Io3614891497

K. Vijaya Kumar et al Int. Journal of Engineering Research and Applications
ISSN : 2248-9622, Vol. 3, Issue 6, Nov-Dec 2013, pp.1489-1497

RESEARCH ARTICLE

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OPEN ACCESS

Structure-Property Correlation of Sol-Gel Processed
Co0.5Ti0.5ZnFeO4 Ceramic
K. Vijaya Kumar1*, M. Lakshmi2, M Buchi Suresh3
1

Department of Physics, Jawarharlal Nehru Technological University Hyderabad College of Engineering,
Nachupally (Kondagattu), Karimnagar-Dist., 505501, A. P, INDIA.
2
Department of Physics, SSJ Engineering College,V. N. Pally, Hyderabad, 500075, A.P., INDIA.
3
Centre for Ceramic Processing, International Advanced Research Centre for Powder Metallurgy and New
Materials, Balapur, Hyderabad, 500005, A. P., INDIA.

Abstract
Titanium doped Cobalt Zinc Ferrite nano powder of chemical composition Co0.5Ti0.5ZnFeO4 was synthesized
using sol-gel method and calcinated at different temperatures ranging from 500-800 0C. The X-ray diffraction
(XRD) and Fourier Transform Infrared techniques (FTIR), Scanning Electron Microscopy (SEM) and electrical
properties were carried out at room temperature. The grain size becomes larger with increase of calcination
temperature ranging from 47.71-83.62 nm. The X-ray diffraction studies reveal the formation of single phase
cubic spinel structure. The SEM micrographs show the uniform distribution of the particles, the average size
was estimated to be 0.350 μm. IR absorption bands are observed around 600 cm -1 and 400 cm-1 of the tetrahedral
and octahedral sites respectively. The effect of calcination temperature on electrical properties was studied and
conduction phenomenon in the samples is discussed.
Keywords: Ferrites, Sol-gel technique, XRD, SEM, EDS, FTIR, Dielectric constant, Dielectric loss

I. Introduction
In recent years, ferrite nano-particles have
drawn major attention because of their unique physical
properties, such as electrical conductivity, optical band
gap, refractive index and magnetic properties and
superior mechanical properties such as hardness of
nanomaterials and chemical properties compared with
their counterpart bulk materials. Polycrystalline nanoferrite particles have become immensely popular
magnetic materials for a wide variety of applications
such as electronic ignition systems, generators,
vending machines, medical implants, wrist watches,
inductor core, transformer circuits, magnetic sensors
and recording equipment, telecommunications,
magnetic fluids, microwave absorbers, other highfrequency applications, etc [1].
Cobalt–zinc ferrite as a special case has
interesting properties such as high mechanical
hardness, high Curie temperature, low porosity, high
chemical stability and reasonable cost [2]. They are
also used in radio-frequency circuits, high quality
ﬁlters, rod antennas, transformer cores, high-speed
digital tapes, read/write heads and other devices [3, 4].
A large number of methods have been developed to
prepare Co-Zn nano ferrite, such as
the coprecipitation, ceramic technique, forced hydrolysis,
microwave combustion method, salvo thermal method,
the standard solid- state reaction technique, solgel
method and the PEG – assisted hydro thermal method.
Among them we have selected the sol- gel method [5].
Sol-gel method has the advantage of good
stoichiometric control and production of ultrafine
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particles with a uniform size distribution in a relatively
short processing time. It is a simple process, which
saves time and energy consumption over the
traditional methods and requires only low sintering
temperature [6]. Recent studies have shown that
reduction in the size of magnetic materials may lead to
novel properties improved better than to the properties
of the bulk materials, due to small volume (super
paramagnetism) or high surface to volume ratio (spin
canting).
The diversity in properties of ferrites has
paved the way for the development of a wide variety
of ferrites for various applications such as permanent
magnets and electrical and electronic compounds [7,
8]. Their properties are very sensitive to the type of
substitution and sintering conditions such as
temperature, time and heating rate [9]. A selective
magnetic dilution is very important in ferrites. The
nonmagnetic ions that can be used in such dilution
should have ionic radius comparable with that of the
magnetic ions. In this case we can improve the
electronic and magnetic properties of ferrite samples.
It is found that small substitution of Fe ions by rare
earth ion may favorably inﬂuence the magnetic and
electrical properties of ferrite. It is thus possible to
obtain a good magnetic material for use in high
frequency applications.
The interesting and useful magnetic and
electrical properties of soft ferrites are governed by the
choice of the cations along with Fe2+, Fe3+ ions and
their distribution between tetrahedral (A) and
octahedral (B) sites of the spinel ferrite, as well as
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preparation conditions [10]. Although a tremendous
work has been reported on Zn doped Cobalt ferrites,
but the simultaneously huge investigation is required
on the variation of electrical and magnetic properties
of Co-Zn nano ferrites with Ti4+ ions [11-13]. In the
present work, sol-gel method is used to prepare
Co0.5Ti0.5ZnFeO4 nano powder. Further the effect of
the annealing temperature on the structural, micro
structural and electrical properties of Co0.5Ti0.5ZnFeO4
was investigated. In the present work, systematic study
of the electrical impedance spectroscopy, X-ray
density, SEM, bulk density and porosity of cobalt zinc
ferrites have been carried out in order to find the
relationship of these properties with the annealing
temperature.

II. Experimental Procedure:
Fe(NO3)3.9H2O (99.0% pure LOBAL
Chemie), Zn(NO3)2 .6H2O (99.0% pure SDFCL),
Co(NO3)2 .6H2O (99.0% pure SDFCL), TiCl4 (99.0%
pure SDFCL) and C6H8O7.H2O (Hydrated citric
acid)(99.5% pure MERK) were used as raw materials.
Stoichiometric amount of metal nitrates and
appropriate dosage of citric acid are dissolved in
minimum quantity of deionised water and stirred well.
Citric acid helps the homogenous distribution of the
metal ions to get segregate from the solutions. After
adjusting the metal nitrate and citric acid ratio to 1:1,
the mixed solution was neutralized to a pH value of 7
by adding liquid ammonia, since the base catalysts are
employed in order to speed up the reaction. After the
mixed solution was heated at 60˚C on a hot plate and
continuously stirred using a magnetic stirrer for 1 hr,
the solution turned into brown sol. Then heated at
100˚C and stirred constantly, the sol became sticky
gel. Increasing the temperature up to 200˚C led to the
self-ignition of the gel. The dried gel burnt in a self –
propagating combustion reaction until all the gel was
completely burnt out to form a voluminous and fluffy
powder with a large surface area. This powder is
further crushed in agate mortar to obtain the nano
sized powder. The resultant powder is heated at
500oC, 600oC, 700oC and 800oC, respectively for 4 h
to form spinel CoZnTi Ferrite nano particles. The
maximum particle size after grinding was 83.62nm.
These powders were pressed into pellets. The diameter
and thickness of the pellets are 10 mm and 2 mm,
respectively. The pellets were calcinated for 4 h at
950oC.
The X-ray diffraction (XRD) patterns of all
the prepared samples were taken by X-ray
diffractometer using Cu Kα radiation (λ=1.54°A), The
diffraction peaks are broad because of the nano meter
size of the crystallite. A careful analysis of the XRD
patterns helps to determine the respective planes and
face centered cubic structure of these ferrites. Well
resolved peaks in XRD pattern clearly indicate the
single phase and polycrystalline nature of the samples.
The size of crystal is evaluated by measuring the full
width half maximum (FWHM) of the most intense
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peak (311) from XRD and by using the Debye
Scherrer’s formula.
The size of the crystallite is evaluated using
the formula, 𝐷 =0.94λ / βCosθ, where D is the
crystallite size, λ is the wavelength of incident X-ray,
θ is the diffraction angle and β is the full-width at half
maximum (FWHM). For electrical characterization,
powders were compacted and sintered at 950 oC for 4
h. The AC impedance spectroscopy measurements
using two probe method were carried out with
solartron SI1260 impedance analyzer. For the
electrical measurements ohmic contacts were made by
using silver paste on two faces of the samples. For
temperature measurements specimens were placed in a
furnace where temperature could be controlled.
III. Results and discussion:The XRD patterns of Ti doped cobalt zinc
ferrite nano-particles at different calcinations
temperatures of 500, 600, 700 and 800 oC for 4 h are
shown in Fig. 1. Samples show the reflection planes of
(111), (220), (311), (222), (400), (422), (511) and
(440) which confirm the presence of single-phase of
ferrite phase with a face centered cubic structure.
Except for the impure phase of α-Fe2O3 which is found
in all calcined samples and occurs naturally as
hematite [14]. The XRD patterns also indicated
increase in crystallinity by increasing the calcination
temperature, due to the removal of stresses with the
heating process.
Table 1: Variation of particle size, crystallite size,
lattice constant and X-ray density with calcination
temperature.
SAMP Calcinati Crystal LATTIC X-RAY
LE
on
lite size
E
DENSI
Tempera
(D)
CONST
TY
ture
nm
ANT
g/cc
(˚C)
a(A˚)
R5
500
47.71
8.384
5.3702
R6

600

65.13

8.390

5.358

R7

700

83.38

8.392

5.354

R8

800

83.62

8.393

5.353

The values of particle size, lattice parameters
and X-ray density are furnished in Table-1. These
values are slightly lower than the lattice parameter of
the standard pattern (JCPDS 35-1373). From the table1, it can be clearly understood that with the increase of
the calcination temperature, the diffraction peaks
become sharper and increase in intensity. This
indicates intensification in crystallinity that originates
from the increment of crystalline volume ratio due to
particle size enlargement of the nuclei [15].
Fig. 2 shows the FTIR spectra of
Ti0.5Co0.5Zn1.0Fe1.0O4 nano particles of all the
considered samples in the range of 400 to 4000cm-1.
For ferrites, generally two assigned absorption bands
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appear around 600cm-1, which is attributed to
stretching vibration of tetrahedral group Fe-O and that
around 400cm-1, which is attributed to the octahedral
group complex Fe-O. The powders heat treated at
different temperatures show characteristic absorptions
of the ferrite phase with a strong absorption around
600cm-1 and another absorption in the range of 410450cm-1. The difference in the band positions with
calcination temperature is expected because of the
difference in the M2+-O2- distance for the octahedral
and tetrahedral groups. Waldron studied the
vibrational spectra of ferrites and attributed the sharp
absorption band around 600 cm-1 to the intrinsic
vibrations of the tetrahedral groups, and the other band
to that of the octahedral groups [16].
Fig. 3 shows the SEM images of
Co0.5Ti0.5ZnFeO4 ferrite prepared by sol-gel process
with different calcination temperatures. It can be seen
that the grain size becomes larger with the increase of
calcination temperature with the size range of 47.71 83.62 nm. The increase in grain size results in a
decrease of fraction of low coordinated atoms at the
surface skin of grains, which decreases the lattice
stresses due to inward shrinking atoms lying on the
surface. Therefore, the lattice parameter of the
prepared samples increased with an increase in grain
size. It is obvious that when cell volume increases, the
theoretical density decreases. Fig. 4 shows EDS
analysis of all the samples and it shows the presence of
elements such as Titanium, Cobalt, Zinc and Iron in all
the samples.
The particle size distributions of Ti doped
Co-Zn ferrite samples are shown in Fig. 5. The results
indicate that the samples prepared by the thermal
treatment method are uniform in morphology and
particle size distribution. The particle sizes increased
with increasing calcination temperature (Table 1). The
smallest particle size obtained in this study was 7 nm
for R5 and particle size reached to 47 nm at the
highest calcination temperature for R8. This suggests
that several neighboring particles fuse together to
increase particle sizes by melting their surfaces [17].
This grain growth of particle size enlargement at
higher calcination temperatures has been observed
previously in cobalt ferrite [18] and in zinc ferrite [19]
systems.
Fig. 6 shows the variation of the dielectric
constant with frequency measured at room
temperature. In all the samples the dielectric constant
decreases with increase in frequency exhibiting a
normal ferrimagnetic behaviour. A more dielectric
dispersion is observed at lower frequency region and it
remain almost independent of applied external field at
high frequency side. The sample R5 showed a
maximum dispersion while that R8 showed a least
frequency dependence. The dielectric dispersion
observed in the lower frequency region is due to
Maxwell–Wagner interfacial type of polarization,
which is in agreement with Koops phenomenological
theory [20]. The presence of Fe2+ ions in excess
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amount favours the polarization effects. The decrease
in dielectric constant with increase in frequency is due
to lag of hopping frequency of electrons between Fe 2+
and Fe3+ ions against the frequency of external applied
ac field and becomes independent beyond a certain
limit. The plot of dielectric loss tangent (tanδ) against
log frequency is shown in Fig. 7. All the samples show
an increase in tanδ with frequency up to a certain
value and decreases with increasing frequency
indicating a maximum at about 100 kHz of applied
frequencies. Similar types of maxima in the plot of
loss tangent versus frequency have been reported for
doped Zn ferrite [21] and doped Ti ferrite [22] ferrite
systems. The R5 sample however, shows more
dielectric loss at low frequency region as compared to
other samples, which may be due to the presence of
space charge polarization resulting into the more
inhomogeneous dielectric structure [23]. The condition
for observing a maximum in the dielectric loss of a
material is given by the relation wτ=1, where
w=2Πfmax and τ is the relaxation time. Therefore, a
maximum can be observed when the jumping or
hopping frequency of electrons between Fe2+ and Fe3+
becomes nearly equal to the frequency of the applied
field [24]. The sharp peak can be observed when both
the frequencies exactly matches with each other.
To elicit more information about the
mechanism of electrical transport in this compound,
impedance measurements are carried out as a function
of frequency between 0.1 Hz and 10 MHz. The
impedance spectroscopy helps in the separation of
grain and grain boundary effects because each of them
has different relaxation times, resulting in separate
semi-circles in complex impedance plot. The
relaxation time (τ) is a parameter that depends on the
intrinsic properties of the material governing the
distribution of resistive and capacitive components in
the material. So, the results obtained using impedance
analyser are basically unambiguous and provide true
picture of the sample electrical behaviour.
Fig. 8 shows the variation of Z″ with
frequency at different temperatures. The plots show
that Z″ values attain a peak (Z″max) for all the
samples, which shifts to higher frequency with
increasing temperature and all the curves merge at
higher frequencies. The shifting of peaks towards
higher frequency indicates that the relaxation time is
decreasing with the increase of temperature. The peak
broadening with increasing temperature suggests the
presence of temperature dependent electrical
relaxation phenomenon in the material [25] and is due
to the material in-homogeneity of the polycrystalline
sample. The relaxation process is due to the presence
of space charges whose mobility increases at higher
temperature. This shift in frequency maxima indicates
active conduction through the grain boundary. The
magnitude of Z″max also decreases with increase in
temperature. The merger of Z″ values in the high
frequency domain may be possibly an indication of the

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accumulation of space charges in the material at low
frequency and at higher temperature.
Fig. 9 shows the plot of Z′ vs Z″ (Cole–Cole
plots) taken over a frequency range of 1 Hz–10MHz of
Ti doped cobalt zinc ferrite calcined at different
temperatures. It is observed that for R5-R7 samples
single deviated semicircular arc is observed and two
semicircular arcs could be traced for R8 sample with
different values of resistance for grain (Rg) and grain
boundary (Rgb). The high frequency semicircle
corresponds to a bulk contribution and low frequency
corresponds to grain boundary effect. Hence grain and
grain boundary effects could be separated at these
temperatures. The values of Rg and Rgb are obtained
from the intercepts of the traced semicircles with Z′
axis. It can be clearly noticed that the values of Rg and
Rgb decreases with rise in calcination temperature.
Two semicircle arcs of the impedance spectrum can be
expressed by an equivalent circuit consisting of a
parallel combination of low resistances and constant
phase elements connected in series. The spectrum
reveals relatively large grain boundary contribution to
the total resistivity because close to the grain
boundaries, transport properties of the materials are
controlled by imperfections, expected to be present in
higher concentration than in grains leading to an
additional contribution to the grain boundary
impedance. The internal space charge created at the
grain boundaries may lead to a significant increase in
the concentration of mobile effects. The peak
frequency for grain boundaries is much smaller than
that for grains due to their large resistance and
capacitance compared to those of grains.
The AC resistivity was calculated using the
formula ρ=Rx(t/A), where R is resistance. It is
observed that the AC resistivity decreases with
increase in calcinations temperature. Also the
resistivity of all the samples was found to decrease
with the increase in frequency upto 10MHz. The
conduction in ferrites is electronic in nature as
proposed by Verway [26]. The charge transfer takes
place owing to hopping of electrons between Fe2+ and
Fe3+ states at the octahedral sites of the spinel lattice.
A variation in electrical resistivity with temperature of
heat treatments in CoxFe3yxO4 system, has been
observed by Na et al. [27]. From the above results, it is
concluded that the decrease in electrical resistivity was
attributed to the increase in electron concentration.

IV. Conclusions
Co-Ti-Zn Ferrite with particle size of 7-47
nm were synthesized by sol-gel process and calcined
at different temperatures. Different particle size of
Co0.5Ti0.5ZnFeO4 ferrite powders were obtained by
varying the calcination temperature and the grain size
becomes larger with the increasing calcination
temperature. To stabilize the particles, they were
thermally treated at various temperatures from 623 to
823 K at which calcination occurred, thereby
stabilizing the particles, controlling the growth of the
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nano-particles, preventing their agglomeration, and
creating a uniform distribution of particle sizes.
Particle sizes of 7–47 nm were obtained with
calcination temperatures between 623 and 823 K, as
confirmed by XRD and SEM analyses.

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28
(5)
(1992)
2433–2435

(311)

R5
R6
R7
R8

6000
5500

* (220) *
(222)
*

Intensity (arb. units)

5000
4500
4000

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(422)
(220) (331)
(511)

* (440)

3500
3000
2500
2000
1500
1000
500
20

40

60

80

2

Fig.1: X-ray diffraction patterns of Co0.5Ti0.5ZnFeO4 powders calcinated at in the temperature range 500800 oC
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Fig.2: FTIR plots of Co0.5Ti0.5ZnFeO4 powders calcinated at in the
temperature range 500-700 oC

Fig.3: SEM images of Co0.5Ti0.5ZnFeO4 powders calcinated at in the
temperature range 500-800 oC

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Fig.4: EDS analysis of Co0.5Ti0.5ZnFeO4 powders calcinated at in the temperature range 500, 600, 700 &
800 oC (top to bottom)

Fig.5: Particle size distribution of the powders heat treated at different temperatures
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Fig.6: Variation of capacitance with frequency

Fig.7: Variation of dielectric loss tangent with frequency

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Fig.8: Variation of Z″ with frequency at different temperatures of Co0.5Ti0.5ZnFeO4

Fig.9: Cole-Cole plots in the frequency range 1 Hz-10 MHz of Co0.5Ti0.5ZnFeO4
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