite nanorods synthesized at the
optimum conditions mentioned above. Because it is visible in Fig. 10, the optimized sample includes
uniform nanorods with 67 nm average diameter and 900 nm average lengths.

Figure 9. SEM images of the samples synthesized at different concentrations of CTAB; 3 g.L-1 (a), 2
g.L-1 (b), 1 g.L-1 (c) and 0.5 g.L-1 (d).

Figure 10. SEM images with different magnifications (a: 5000X and b: 15000X) and TEM images (c
and d) of the optimized magnetite nanorods
Int. J. Electrochem. Sci., Vol. 7, 2012 2089

4. CONCLUSIONS

Magnetite nanorods can be prepared by using a pulsed- current electrochemical method. In this
method, pulse height (pulsed current amplitude), pulse frequency, electrolyte concentration, solution
temperature and synthesis additive are effective parameters that can change the morphology, the
particles sizes, and the composition of samples. By using suitable amounts for the effective parameters,
we can synthesize pure magnetite in uniform nanorods. The solution temperature is a most important
parameter that can change a sample composition from magnetite to a magnetite and hematite mixture.
CTAB is a suitable additive to control the magnetite morphology. The experimental results showed
that the pulsed current method is a confident and controllable method to synthesize metal oxide
nanoparticles.

ACKNOWLEDGMENT
We gratefully acknowledge the support of this work by Payame Noor University Research Council
(Abhar Branch).

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