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International Journal of Electronic Engineering Research

ISSN 0975 - 6450 Volume 2 Number 1 (2010) pp. 125–134


© Research India Publications
http://www.ripublication.com/ijeer.htm

Magnetic and Transport Properties of Cobalt Ferrite

1
A.M. Bhavikatti, 2Subhash Kulkarni and 3Arunkumar. Lagashetty
1
Rural Engg. College, Bhalki, Karnataka state, INDIA
E-mail: arvindbhavikatti@gmail.com
2
Jaypraksh Narayan College of Engg, Mahaboobnagar, AP state, INDIA
E-mail: subhashsk@gmail.com
3
Appa Institute of Engg. Technology, Gulbarga, Karnataka state, INDIA.
E-mail: arun_lagshetty@yahoo.com

Abstract

Cobalt ferrite (CoFe2O4) is known as a hard magnetic material with moderate


magnetization. It is known for its high coercivity, great physical and chemical
stability. Here, electrical and magnetic properties of cobalt ferrite were
investigated to understand the conduction mechanism. Cobalt ferrite particles
were synthesized by microwave route. The XRD analysis confirmed the
formation of the ferrite structure. The room temperature hysteresis loops were
taken on the present sample in the field of 108KOe using VSM. The DC
resistivity was measured with a keithly 2010 electrometer using two probe
method in the temperature range (00C-4500C). The resistivity obtained here is
very high. But the conductivity obtained is very low. The electrical
conductivity results revealed a semiconductor behavior with the temperature.
The impedance spectroscopy technique was employed to investigate the
variation of real and imaginary part of impedances with different temperatures
at four different frequencies 1 KHz, 10 KHz, 100 KHz and 1 MHz. All
possible mechanisms contributing to the results have been discussed in this
paper.

Key words: Microwave route, Cobalt ferrite, hysteresis, Resistivity,


Conductivity, impedance spectroscopy.

Introduction
In the recent years, electromagnetic interference (EMI) has become a specific type of
environmental pollution, due to the rapid growth in utilization of electrical and
electronic devices in industrial, commercial and military applications, and much
126 A.M. Bhavikatti et al

attention has been paid towards finding suitable microwave absorber to solve this
problem [1][2]. Many researchers have indicated that ferrites with spinel structure and
hexagonal structure are promising electromagnetic microwave absorbent [3].The
spinel ferrites have remarkable magnetic and electrical properties especially CoFe2O4
is interesting because of its struructural, magnetic and electrical
conductivity[Trestman et al 1983, Broemme 1991 and Mohan et al 1992]. The
CoFe2O4 possesses a partially inverse structure and the degree of inversion depends
on the method of preparation and the heat treatment[ Sawatzky et al 1968].
CoFe2O4 has a spinel crystal structure. Spinel ferrites crystallize to cubic closed-
pack structure of oxygen ions in which tetrahedral [A] and octahedral [B] sites are
occupied by cations. They have the general formula (M1-λFeλ)A (MλFe 2-λ)BO4 where
M represented metal cations and λ inversion parameter.When the value λ is 1, then the
system is perfectly inverse spinel while 3/2 for the random arrangement and 0 for
perfectly normal spinel[4]. The quantities such as magnetization, coercivity,
permittivity, conductivity are greatly influenced by porosity, grain size and
microstructure of the sample.Ferrites containing cobalt exhibit several interesting
properties which make them suitable for switching and memory devices. At
frequencies above 50 MHz, cobalt is preferred to preclude magnetic losses. Cobalt is
invariably doped to various ferrites for the rapid relaxation to lattice [1].
Earlier [5], we have reported the results on ac conductivity and dielectric behavior
of cobalt ferrite. Now, the aim of the present work is to study the magnetic and
transport properties of cobalt ferrite over a wide range of frequencies as a function of
temperature using two probe and impedance spectroscopy techniques.

Experimental procedure
Microwave synthesis of cubic CoFe2O4 was carried out using metal oxalate precursors
employing microwave route. Urea is used as fuel for complete conversion of iron and
cobalt oxalate in to Cobalt ferrite particles. Cobalt oxalate, ferrous ammonium
sulphate, oxalic acid and urea used were AR grade. The process flow chart is shown
in fig [1].

Preparation of Cobalt ferrite


In our earlier work [6], we have reported preparation of cobalt ferrite using
microwave route. In brief, metal salts were dissolved in oxalic acid and both are
stirred. Then, known quantities of these two oxalates and urea (as fuel) are ignited in a
microwave oven for complete conversion of metal oxalates in to crystalline cobalt
ferrite particles.

Preparation of pellet
The powders were crushed and ground finally. A few drops of PVA binder was added
to the powder and passed in to pellets of 1cm diameter and 1cm thickness for
conductivity and impedance measurements by applying a pressure of 70Mpa. The
binder burn off was carried out by a slow heating rate and soaking time being an hour.
Magnetic and Transport Properties of Cobalt Ferrite 127

Instrumentation
The cobalt ferrite is pressed in the form of circular pellets of 1cm diameter and 1cm
thickness. The dc conductivity measurements of cobalt ferrite are made using the
conducting silver paste as electrodes on both sides. D c conductivity measurements
and resistivity measurements, their variation with temperatures were carried out with
Keithly 2010 electrometer using two probe method. The magnetic characterization of
the particles was done using Vibrating sample magnetometer (VSM). The impedance
spectroscopy was carried out to find the variation of real and imaginary part of
impedance with temperature at different frequencies using HP-4192 Impedance
analyzer.

Figure 1: Synthesis scheme of Cobalt ferrite.

Magnetic properties of Cobalt ferrite


Cobalt ferrite is an important material not only for its moderate magnetic properties
but also for its catalytic properties which depends on the textural and morphological
characteristics. This kind of ferrite is a spinel but it exhibits a large coercivity
differently from the rest of the spinel ferrites [7].
128 A.M. Bhavikatti et al

Ferromagnetic materials include iron, nickel and cobalt and compounds


containing these elements. In the absence of applied magnetic field, each atom has
very strong magnetic dipole moments due to uncompensated electron spins. Regions
of many atoms with aligned dipole moments called domains form. In the absence of
applied magnetic field, the domains are randomly oriented so that, the net
macroscopic magnetization is zero [8]. Here, the strong spin interactions will cause
the atomic moments to align parallel to each other. These materials have a very large
and positive magnetic susceptibility. Note that, ferromagnetism will occur below a
critical temperature called the Curie temperature TC. At temperature above TC, the
material becomes paramagnetic.
Fig (2) shows the M-H loops obtained using vibrating sample magnetometer
(VSM) at room temperature with maximum applied field up to 108KOe. The
hysteresis loops measurements were restricted on the dependence of temperature. The
shapes of the hysteresis loops depend on the temperature. The saturation
magnetization (Ms) obtained at room temperature was found to be 71.40 Gauss and
remanent magnetization (Mr) was 39.27 Gauss. The obtained hysteresis loop is very
narrow but not rounded shape with a high coercivity( 272.73 Oe) indicating the
formation of a hard ferrite. Fig( 2) demonstrates that, the synthesized ferrite is a not
very hard magnetic material, because of its small coercive field HC=272.73 Oe.
Furthermore, its remanent magnetization of 39.27 Gauss is quite low in comparison to
that of hard magnetic materials..The internal area of hysteresis loop represents the
capability of magnetic energy storage of the material.

Figure 2: Hysteresis curve of Cobalt ferrite at room temperature.


Magnetic and Transport Properties of Cobalt Ferrite 129

Transport properties of cobalt ferrite


Resistivity
In general, the electrical properties of the ferrite materials depend upon chemical
composition, preparing process, and microstructure. The relationship between
resistivity and temperature could be expressed as
ρ= ρ0eE ρ /KT ------------
Where ρ= is the resistivity at temperature T
ρ0= is the pre –exponential constant which equals the resistivity at infinitely high
temperature
k= is the Boltzman’s constant
E ρ= is the activation energy
Ensuring the semiconductor behavior of ferrites, the dc resistivity decreases with
the rise in temperature.[9]

Resistivity at room temperature


The DC resistance was measured with a low noise multimeter (Keithley 2010) using
two probe method. It is observed that, dc resistivity decreases with rise in temperature
in the low temperature region ensuring semiconducting behavior as per previous
studies.
Fig(3) shows the variation of dc resistivity with temperature. High dc resistivity
of~ 9.75×1010 ohms cm is obtained at room temperature and decreases with increase
in temperature. The resistivity of the sample decreases with increase in temperature
according to Arrhenious equation. Increase in temperature of the sample will help the
trapped charges to be liberated and participate in the conduction process, with the
result of decreasing the resistivity[10] The resistivity first decreases to a minimum at
750C and after that increases from 1150C reaching a maximum of 1.3×1010 ohm cm at
4000C. This increase in the resistivity may be due to hindrance of the hopping
mechanism between Fe2+ and Fe3+[11]. The rapid increase in resistivity may also be
due to the increase in the porosity of the material as reported earlier[12]. The dc
characteristics show semiconducting behavior at low temperature and metallic
behavior at high temperature as reported earlier by( KD Mandal et al 2003). From
literature it is observed that, the general practice in the preparation of high resistivity
ferrites is to avoid excess iron in the lattice and to add small quantities of manganese
or cobalt[13]Hudson[14] has shown that the dielectric losses in ferrites are generally
reflected in the resistivity measurements, a material with low resistivity exhibits high
dielectric loss and vice-versa. A similar inverse trend is reported in Li-cd[15] and Li-
Mg-Zn ferrites[16].
130 A.M. Bhavikatti et al

10 -8
1.4x10 4.0x10
Conductivity
10 -8
1.2x10 3.5x10

10 -8
1.0x10 3.0x10

9 -8
8.0x10 2.5x10

Conductivity
Resistivity

9 -8
6.0x10 2.0x10

9 -8
4.0x10 1.5x10

9 -8
2.0x10 1.0x10

-9
0.0 5.0x10

9
-2.0x10 0.0
0 50 100 150 200 250 300 350 400 450
0
Temprature (C )

Figure 3: Variation of resistivity and Conductivity with temperature.

DC Conductivity
Generally, the total conductivity is the summation of the band and hopping parts as
per equation
σtot= σ0(T)+σ(ωt)-------------
The first term is dc conductivity due to the band conduction, it is frequency
independent. The second term is the pure ac conductivity due to the hopping
processes at the octahedral site [4].
Fig (3) shows the variation of dc conductivity Vs temperature for the cobalt
ferrite. This plot shows that dc conductivity increases from room temperature to 1250
C. The conductivity increases with temperature as expected from the semiconductor
behavior of spinel ferrites. So, conductivity peak (3.75× 10-8 S/cm) may be observed
at 1250 C. After that it starts decreasing up to 2000C. From 2000 C temperatures
onwards there is a small decrease in dc conductivity up to 2500 C and after that it
remained constant up to 4000 C. In cobalt ferrites, the hopping of both electrons holes
contribute to the electrical conductivity. The decrease in the number of iron ions in
octahedral site will result in the decrease of Fe2+↔ Fe3+ pairs contributing to the
decrease in conductivity at high temperature [17].

Complex Impedance Spectroscopy


Complex impedance data were obtained at various temperatures in the frequency
range 1 KHz-1MHz using HP-4192 Impedance analyzer. 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 us data having both resistive (real part) and reactive (imaginary)
components [4].
Magnetic and Transport Properties of Cobalt Ferrite 131

Variation of real part of impedance Z΄ as a function of temperature at different


frequencies
From Fig (4), impedance maximum of 3.7× 105Ohms is observed at around 4000 C at
1KHz.Impedance relaxation is observed at high temperatures only at low frequencies
(<10 KHz). The reason for this behavior at high temperatures may be due to the
space- charge relaxation at low frequencies, which is related to the charge carriers in
association with the oxygen vacancies. As the frequency is further increased, Z΄
decreases reaching the lowest value (230 Ohms) at 1 MHz frequency [18].It is
observed that the values of Z΄ decreased with increasing frequency indicating an
increase in ac conductivity with frequency [4].

5
4.0x10 Z' 50000 Z'
5
3.5x10

5 40000
3.0x10

5
2.5x10
30000
5
Z'

Z'

2.0x10

5
1.5x10 20000

5
1.0x10
10000
4
5.0x10

0.0 0
0 100 200 300 400 500 600 700 0 100 200 300 400 500 600 700
0 0
Temprature C Temprature C

4
1.2x10
Z' 250
4
Z'
1.0x10

200
3
8.0x10

150
3
6.0x10
Z'
Z'

3
100
4.0x10

3 50
2.0x10

0.0 0

0 100 200 300 400 500 600 700 0 100 200 300 400 500 600 700
0 0
Temprature C Temerature C

Figure 4: Variation of real part of impedance Z΄ as a function of temperature at


different frequencies (a) 1 KHz (b) 10 KHz (c) 100KHz (d) 1MHz.

Variation of imaginary part of impedance Z˝ as a function of temperature at


different frequencies
From Fig (5 ) the variation of imaginary part of impedance Z˝ as a function of
temperature at different frequencies is observed. Z˝ maximum of 1.1 ×106 Ohms is
observed at low frequency of 1 KHz and at high temperature of around 4200 C.As the
132 A.M. Bhavikatti et al

frequency is further increased, Z˝ decreases reaching a minimum small value of


1360K Ohms at 1MHz.These peaks are frequency dependent and are seen shifting
towards the higher temperature side with increase of frequency. The magnitude of Z˝
maxima decrease with frequency indicates increasing loss in the resistive property of
the sample. This behavior of impedance pattern arises possibly due to the presence of
space charge in the sample [18].

5
6 Z'' 1.4x10
1.2x10
Z''
5
6
1.2x10
1.0x10

5
5
1.0x10
8.0x10
4
8.0x10
5
6.0x10
Z''

Z''
4
6.0x10
5
4.0x10
4
4.0x10
5
2.0x10
4
2.0x10
0.0

0.0
0 100 200 300 400 500 600 700
0 100 200 300 400 500 600 700
0
Temprature C 0
Temprature C

1380
1.4x10
4 Z''
Z''
1360
4
1.2x10
1340

1.0x10
4 1320
Z''

1300
Z''

3
8.0x10
1280

3
6.0x10
1260

4.0x10
3 1240

1220
0 100 200 300 400 500 600 700
0 100 200 300 400 500 600 700
0
Temprature C 0
Temperature C

Figure 5: Variation of imaginary part of impedance Z as a function of temperature at


different frequencies (a) 1 KHz (b) 10 KHz (c) 100KHz (d) 1MH.

Conclusions
We have studied the fabrication, magnetic and transport properties of cobal ferrite
synthesized by the microwave route. Magnetic characterization was done using VSM
with maximum applied field of 108KOe.The high coercivity obtained (272.73 Oe)
indicates the formation of a hard magnetic material.. The resistivity obtained here is
very high i.e, 9.75× 1010 ohms cm. High value of dc resistivity makes this ferrite
suitable for the high frequency applications where eddy current losses become
appreciable. Temperature dependent dc resistivity decreases with an increase in
temperature ensuring the normal behavior of semiconducting materials. But the
Magnetic and Transport Properties of Cobalt Ferrite 133

conductivity obtained is very low i.e, 3.75×10 -8 S/cm. The impedance spectroscopy
technique was employed to investigate the variation of real and imaginary part of
impedances with different temperatures at four different frequencies. Z΄ maximum
was observed at 1KHz( i.e 3.7× 105 Ohms).But Z΄ minimum was observed at 1MHz(
i.e 230 Ohms)Similarly, Z maximum was observed at 1KHz(i.e 1.1× 106 Ohms) and
Z minimum was observed at 1 MHz (i.e 1360 Ohms).

Acknowledgements
We are indebted to Dr.Harshavardhan of IICT, Hyderabad for helping in magnetic
measurements. We wish to thank Dr.B.B.Lal, Principal, REC Bhalki for his constant
encouragement. Thanks are due to Sri.Shahi.M.Lohar of REC Bhalki for his help
while preparing the manuscript.

Biographies
A M Bhavikatti received a degree in Electronics & communication in 1985, has
completed ME in power electronics in 1991 and is a research scholar in Electronic
materials. Till date, he has more than 20 publications in International and National
journals and Conferences. Presently he is a Professor and Head of Electronics and
Communication Engineering Dept at Rural Engineering College, Bhalki, Karnataka state
Dr.Subhash.S.Kulkarni completed BE in Electronics and Communication Engg in
1988 and Masters program in Electronic Design & Technology from Indian Institute
of Science, Bangalore in 1995.He was awarded PhD from IIT, Kharagpur in 2002 in
the area Geometric Deformable Models for Image Segmentation. Presently he is
working as Principal in Jayaprakash Narayan College of Engineering, Mahabubnagar,
Andhra Pradesh. Till date he has more than 30 publications in International &
National journals and Conferences and is guiding 8 research scholars.
Dr.Arunkumar.Lagashetty completed M.Sc in 2000 and M.phil in 2001 from
Gulbarga University, Gulbarga. He was awarded PhD from Gulbarga University in
2004 in the area of Physical chemistry. He was a Junior Research fellow for an UGC
Project. Till date he has more than 28 publications in International and National
journals and more than 30 publications in conferences. Presently, he is working as a
Head of department of Chemistry at Appa Institute of Engineering and Technology,
Gulbarga, Karnataka state.

References

[1] B.K.Bammannavar ,L.R.Naik ,R.B.Pujar, B.K.Chougale, ‘’Influence of Time


and Temperature on Resistivity and Microstructure of Cu xCo1-x Fe2O4 Mixed
ferrites’ ’Progress in Electromagnetic Research letters, Vol4, 2008, pp121-123
[2] I.C. Nlebedim, N Ranvah, P.I. Williams, Y Melikhov, F Anayi, J.E. Snyder,
A.J. Moses, D.C. Jiles - Influence of vacuum sintering on microstructure and
134 A.M. Bhavikatti et al

magnetic properties of magnetostrictive cobalt ferrite, Journal of Magnetism


and Magnetic Materials ,321, 2009, pp2528–2532
[3] Xiaofei Cao, Kangning Sun, Chang Sun, Liang Leng ‘’the study on
microstructure and microwave-absorbing properties of lithium zinc ferrites
doped with magnesium and copper’’ Journal of Magnetism and Magnetic
Materials, 321, 2009, pp2896–2901
[4] A.M.M.Farea,S.Kumar, K.M.Batoo, A.Yousef, C.G.Lee,Alimuddin, “
Structure and electrical properties of Co 0.5Cd xFe 2.5-xO4 ferrites” Journal of
Alloys and Compounds, 464, pp 361-369, 2008
[5] A.M.Bhavikatti, Dr.Subhash.Kulkarni, Dr.Arun.Lagashetty, “Evaluation of
a.c. conductivity and dielectric behavior of Cobalt ferrite (CoFe2O4)”, at
International Conference on HI-Tech Materials (ICHTM-09) held at IIT
,Kharagpur, on Feb 11 – 13th 2009.
[6] Arunkumar.Lagashetty, V,Havanoor, S.Basavaraj, S.D.Balaji,
R.Venkataraman, Sci & Tech.Adv.Mater,8, 484, 2007
[7] J.B.Silva ,W.D.Brito, N.D.S.Mohallem, ‘’Influence of heat treatment on cobalt
ferrite ceramic powders’’Intl.Jrl.Materials Science and Engineering, B 112,
2004,pp182
[8] James.T.Aberle, 2002
[9] L.Li, Z.Lan,Z.Yu,Ke.Sum, Z.Xu,and H.Ji ‘’Microstructure, Electrical, and
Magnetic Properties of ZrO2 Added MnZn Ferrites’’IEEE transactions on
magnetics, Vol 44, No A9,Sept 2008
[10] J.Chand, M.Singh, ‘’Electric and Dielectric properties of MgGd0.1Fe1.9O4
ferrite’’ Accepted Manuscript, June 2009, Journal of Alloys and Compounds,
[11] M.U.Rana, M.U.Islam, U.Qadri, S.B.Niazi, ‘’Fabrication & Characterization
of W-type Hexa-ferrites’’, Journal of Research(Science), Bahauddin Zakariya
University,Vol 17,No 4, Oct 2006, pp 222
[12] A.A.Sattar, H.M.El-Sayed, W.R.Agami and A.A.Ghani, ‘’ Magnetic
properties and Electrical Resistivity of Zr4+ Substituted Li-Zn Ferrite,
American Journal of Applied Sciences 4(2); pp 93, 2007
[13] P.A.Shaikh, R.C.Kamble, A.V.Rao, Y.D.Kolekar, ‘’Studies on structural and
electrical properties of Co1-x Nix Fe1.9Mn0.1O4 ferrite’ Intl.Journal of Alloys
and compounds, 482(2009), pp277
[14] A.S.Hudson, Marconi Rev. 37(1968), 43
[15] K.D.Radha, Ravinder, Indian J. Pure. Appl.Phys, 33(1995), 74
[16] A.M.Shaikh, S.S.Bellad, B.K.Chougle, J.Magn, Magn.Mater, 136(1999),384
[17] A.Narayanasamy,N .Sivakumar, ‘’ Influence of mechanical milling and
thermal annealing on electrical and magnetic properties of nanostructured Ni-
Zn cobalt ferrites’’,Bull Mater Sci.,Vol 31, No 3, June 2008,pp 375-376
[18] R.Rizwana, T.Radha Krishna,A.R.James P.Sarah, “ Impedance spectroscopy
of Na and Nd doped strontium bismuth titanate’’, Cryst.Res.Technol,42, No7,
699-706, 2007

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