Materials Research Bulletin 47 (2012) 3952–3958

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Materials Research Bulletin

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Structural and frequency dependent dielectric properties of Fe3+ doped ZnO

nanoparticles
M. Mehedi Hassan a,*, Arham S. Ahmed a, M. Chaman a, Wasi Khan a, A.H. Naqvi a, Ameer Azam a,b
a
Centre of Excellence in Materials Science (Nanomaterials), Department of Applied Physics, Aligarh Muslim University, Aligarh 202002, India
b
Centre of Nanotechnology, King Abdulaziz University, Jeddah, Saudi Arabia

A R T I C L E I N F O A B S T R A C T

Article history: Polycrystalline Fe doped ZnO nanoparticles were synthesized through citrate gel method. Microstruc-
Received 19 January 2012 tural studies were carried out using XRD, FESEM, EDS, TEM, SAED and FTIR spectroscopy. XRD and TEM
Received in revised form 9 June 2012 results clearly show the formation of all samples in single phase without any impurity and the average
Accepted 10 August 2012
crystallite size has been observed to vary between 10 nm and 20 nm. Band at 500 cm1 observed in FTIR
Available online 18 August 2012
spectrum is attributed to the Zn–O stretching confirms the formation of ZnO nanoparticles. The dielectric
constant, loss tangent and ac conductivity were studied as a function of frequency and composition using
Keywords:
LCR meter. All the dielectric parameters show dispersion and decreases with increase in Fe content. The
A. Nanostructures
observed dielectric behavior is explained on the basis of Maxwell–Wagner model and Koops
B. Sol-gel chemistry
C. Impedance spectroscopy phenomenological theory. The impedance analysis shows only one semicircle of all samples suggesting
C. X-ray diffraction that the contribution of grain boundaries is dominated over grain contribution.
D. Dielectric properties ß 2012 Elsevier Ltd. All rights reserved.

1. Introduction
Metal oxide nanostructures such as zinc oxide (ZnO), indium
oxide (In2O3), tin oxide (SnO2) and doped oxides have been
intensively investigated in recent years [1–8]. Among these metal
oxide nanostructures, ZnO is gaining more interest because it is an
abundant, inexpensive and non-toxic material as compared to
others. ZnO is a II–VI semiconductor material with a wide band gap
(3.37 eV) and the large exciton binding energy (60 meV) at room
temperature [9]. Zinc oxide nanoparticles are used in a variety of
applications such as UV absorption, antibacterial treatment [10],
catalyst [11], photocatalyst [12] and additive in many industrial
products. It is also used in the fabrication of solar cells [13], gas
sensors [14,15], luminescent materials [16], transparent conductor
[17], heat mirrors and coatings [18]. Different physical methods
such as pulse laser deposition [19,20], vapor phase transparent
process [21] and chemical vapor deposition [22] have been
developed for the preparation of nanostructures of ZnO. Sol–gel
method is one of the most important wet chemical methods for the
preparation of metal oxide nanoparticles [23] which is based on
the hydrolysis of reactive metal precursor.
Many physical properties, such as electrical conductivity,
piezoelectricity and defect structure, are greatly influenced by
the amount of excess Zn and impurities [24]. There are various
* Corresponding author. Tel.: +91 9528204837; fax: +91 5712700042.
E-mail address: mehedi403@rediffmail.com (M. Mehedi Hassan).
ways to modify the dielectric and other properties of metal oxide
nanostructure. Introducing the dopant into the structure is one of
them. Literature review suggests that several additives (cations:
Fe, Cu, Co, Cr, Al, Mn, Mg; anions: P, S) can lead to an increase in the
surface area of ZnO based powders. The added active elements
stabilize the ZnO surface, and promote a decrease in grain size. It
has been found that Fe3+ doped ZnO nanoparticles with lower
crystallinity and high surface area have the higher catalytic activity
and sensor signal than both pure ZnO and Fe2O3 system [25]. In
many cases metal oxides such as SnO2, TiO2, CuO, CeO2, Fe2O3,
ZnFe2O4 were often used as dopants [26]. The dielectric properties
of pure ZnO are developed due to the defects of zinc excess at the
interstitial position and the lack of oxidation. As pure ZnO is
sensitive to oxidation, absorption of O2 is inclined to decrease its
dielectric properties. In cases where ZnO is doped with different
dopants, the dielectric properties are changed by extrinsic defects
and these trials have been attempted [27].
There are various papers reported on the structural, optical,
magnetic and gas sensing properties of Fe doped ZnO [28–33]. Kuo
et al. investigated ethanol vapor sensing with nanosize Fe doped
ZnO thin films. Bin et al. showed that large red shift in Raman
scattering and photoluminescence of Fe-doped ZnO nanocanti-
lever arrays. Ahn et al. reported the magnetic moment per Fe atom
increased with increasing Fe concentration. Cheng et al. studied
the structural, optical and magnetic properties of Fe-doped ZnO
and reported that with increasing the concentration of Fe, the
optical band gap shifts slightly to lower energies (66 meV for
x = 0.20) than that of the pure ZnO. Magnetization measurement

0025-5408/$ – see front matter ß 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.materresbull.2012.08.015
 M. Mehedi Hassan et al. / Materials Research Bulletin 47 (2012) 3952–3958 3953

indicated that all samples were ferromagnetic at room tempera-

ture. Dinesha et al. reported the temperature dependent electric
behavior of Fe doped ZnO and showed that the DC electric
conductivity increases with temperature in the range 300–600 K
while it decreases with the increase of Fe concentration [34]. To the
best of our knowledge there are few papers reported in literature
on detailed frequency dependent dielectric behavior of Fe doped
ZnO. We realized that the study of frequency dependent dielectric
properties of Fe doped ZnO nanoparticles is a least explored area
till now and we, therefore, were motivated to take up this task. This
paper reports the modification induced in structural, dielectric and
complex impedance properties of Fe doped ZnO nanostructure
synthesized by citrate gel method.

2. Experimental

2.1. Synthesis

Zinc acetate [Zn(CH3CO2)22H2O] and Ferric nitrate

[Fe(NO3)39H2O] were used as the sources of zinc and iron
respectively. In this synthesis procedure, citric acid was added to Fig. 1. X-ray diffraction patterns of Fe doped ZnO powder.
100 ml of distilled water to make its pH 1.5 at 50 8C under magnetic
stirring. Then required amounts of Zn(CH3CO2)22H2O and Table 1
Variation of crystallite size, lattice parameters and unit cell volume with doping
Fe(NO3)39H2O were added to dissolve. The Fe molar contents in
concentration.
the samples were 0%, 3%, 5%, 7% and 10%. When the solution
became homogeneous 10 ml of ethylene glycol was added and a sol Fe concentration Crystallite Lattice Unit cell
(%) size (nm) parameter volume (Å3)
was formed. Now required amount of aqueous ammonia was
added to solution drop wise. The resulting suspension was a (Å) c (Å)
continuously stirred for about 50 min. A yellow colored gel was 0 19.97 3.271 5.221 48.38
formed which was centrifuged at 6500 rpm and washed several 3 14.77 3.265 5.214 48.13
times with water and alcohol to remove organic impurities. Then 5 12.41 3.264 5.210 48.07
7 11.09 3.260 5.208 47.93
the gel was dried at 110 8C for 12 h in an oven. The dried gel was
10 10.58 3.258 5.204 47.84
ground to make fine powder. The dried powders were further
calcined at 450 8C for 2 h to obtain crystalline phase. Finally, Fe
doped ZnO nanoparticles were obtained. concentration, the (1 0 1) peak exhibits an increase in line
broadening. It is also observed from the XRD patterns that some
2.2. Characterization peaks appearing in pure ZnO at higher angles disappear in the Fe
doped ZnO samples. This indicates that the samples are transform-
Fe doped ZnO nanoparticles were characterized using XRD, ing into more ordered state as a result of Fe doping. The crystallite
FTIR, SEM and TEM. The crystalline phase, structure and particle size for all the samples was calculated using Scherrer’s formula
size of Fe doped ZnO nanoparticles were obtained by X-ray
diffraction using Cu-Ka radiations (l = 1.5406 Å´) in 2u range from
208 to 808. The particle size and morphology were obtained by 0:9l
D¼ ;
FESEM (NANO NOVA). The elemental constituent was determined b cos u
by using EDS attached with the FESEM. Transmission electron
microscopy (TEM) micrographs and selected area electron where l is the wavelength of X-ray radiation, b is the full width at
diffraction (SAED) pattern were obtained using a HR-TEM (Tecnai half maximum (FWHM) of the peaks at the diffracting angle u. The
G2 F20 Super Twin) at operating voltage 200 kV. The bonding calculated crystallite size of all samples is shown in Table 1. It is
between different atoms and chemical information of the particles clear from Table 1 that the crystalline size of ZnO decreased from
was collected by FT-IR spectra (Perkin Elmer). The Fe doped ZnO 20 nm to 10 nm when Fe3+ content increased from 0% to 10%.
pellets of 13 mm diameter and 1 mm thickness were prepared, The data shows that the presence of Fe3+ ions in ZnO prevented the
which were sintered at 600 8C for 6 h. The pallets were coated on growth of crystal grains. The variations in the lattice parameters
adjacent faces with silver paste forming parallel plate capacitor. and unit cell volume was also calculated for different doping
Dielectric and complex impedance measurements were carried out concentrations and presented in Table 1. The ionic radius of Fe3+ is
in the frequency range 75 kHz–7 MHz using Agilent LCR meter 68 pm whereas that of Zn2+ is 74 pm. When Fe is doped into ZnO
(4285A). nanostructure the Fe3+ ions substitute the Zn2+ ions. It may be
considered that Fe3+ ions cause the reduction of the lattice
3. Result and discussion parameters due to the smaller ionic radius which is already proved
by some authors [30–32]. XRD patterns also exhibit that as the Fe
3.1. X-ray analysis content increases, the intensity of XRD peaks decreases and FWHM
increases which shows the degradation of crystallinity and
Fig. 1 shows X-ray diffraction patterns of pure and Fe doped decrease in crystallite size. It means that the Fe3+ ions occupy
samples. All XRD patterns were analyzed using PowderX software the regular lattice site of Zn2+, they produce crystal defects around
which shows that all samples are in single phase with hexagonal the dopants and the charge imbalance also arises. Fig. 2 shows
structure and there are no anomalous peaks related to Fe metal variation of crystallite size with the concentration of Fe doped into
clusters or Fe oxides secondary phases. With increasing Fe ZnO nanostructure.
3954 M. Mehedi Hassan et al. / Materials Research Bulletin 47 (2012) 3952–3958

Fig. 2. Variation of crystallite size for Fe doped ZnO samples.

3.2. SEM and EDS analysis

The morphology of pure and Fe doped ZnO nanoparticles were

studied by FESEM. Fig. 3a and b shows the magnified SEM
micrographs for pure ZnO and 7% Fe doped ZnO sample
respectively. These figures show the presence of large spherical
aggregates of smaller individual nanoparticles of various sizes. It is
clear from the highly magnified images (Spectrum 1) of 7% Fe
doped ZnO, shown in Fig. 3c, that Fe doped ZnO particles exhibit
uniform shape and narrow size distribution with particle size in
the range 13–46 nm. Fig. 4 shows the energy dispersive X-ray
spectrum (EDS) for Fe doped ZnO nanoparticles. The EDS analysis
demonstrated that both Zn and Fe elements are present in the
sample which confirms the successful doping of Fe in the ZnO host
structure and corroborates the results obtained by XRD analysis.
The EDS results are also consistent with the atomic percentage of
Fe is 6.96% for 7% Fe-doped ZnO which confirms the dopant level in
the sample.

3.3. TEM and SAED analysis

Complementary morphological description can be achieved

through the TEM with the SAED study. Fig. 5(a) shows the TEM
image of 7% Fe doped ZnO nanomaterials. It is clearly shown from
the image the particles are more or less spherical in shape with
particle size distribution between 8 and 15 nm. The average
particles size has been calculated to be found 10 nm shown in bar
graph, Fig. 5(b) which is approximately equal to the size obtained
from the XRD spectra. Fig. 5(c) shows the selected area electron
diffraction (SAED) pattern. The bright points in SAED pattern show
the crystalline nature whereas the ring pattern confirms the
polycrystalline nature of the sample. All these images confirm that
Fe is successfully doped in ZnO nanostructure and the particles are
composed of many single crystallites of varying size and
orientation without any major lattice defects.

3.4. FTIR analysis

FTIR spectra were recorded in solid phase using KBr pellet

technique in the region 2000–400 cm1. FTIR spectra of pure and
doped ZnO nanoparticles are shown in Fig. 6. The band observed at Fig. 3. (a) SEM image of Pure ZnO. (b) SEM image of 7% Fe doped ZnO. (c) Highly
1628 cm1 is due to the OH bending of water. A strong band at magnified image of (Spectrum 1 of b) of 7% doped ZnO.
500 cm1 is assigned to the Zn–O stretching band which is
consistent with that reported elsewhere [35]. Shifting of this band
as a result of Fe doping suggests microstructural changes taking
 M. Mehedi Hassan et al. / Materials Research Bulletin 47 (2012) 3952–3958 3955

Fig. 4. EDS image of Fe doped ZnO.

Fig. 5. (a) TEM image, (b) bar graph and (c) SAED pattern of 7% Fe doped ZnO.

place in the ZnO matrix. Due to adsorption of CO, few peaks at (8.854  1012 F/m) and A is the cross sectional area of the flat
1125 cm1 (C–O), 1406 cm1 (C55C) and 1572 cm1 (C–H) are also surface of the pellet.
observed [36,37]. The complex or imaginary dielectric constant e00 for all the
samples was calculated using the relation:
3.5. Dielectric constant
e00 ¼ e0 tan d (3)
In solids, the dielectric properties can be explained as a function
of frequency of applied electric field, temperature, crystal structure
and other parameters. The dielectric response in a solid material
can be briefly described by expressing the relative dielectric
constant as a complex quantity made up of a real component and
an imaginary component, i.e.,

e ¼ e0 þ jė (1)

where e0 and e00 are the real and imaginary part of dielectric
constant, representing the amount of energy stored in a dielectric
material as polarization and the energy loss respectively, while
applying an electric field. In order to understand the influence of
microstructure, composition and intergranular potential barrier on
the electrical properties of ceramic, the frequency dependent real
dielectric constant can be calculated using the relation:

C pt
e0 ¼ (2)
e0 A
where Cp is the capacitance of the specimen in Farad (F), t is
thickness of pellet, e0 is the permittivity of free space Fig. 6. FTIR spectrum for Fe doped ZnO structure.
3956 M. Mehedi Hassan et al. / Materials Research Bulletin 47 (2012) 3952–3958

Fig. 8. Variation of dielectric loss for all samples at room temperature.

Fig. 7. Variation of real part of dielectric constant for all samples at room
temperature.

where tan d is the dielectric loss tangent which is proportional to
the loss of energy from the applied field into the sample (this
energy is dissipated as heat) and therefore denoted as dielectric
loss. Fig. 7 shows the variation of real part of dielectric constant
with respect to the frequency of applied electric field between the
ranges of 75 kHz to 7 MHz for all the samples. It is observed that
the dielectric constant decreases as doping concentration
increases. The decrease in dielectric constant indicates the
formation of microstructure with semiconducting ZnO grains
surrounded by insulating grain boundaries and also suggest the
existence of interface states in the grain boundaries. It is also
evident from Fig. 7 that all the samples show dielectric dispersion.
The dispersion is rapid at lower frequencies but it is slow and
approaches to almost frequency independent behavior at high
frequencies (microwave frequency). The observed dielectric
behavior can be explained in the light of Maxwell–Wagner
interfacial type of polarization [38,39] and Koops phenomenologi-
cal theory [40]. According to this model, a dielectric medium is
assumed to be made of well conducting grains which are separated
by poorly conducting (or resistive) grain boundaries. The grain
boundaries are found to be more effective at lower frequencies,
while grains are effective at higher frequencies. The grain
boundaries are formed during the sintering process due to the
superficial reduction or oxidation of crystallites in a porous
material as a result of their direct contact with the firing
atmosphere [41,42]. The frequency independent behavior of all
the samples at higher frequency of applied electrical field is just
because of the charge carriers which are responsible for different
mechanisms of polarization and that lag behind the applied
alternating field. As a result they cannot follow the changes in the
applied field over a certain frequency limit, as the frequency
increases.
similar to the dielectric constant. The value of tan d is large at lower
frequencies, while becomes lower at higher frequencies. Plot of
tan d for pure ZnO and 3% Fe doped ZnO display small peaks at
lower frequencies which may represent the relaxation peaks.
These peaks occur when jumping frequency of localized electric
charge carrier becomes approximately equal to that of the
externally applied ac electric field [43]. It is evident that the
overall values of tan d are found to decrease with increasing the
concentration of Fe3+ ions for all the samples.
3.7. ac conductivity
Fig. 9 shows the variation of ac conductivity (sac) for Fe doped
ZnO nanoparticles at room temperature. It is clear from the graphs
that the conductivity increases as the frequency of applied ac field
increases. The ac conductivity of a dielectric sample can be
calculated using the relation:
s ac ¼ e0 e0 v tan d (4)
where v is the angular frequency. It is also evident from Fig. 9 that
the ac conductivity decreases as the Fe content increases in the ZnO
matrix. It can be attributed to the fact the presence of Fe3+ hole
doping induced by Zn2+ vacancies which increases the donor
defects and dilute the system. Therefore, n-type conductivity of the

3.6. Dielectric loss

Dielectric loss (tan d) is represented as dissipated energy in a

dielectric system. It is considered to be caused by domain wall
resonance. At higher frequency the losses are found to be low since
domain wall motion is inhibited and magnetization is forced to
change rotation. According to Eq. (3) tan d is proportional to the
imaginary part of dielectric constant. The variation of tan d as
function of frequency at room temperature is shown in Fig. 8. It is
clear that the dielectric loss decreases with the increase in
frequency for all the samples which exhibit dispersion behavior Fig. 9. Variation of ac conductivity for all samples at room temperature.
 M. Mehedi Hassan et al. / Materials Research Bulletin 47 (2012) 3952–3958
Fig. 10. Variation of ln sac with respect to ln v for Fe doped ZnO.
host ZnO matrix decreases as Fe content increases. The ac
conductivity of dielectric materials is temperature and frequency
dependent, and obeys the empirical formula of frequency
dependence and is governed by the ac power law [44]:
s ac ðvÞ ¼ Bvn
where ‘B’ and ‘n’ are constants that depend upon both the
temperature and composition; B has the units of conductivity and
n is dimensionless. The value of n lies between 0 and 1. When n = 0,
the electrical conduction is frequency independent or dc conduc-
tion and for n  1, the conduction is frequency dependent or ac
conduction [45]. The exponent parameter n has been calculated for
each composition by plotting ln s versus ln v according to the
above equation as shown in Fig. 10, which represents straight lines
with slope equal to the exponent parameter n and intercept parts
equal to ln B on vertical axis at ln v = 0. Fig. 11 shows the variation
of ‘n’ as a function of composition. The values of the exponent ‘n’
have been found to vary between 0.0735 and 0.1057, which
suggests that the conduction phenomenon in the studied samples
is due to the hopping of charges.
3.8. Impedance analysis
There are two methods that can be used to measure cell
polarization: an ac method, and a dc method [46]. The polarization
Fig. 11. Variation of n with Fe content for Fe doped ZnO.
3957
Fig. 12. Cole–Cole plots for all samples.
resistance determined from ac measurements can be different
from that determined from dc measurements. In the ac method,
the cell is subjected to an AC source of variable frequency, and the
(5) cell response is measured as a function of frequency. An impedance
spectroscopy method is widely used to characterize electrical
properties of materials and their interfaces with electronically
conducting electrodes. The impedance measurements on a
material give the data having both resistive (real part) and reactive
(imaginary part) components. It can be displayed conventionally in
a complex plane plot (Nyqiust diagram) in terms of any of the four
possible complex formalisms, the permittivity (e*), the impedance
(Z*), the admittance (Y*), the electric modulus (M*) and dielectric
loss (tan d) or dissipation factor. They are related to one another
[47] as follows:
s00 M 00 Z0 Y0
tan d ¼¼ ¼ 0 ¼ 00 ¼ 00 (6)
s0 M Z Y
To distinguish between the grain and grain boundary contri-
bution of polycrystalline ZnO nanoparticles with 0, 3, 5, 7 and 10%
doped Fe contents, impedance spectroscopy measurements have
been carried out in the frequency range 75 kHz–7 MHz at room
temperature. Fig. 12 shows impedance complex plane plots (Z*-
plots) or Nyqiust plots obtained by plotting the imaginary part
with corresponding real part at room temperature. It is evident
that all samples show one semicircle, which is due to the
conduction of the grain boundaries only. In the term of impedance
plots, the lower frequency dispersion corresponds to the presence
in grain boundary and the higher frequency dispersion corre-
sponds to the processes in the grain.
4. Conclusions
In this paper we have successfully synthesize (0%, 3%, 5%, 7% and
10%) Fe doped ZnO nanoparticles using sol–gel citrate method. The
XRD and TEM patterns confirmed single phase formation of all
compositions without any impurities. Crystallite size and lattice
constants were observed to decrease with the increase in dopant
concentration. There is no change in the hexagonal symmetry of
ZnO with Fe doping. The dielectric parameters revealed normal
dielectric behavior. The dielectric constant and dielectric loss
decreases with increase in frequency and also dopant concentra-
tion, which has been explained on the basis of Maxwell–Wagner
model. The ac conductivity also shows the frequency and
composition dependent behavior. The complex impedance spectra
3958 M. Mehedi Hassan et al. / Materials Research Bulletin 47 (2012) 3952–3958
are signifying the control of grain boundary resistance in doped
materials.
Acknowledgements
Authors are grateful to the Council of Science & Technology
(CST), Govt. of UP, India for financial support in the form of Center
of Excellence in Materials Science (Nanomaterials). One of the
authors (M.M. Hassan) is grateful to the University Grants
Commission (UGC) for providing financial support in the form of
Maulana Azad National Fellowship.
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