Powder Technology 212 (2011) 218223

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Frequency, temperature and In 3+ dependent electrical conduction

in NiFe2O4 powder
Sagar E. Shirsath a, b,, B.G. Toksha b, Maheshkumar L. Mane b, V.N. Dhage b, D.R. Shengule a, K.M. Jadhav b
a
b

Department of Physics, Vivekanand College, Aurangabad 431 001 (MS), India

Department of Physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad 431 004 (MS), India

a r t i c l e

i n f o

Article history:
Received 21 February 2011
Received in revised form 22 April 2011
Accepted 23 May 2011
Available online 31 May 2011
Keywords:
Ferrite
DC resistivity
Dielectric properties
AC conductivity

a b s t r a c t
A series of polycrystalline spinel ferrites with the composition NiInxFe2-xO4 (0 x 0.3) were prepared by the
solid state reaction to study the effect of In 3+ ions substitution on their dc electrical resistivity and dielectric
properties. The dc resistivity has been investigated as a function of temperature and composition. The indium
ion increases the dc resistivity and activation energy of the system. A study of the dielectric properties of these
mixed ferrites, as a function of composition, frequency and temperature, has been undertaken. The dielectric
constant (), dielectric loss () and dielectric loss tangent (tan) all decreases with frequency as well as with
the composition. The dielectric constant () and dielectric loss tangent (tan) were increases with increasing
temperature. AC conductivity increases with increase in applied frequency. The dielectric behavior of the
present samples is attributed to the MaxwellWagner type interfacial polarization. The conduction
mechanism in these ferrites is due to electron hopping between Fe 2+ and Fe 3+ ions on adjacent octahedral
sites.
2011 Elsevier B.V. All rights reserved.

1. Introduction
Nickel and substituted nickel ferrite is one of the versatile and
technologically important soft ferrite materials because of their
typical ferromagnetic properties, low conductivity and thus lower
eddy current losses, high electrochemical stability, catalytic behavior
etc. [13]. The polycrystalline soft ferrites having high dc resistivity
are used in making the core of the transformers and chokes, ferrites
having extremely low dielectric loss and therefore very useful for
microwave communication [4]. The dielectric properties of the
polycrystalline soft ferrites are sensitive to the applied electric eld
frequency, preparative methods and preparation conditions, chemical
compositions and doping of additives.
Study of the effect of temperature, composition and frequency on
the dielectric behavior and dc resistivity offers much valuable
information on the behavior of the localized electric charge carriers
which can lead to a good explanation and understanding of the
mechanism of electric conduction and dielectric polarization in ferrite
systems [5]. Electrical properties for substituted NiFe2O4 have been
studied by various researchers [68]. Our previous report deals with

Corresponding author at: Department of Physics, Dr. Babasaheb Ambedkar

Marathwada University, Aurangabad 431 004 (MS), India. Tel.: + 91 2402240950;
fax: + 91 2402361270.
E-mail address: shirsathsagar@hotmail.com (S.E. Shirsath).
0032-5910/$ see front matter 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2011.05.019

the structural and magnetic properties of In 3+ substituted NiFe2O4

[9]. Though the electric properties of In 3+ substituted MgMn [10],
NiZnTi [11] and MnZn [12] ferrites have been studied previously,
but In 3+ substituted NiFe2O4 ferrite system for their resistivity and
dielectric properties has not been treated in the literature. The
electrical conductivity and the magnetic properties of ferrites are
governed by the Fe 2+Fe 3+ interaction (spin coupling of the 3d
electrons) and also due to Ni 2+ ions [13]. According to literature
reports the resistivity of the parent spinel ferrite increases with the
substitution of In 3+ ions [10,11]. In view of this fact, we have
investigated the electrical and dielectric properties of In 3+ substituted
NiFe2O4 in order to understand the conduction mechanism and the
role of In 3+ ions.
2. Experimental procedure
Ferrite samples of the system NiInxFe2-xO4 with x values ranging
from 0.0 to 0.30 (in the step of x = 0.05), were prepared by the solid
state reaction. The details of the experimental procedure were already
discussed in our previous work [9]. The dc resistivity of the samples
was measured using the two-probe method where silver paste is used
as a contact material. The sample is rmly xed between two
electrodes to have a good surface contact. An auxiliary heater is used
for heating of all investigated samples. The temperature was
measured using a chromelalumel thermocouple.

S.E. Shirsath et al. / Powder Technology 212 (2011) 218223

219

(440)

(511)
(422)

(222)

(400)

(220)

Intensity (arb. unit)

(311)

0.30
0.25
0.20
0.15
0.10
0.05

5m

0.00

20

30

40

50

60

70

80

2 (degree)
Fig. 1. X-ray diffraction patterns of NiInxFe2-xO4.

3. Results and discussion

3.1. Structural properties
The X-ray diffraction patterns of all the samples are given in Fig. 1.
The X-ray diffraction patterns show the formation of single phase
cubic spinel structure without any impurity peak. The lattice constant
a was calculated from the interplaner spacing d-values and the
corresponding
Miller indices (hkl) using the equation,
p
a = d h2 + k2 + l2 [8]. It is observed that a increases from
8.337 to 8.424 as the In 3+ substitution increases. This can be
related to the fact that the In 3+ ion has ionic radius of 0.91 , which is
larger than the Fe 3+ (0.67 ). When the larger indium ions enter the
lattice, the unit cell expands while preserving the overall cubic
symmetry.
Small amount of pores in SEM image (Fig. 2) reveals that the
sintering is done in a satisfactory manner. The enhancement of the
grain growth is observed as effect of increasing indium content.
Uniform grains are progressively increased from 2.5 m (x = 0.0) to
8.1 m (x = 0.3) with increasing In 3+ content x and the ferrite sample
exhibit an aggregated continuous grain growth.

5m
Fig. 2. Typical SEM for (a) x = 0.1 and (b) x = 0.2 of NiInxFe2-xO4.

the sintering process, and electron exchange is believed to be between

the iron ions and nickel ions [15] which can be written as;
2 +

Ni

3 +

+ Fe

Ni

= 0

Eg
kB T


1

where 0 is the pre-exponential factor with the dimensions of

-cm, kB is the Boltzman constant (8.6173439 10 5 eV/K), Eg is the
activation energy, and T is the absolute temperature.
The conduction mechanism of ferrites can be explained on the
basis of the Verwey de Boer [14] mechanism that involves exchange of
electrons between the ions of the same elements present in more than
one valence state and distributed randomly over crystallographic
lattice sites. A very small amount of Fe 2+ and Ni 3+ are formed during

0.00
0.05
0.10
0.15
0.20
0.25
0.30

4.50x106

3.75x106

(cm)

2 +

+ Fe

The decrease in resistivity with increase in temperature is due to

the increase in drift mobility of the charge carriers. Also conduction in
ferrites is attributed to hopping of electrons from Fe 3+ to Fe 2+ at
elevated temperatures [4]. For spinel ferrite samples usually three

3.2. DC resistivity
Fig. 3 shows the variations in dc resistivity with temperature. It is
observed from Fig. 3 that for all the samples resistivity decreases with
increasing temperature, indicating the semiconducting nature of the
samples. The temperature dependence of resistivity found to follow
the Arrhenius equation [10].

3 +

3.00x106

2.25x106

1.50x106

7.50x105
1.2

1.3

1.4

1.5

1.6

1.7

1000/T (K-1)
Fig. 3. Variations in dc resistivity with temperature.

1.8

S.E. Shirsath et al. / Powder Technology 212 (2011) 218223

linear regions are observed in the log vs. 1000/T plot from room
temperature to well above Curie temperature (Tc). The change in slope
indicates change in conduction mechanism. The rst low-temperature
region is attributed to the conduction due to impurities, voids, defects, etc.
The second temperature region (up to Curie temperature) is attributed to
ferrimagnetic region. Third temperature region (above Curie temperature) is attributed to paramagnetic region [16]. In the present case we
observed only two regions separated at a particular temperature
(675860 K) which may corresponds to Curie temperature of the
samples. The temperature region above 860 K again follows linearity.
The Curie temperature determined from resistivity plots shows decreasing trend with increase in In3+ content, as shown in Table 1. This effect
can be explained on the basis of the number of magnetic ions present in
the two sublattices and their mutual interactions. As the concentration of
In3+ ions increases at the octahedral site, they replaced Fe3+ ions. This
leads to a decrease in the AB interaction of the type Fe3+(A)O2Fe3+(B).
Since Curie temperature is determined by an overall strength of the AB
exchange interaction, the weakening of the Fe3+(A)O 2Fe 3+(B)
interaction results in a decrease of the Curie temperature, when the
concentration of the In3+ ions increases successively in the nickel ferrite.
The resistivity plots (Figs. 3 and 4) clearly indicates that resistivity
also varies with the substitution of In3+ ions. It is observed from Fig. 4
that, as substitution of In3+ ions increase in NiFe2O4 the resistivity
founds to increase. Though the variation is less rapid for lower indium
concentrations, the substitutions have resulted in higher DC resistivities
with the increase in x. As is evident from the compositions all the
samples in the system contain a xed quantity of nickel. Since all the Ni2
+
ions invariably reside on octahedral sites [10], they are expected to
lock up with the Fe2+ ions that developed in the course of preparation,
which is inevitable, to maintain the charge balance [17]. This locking
process reduces hopping between iron ions such as Fe 2+Fe3+ in
octahedral sites and contributes to increase the resistivity slightly for all
the compositions in the system. Since indium ions are known to have
initial preference for A-sites [11], the substitution at rst is considered to
replace Fe3+ ions at tetrahedral sites only and this replacement of Fe3+
ions (0.67 ) by In3+ ions (0.91 ) obviously pushes the tetrahedron of
4 oxygen ions around it, thus, reducing the distance between two metal
ions in B-sublattice, which increases the hopping probability. This
process contributes to decrease slightly the resistivity as long as the
indium ions substitute iron ions at the A-sites. The observed resistivity
behavior for smaller concentrations of indium is in accordance with the
above two processes and suggests that the former process is slightly
dominant over the latter and the resistivity is slightly increased up to
x b 0.10 indium concentration. However, for higher concentrations of
indium, the resistivity is increased signicantly. This can be explained
with the supposition that the indium ions at higher concentrations
occupy B-sites as well [11]. It may also be due to the indium ions in
B-sites do not participate in the conduction processes, but limit the
degree of conduction by acting as scattering centers in the sense that
they reduce the number of Fe3+ ions [18]. The total number of iron ions
present at B-sites decreases with every step of indium concentration and
also the available Fe 2+ ions for hopping at these sites decrease in
number; thus, under these situation, it may lead to balance the
quantities of Fe2+ and Ni2+ ions to lock-up effectively and result in
Table 1
Activation energy in paramagnetic (Ep), ferrimagnetic (Ef) region, Ep Ef (Eg) and Curie
temperature (TC) of NiInxFe2-xO4.
Comp. x

Ep (eV)

Ef (eV)

Eg (eV)

TC (K)

0.00
0.05
0.10
0.15
0.20
0.25
0.30

0.421
0.445
0.467
0.49
0.547
0.616
0.707

0.052
0.066
0.077
0.088
0.121
0.132
0.165

0.369
0.379
0.390
0.402
0.426
0.484
0.542

840
795
771
745
730
695
675

2.4
0

at 600 C

Resistivity (x 106 -cm)

220

2.0

1.6

1.2

0.8

0.00

0.05

0.10

0.15

0.20

0.25

0.30

In content x
Fig. 4. Variations in dc resistivity with In3+ content x.

higher resistivity. The observed higher resistivity for higher indiumconcentrated samples is in agreement with these considerations. The
activation energies for conduction are computed from log verses 1000/
T plots for all the samples and the data is given in Table 1. In the table Ef
is the activation energy corresponding to ferrimagnetic region and Ep
that corresponding to paramagnetic region. It is noted from the table
that the activation energies in paramagnetic region is higher than those
in ferrimagnetic region. This could be attributed to the disordered states
of the paramagnetic region and the ordered states of the ferrimagnetic
region [19]. This also suggests that the process of conduction is affected
by the change in magnetic ordering [20]. It can also be noted from the
table that as In3+ content increases, the resultant activation energies
(Ep Ef = Eg) of electric conduction also increase. Higher values of
activation energy have been found to correspond to low conductivity
values of samples. It may also be due to the probability of electron
hopping responsible for electrical conduction in ferrites depends upon
the activation energy, which is associated with the electrical energy
barrier experienced by the electrons during hopping [21,22]. Hence
higher activation energy implies the higher electrical resistivity. The
magnitude of activation energy for all the compositions with In3+
content suggests that the conduction process in the present ferrites is
due to hopping of polarons.
3.3. Dielectric properties
3.3.1. Frequency dependent dielectric properties
The variation of the dielectric constant () and dielectric loss () as a
function of frequency for all samples at room temperature is shown in
Figs. 5 and 6 respectively. It can be seen that all the samples show strong
frequency dependence as well as composition dependence. Therefore, the
dielectric variation of present system may be separately discussed in two
aspects i.e. frequency dependence and composition dependence. It is clear
that the dielectric constant and dielectric loss decreases with increasing
frequency. The high values of dielectric parameters at lower frequency
region is due to MaxwellWagner interfacial type of polarization [23,24]
for the inhomogeneous double layer dielectric structure which is in
agreement with Koops Phenomenological theory [25].
The dielectric constant and dielectric loss decreases with increasing frequency and then reaches a constant value due to the fact that
beyond a certain frequency of external AC eld, the electron exchange
between Fe 2+ and Fe 3+ cannot follow the alternating eld. The
inhomogeneous dielectric structure was supposed to be consisted by
two layers. The rst one is the fairly well conducting large ferrite
grains which are separated by the second thin layer of the poorly
conducting grain boundaries. The grain boundaries of low

S.E. Shirsath et al. / Powder Technology 212 (2011) 218223

Dielectric constant (')

Table 2
Dielectric constant () and dielectric loss () measured at room temperature at 100 Hz
and at 1 MHz of NiInxFe2-xO4.

0.00
0.05
0.10
0.15
0.20
0.25
0.30

1800
1500
1200

221

Comp. x

0.00
0.05
0.10
0.15
0.20
0.25
0.30

900
600

Dielectric constant

Dielectric loss

100 (Hz)

1 (MHz)

100 (Hz)

1 (MHz)

1734
1213
728
436
346
218
109

65.84
46.09
27.65
16.59
13.17
8.30
65.84

1179
696
348
139
70
59
29

8.58
4.38
2.19
0.88
0.44
0.43
0.21

300

Fig. 5. Variation of dielectric constant () with log f.

observed from Fig. 7 that the dielectric loss tangent decreases with
increase in In 3+ content x. This can be attributed to the increase in
resistivity which causes reduction in tan. Our results on variation of
dielectric loss tangent as a function of frequency suggest that the
sample having compositional formula NiIn0.3Fe1.7O4 has the lowest
dielectric loss tangent tan and highest resistivity.

conductivity and high conductivity are found to be more effective at

lower frequencies while the ferrite grains of higher conductivity and
lower dielectric constant are more effective at high frequencies
[26,27].
Compositional stoichiometry is an important requirement for
obtaining low dielectric constant and dielectric loss. The composition
dependence of the dielectric constant at lower side frequency (i.e.
100 Hz) and at higher side frequency (i.e. 1 MHz) is given in Table 2. It is
clear that the dielectric constant and dielectric loss decreases with
increasing In3+ content. This behaviour can be explained by using the
assumption that the mechanism of dielectric polarization is similar to
that of conduction in ferrites, i.e. the electronic exchange interaction
Fe2+ Fe3+ results in a local displacement of the electrons in the
direction of an electric eld which determines the polarization of ferrites.
The presence of Fe2+ ions in excess amount favours the polarization
effects. Thus, the more dispersion observed in the sample with low
indium ion can be attributed to the presence of Fe2+ ions in excess
amount. The lower value of dielectric constant is obtained due to the
greater structural homogeneity and molecular level of mixing of starting
materials used in the preparation of ferrites by the solid-state technique.
Fig. 7 shows the variation of dielectric loss tangent (tan) as a
function of frequency. It can be observed from Fig. 7 that the dielectric
loss tangent decreases with increase in frequency. It can be further

3.3.2. Temperature dependent dielectric properties

The dielectric constant () and the dielectric-loss tangent (tan)
of the present investigation were computed according to Smit and
Wijn [28] as a function of temperature. The measurements were
carried out from 403 to 773 K, and Fig. 8 show the variation of the
dielectric constant with temperature at a xed frequency of 1 kHz. It is
clear from the gure that the dielectric constant increases with
increasing temperature for all samples. This temperature dependence
of the dielectric constant is in very good agreement with other spinel
ferrite [29,30], for which the dielectric constant increases with
increasing temperature. The variation of the dielectric-loss tangent
with temperature is given in Fig. 9, in which it is observed that the
dielectric-loss tangent increases with increasing temperature. According to Rabkin and Novikova [31], the process of dielectric polarization
in ferrite occurs through a mechanism similar to the conduction
process. From the electronic exchange Fe 3+ Fe 2+ and Ni 2+ Ni 3+,
one obtains the local displacement of the electron in the direction of
the applied electrical eld. This displacement determines the
polarization of both types of charge carrier, n and p, which contributes
to the polarization and depends on temperature. The temperature
dependence of the dielectric constant and dielectric-loss tangent can
be explained by the polarization effect. As temperature increases, the
electrical conductivity increases due to the thermal activity and
mobility of the electrical charge carriers according to the hopping

0
2

log f

0.00
0.05
0.10
0.15
0.20
0.25
0.30

Dielectric loss (")

1000

800

0.00
0.05
0.10
0.15
0.20
0.25
0.30

0.7

Dielectric loss tangent (tan )

1200

600

400

200

0.6
0.5
0.4
0.3
0.2
0.1
0.0

0
2

log f
Fig. 6. Variation of dielectric loss () with log f.

log f
Fig. 7. Variation of dielectric loss tangent (tan) with log f.

222

S.E. Shirsath et al. / Powder Technology 212 (2011) 218223

Dielectric constant (')

2800

2100

The ac conductivity (ac) was calculated from dielectric data using

the relation [33]

0.00
0.05
0.10
0.15
0.20
0.25
0.30

ac = 0 tan

1400

700

0
400

500

600

700

800

Temperature (K)
Fig. 8. Variation of dielectric constant () with temperature.

mechanism. Thus, the dielectric polarization increases, and consequently increases the dielectric constant and dielectric loss tangent.

3.3.3. AC conductivity
The electrical conductivity in ferrite is mainly due to hopping
electron between ions of the same element present in more than one
valance state, distributed randomly over crystallographicaly equivalent lattice sites. Ferrite structurally from cubic close packed oxygen
lattice with the cation at the octahedral (B) and the tetrahedral (A)
sites. The distance between two metal ions on (B) sites smaller than
the distance between two metals ions on (B) and (A) site, therefore
the hopping between (A) and (B) has very small probability compared
with that for BB hopping [32]. The hopping between AA sites does
not exist, due to that there are only Fe 3+ ions at A sites and any Fe 2+
ions formed during processing preferentially occupy B sites only [10].
The charges can migrate under the inuence of the applied eld
contributing to the electrical response of the system. Conductivity
increases with increase in applied frequency when the conduction is
due to hopping of electrons, on the other hand conductivity deceases
when the conduction is due to band conduction.

where is dielectric constant, 0 is permittivity of free space, tan is

the loss tangent and is the angular frequency. The variation of ac
conductivity with frequency is shown in Fig. 10. The plots are
observed to be almost linear conrming the polaron type conduction
present in the prepared samples. In ionic solids, the electrical
conduction is due to migration of ions and this ionic transport
depends on the angular frequency. Thus, ac conductivity is proportional to angular frequency conrming linear nature [34]. In the
present study it has been observed that the ac conductivity gradually
increases as frequency of the applied ac eld increases. The increasing
in (ac) with applied eld frequency can be explained on basis that the
pumping force of the applied frequency that helps in transferring the
charge carriers between the different localized states as well as
liberating the trapped charges from the different trapping centers.
These charge carriers participate in the conduction process simultaneously with electrons produced from the valence exchange between
the different metal ions [35]. In other words, increase in frequency
enhances the electron hoping frequency between the charge carriers
Fe 3+ and Fe 2+, the conductivity increases. Hole hopping between
Ni 2+ and Ni 3+ on B-site also contribute to electric conduction in
ferrites. The frequency dependence can be explained with the help of
MaxwellWagner two layer model or heterogeneous model [23,24] of
the polycrystalline structure of ferrites [25]. According to this theory
two layer formed dielectric structure. The rst layer consists of ferrite
grains of well conducting (ferrous ions), which is separated by a thin
layer of poorly conducting substances, which forms the grain
boundary. These grain boundary are more active at lower frequencies,
hence the hopping frequency of electron between Fe 3+ and Fe 2+ is
less at lower frequencies. As the frequency of the applied eld
increases, the conductive grains become more active by promoting
the hopping electron between Fe 3+ and Fe 2+ ions, thereby increasing
the hopping frequency. Thus we observed a gradual increase in
conductivity with frequency. Further, in the case of nickel ferrite
systems the conduction can be explained with the help of the
presence of nickel on octahedral sites which favors the conduction
mechanism as expressed in Eq. (2).
The composition dependence of the conductivity (ac) for all
samples shows that the ac conductivity increases as the In 3+ ion

0.00
0.05
0.10
0.15
0.20
0.25
0.30

0.00
0.05
0.10
0.15
0.20
0.25

-3.5
-4.0
-4.5

log ac

Dielectric loss tangent (tan )

-5.0
-5.5

-6.0
-6.5

0
400

500

600

700

800

Temperature (K)
Fig. 9. Variation of dielectric loss tangent (tan) with temperature.

10

12

log 2
Fig. 10. Variation of ac conductivity with frequency.

14

S.E. Shirsath et al. / Powder Technology 212 (2011) 218223

increases. The increase in (ac) with increasing In 3+ ion can be

explained on basis that the replacement of Fe 3+ ions by In 3+ ions on
tetrahedral A-site will increase the concentration of both Fe 3+ and
Fe 2+ in [B] sites, so the overall effective of the addition in the system
lead to increase the electrical conductivity.
4. Conclusions
Our experimental results on electrical and dielectric properties of
In 3+ substituted NiFe2O4 leads to draw the conclusions that, the
substitution of indium has brought signicant changes in electrical as
well as dielectric properties of nickel ferrite. The resistivity of nickel
ferrite increases with indium ion substitution. The formation of stable
electric bonds between the In 3+ and Fe 2+ ions and higher activation
energy implies the higher electrical resistivity. The polaron hopping is
responsible for the conduction through the ferrites. The dielectric
parameters decrease with increase in indium composition and
frequency. Increase in frequency enhances the electron hoping
frequency between the charge carriers of Fe 3+ and Fe 2+ which thus
increase the ac conductivity. The observed behaviour of electrical and
dielectric properties of NiInxFe2-xO4 (x = 0.00.3) makes these ferrite
suitable for the high frequency applications where eddy current losses
become appreciable because of their high resistivity and low dielectric
properties.
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