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CHARACTERIZATION AND
ELECTROMAGNETIC STUDIES OF
NANO-SIZED BARIUM FERRITE
A.M.BHAVIKATTI*
Rural Engineering College, Bhalki585328, INDIA
DR.SUBHASH KULKARNI
Jaypraksh Narayan College of Engineering, Mahaboobnagar - 509001, INDIA
Abstract
The present article reports some of the interesting and important electromagnetic and impedance studies of
nanostructured barium ferrite. Here, the nano-sized barium ferrite (BaFe2O4) was synthesized by using
microwave route. The sample was characterized by X-ray diffraction, SEM and IR studies. Electrical
resistance(R) measurements of the sample revealed a very high resistivity and the results indicated a fall in
resistivity with the rise in temperature. The obtained dc conductivity is found to be very low of the order of 10-8
S/cm .The dc conductivity follows the Arrhenius law. The hysteresis M-H loops for this sample was traced
using the Vibrating Sample Magnetometer (VSM) to study the parameters coercivity (Hc), saturation
magnetization (Ms) , remanence (Mr) and squareness ratio( SQR). The complex impedance spectroscopy (CIS)
technique was used to study the electrical response of the nanostructured sample in a wide range of frequencies
(1 KHz to 1MHz) at different temperatures (07000 C).
Key words: Microwave synthesis, nano-sized barium ferrite, resistivity, conductivity, impedance studies
1. Introduction
Ferrites have continued to attract attention over the years. As magnetic materials, ferrites cannot be replaced by
any other magnetic material because they are relatively inexpensive, stable and have a wide range of
technological applications in transformer core, high quality filters, high and very high frequency circuits and
operating devices. The physical properties of ferrites are controlled by the preparation conditions, chemical
composition, sintering temperature and time, type and amount of substitutions [1].
In recent years, nanostructured materials have drawn outstanding attention due to the unique mechanical,
electrical, optical, and magnetic properties. The unique properties of nanostructured materials are due to their
changed electronic structure, close to that of an isolated atom or molecule. Among the nanoscale inorganic
materials, the magnetic metal oxides and their composites are of particular interest due to their exciting
applications in the areas of quantum computing, information storage media, magnetic resonance imaging,
sensors, refrigeration, electromagnetic wave absorption and modulation [2].
Recent studies have shown that, physical properties of nano particles are influenced significantly by the
processing techniques .Since crystalline size, distribution of particle sizes and inter particle spacing have the
greatest impact on magnetic particles, the ideal synthesis techniques must provide superior control over these
parameters .A variety of techniques have been employed for the synthesis of nano particles with definite shapes
and sizes [3].
Nanocrystalline barium ferrites are very interesting because of its chemical properties and thermal studies [4].
These materials are technologically important and have been used in many applications such as magnetic
recording media [5]. Recently, nanocrystalline magnetic materials have been receiving more and more attention
due to their novel material properties, which are significantly different from those of their bulk counterparts [6].
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Barium chloride, ferrous ammonium sulphate, oxalic acid and urea used were AR grade. Microwave method is
used for the synthesis of barium ferrite materials using urea as a fuel for the combustion reaction.
2.1.2 Preparation of pellet
The powders were crushed and ground finally to reduce it to small crystallites of uniform size. The mixture was
dried and a small amount of PVA binder was added to the powder .The resulting powders were pressed by
applying a pressure of 70Mpa in a stainless steel die to make pellets of 1cm diameter and 1cm thickness. The
pellet samples were well polished to remove any roughness present on the surface of pellets. .For the dielectric
and conductivity measurements; silver paint was applied on the polished surfaces of the pellets and air-dried to
have good ohmic contacts. The binder burn off was carried out by a slow heating rate and soaking time being an
hour.
2.1.3 Instrumentation
D c conductivity measurements were carried out with Keithly 2010 electrometer using two probe methods. The
resistance R was measured for different temperatures and the conductivity was calculated. The impedance
spectroscopy was carried out to find the variation of real and imaginary part of impedance with temperature at
different frequencies using HP-4192A Impedance analyzer.
2.1.2 Synthesis of nanosized BaFe2O4
Barium oxalate and iron oxalate precursors was prepared by dissolving equimolar quantities of barium chloride
and ferrous ammonium sulphate with oxalic acid and was stirred well in a separate beakers. The precipitates of
barium and iron oxalate obtained was filtered through sintered glass crucible and was washed with distilled
water till free from chloride ions and oxalic acid, finally with dry acetone and was then dried under vacuum.
The barium oxalate, iron oxalate and urea were mixed in weight ratio 1:1:5 and ground well in a pestle and
mortar. Resultant solid was placed in a crucible and ignited in microwave oven. The reaction was found to be
completed in about ten minutes at high power level and forms a brown crystalline BaFe2O4 material. On cooling
to room temperature no trace of carbon impurities was observed in the final residue of nano-sized barium ferrite.
2.2Characterization:
The powder X-ray diffraction pattern was obtained from GEOL JDX-8P or SEIMEN (Japan) X-ray
diffractometer using CuK radiation. The morphology of the maghemite sample was obtained from Leica
Cambridge-440 scanning electron microscopy. Bonding in as prepared nano-sized barium ferrite was obtained
from Perkin-Elmer FTIR spectrophotometer (Model-1000).
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Hkl
2obs
2lit
Iobs
402
28.240
28.235
60
212
28.435
28.428
100
610
32.720
32.716
50
020
33.269
33.266
30
802
43.610
43.604
10
422
44.172
44.164
23
Peak No.
1
2
3
4
5
6
7
8
9
10
3.2
Vibrational
Frequencies (cm-1|)
3100
1075
530
475
445
440
250
230
210
200
Figure-1 shows SEM image of as prepared barium ferrite sample. The particles are irregular in shape with
compact arrangement. In some particles flakes of agglomerates are also observed. Needle shaped particles
forms globular arrangement with self assembled blocks.
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3.3Infrared studies
The infrared study was performed aiming to ascertain the metal-oxygen and metal-metal bond in the prepared
ferrite sample. Table-2 gives the vibrational frequencies of the as synthesized BaFe2O4. The ferrite sample
shows the absorption in the region 3100, 1075, 530, 475, 445, 440, 250, 230, 210 and 200 cm-1. The peak at
3100 cm-1 corresponds to water of adsorption and the peak at1075cm-1 is due to the presence of some overtones.
The peaks at 530, 475, 445 and 440cm-1 correspond to the metal-oxygen vibrational modes of the spinel
compound [13]. The peaks at around 250, 230, 210 and 200cm-1 is observed is due to metal-metal (Ba-Fe)
vibration frequency range. This confirms the formation of BaFe2O4.
3.4 Resistivity
High dc resistivity of 1.75 109 Ohm-cm is obtained at room temperature and it decreases with increase of
temperature according to the Arrhenius equation. Increasing temperature leads to decrease in resistivity, which
is the normal behavior of semiconducting material. 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.
This decrease in resistivity could be related to the increase in the drift mobility of the thermally activated
electrons according to the hopping conduction mechanism and not to thermally creation of the charge carriers.
[14].
1 .8 0 E + 0 0 9
1 .6 0 E + 0 0 9
1 .4 0 E + 0 0 9
Resistivity
1 .2 0 E + 0 0 9
1 .0 0 E + 0 0 9
8 .0 0 E + 0 0 8
6 .0 0 E + 0 0 8
4 .0 0 E + 0 0 8
2 .0 0 E + 0 0 8
0 .0 0 E + 0 0 0
-2 .0 0 E + 0 0 8
-5 0
50
100
150
200
250
300
350
400
T e m p e ra tu re
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dc S/cm
DC conductivity increases with increasing temperature indicating a semiconducting behavior. The conductivity
obtained here is very less and the maximum conductivity obtained here is 410-8 S/cm at a temperature of 4000
C. The temperature variation of conductivity in this sample studied in the present work confirm to the Arrhenius
law [15] as shown in equation (2),
0 exp(- Edc /KT) -------(2)
Where, Edc activation energy required for the hopping process.
4.0x10
-8
3.0x10
-8
2.0x10
-8
1.0x10
-8
conductivity
0.0
50
100
150
200
250
300
350
400
450
Temperature C
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3.5x10
4x10
Z'
Z'
3.0x10
2.5x10
3x10
2.0x10
Z'
Z'
1.5x10
2x10
1.0x10
1x10
5
5.0x10
0.0
-5.0x10
(a)
100
200
300
400
500
600
700
(b)
Temperature C
100
200
300
400
500
600
700
Temperature C
500
Z'
2500
Z'
400
2000
300
Z'
Z'
1500
1000
500
200
100
100
200
300
400
500
600
700
100
200
300
400
500
600
700
Temperature C
(c)
(d)
Temperature C
Fig (5) Variation of real part of impedance (Z) with temperature at four different frequencies(a) 1KHz (b) 10KHz (c) 100KHz and (d)
1MHz
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3.0x10
1.8x10
(a)
2.5x10
Z''
Z''
(b)
1.6x10
1.4x10
6
2.0x10
1.2x10
1.0x10
Z''
Z''
1.5x10
8.0x10
1.0x10
6.0x10
4.0x10
5.0x10
2.0x10
0.0
0.0
100
200
300
400
500
600
-2.0x10
700
100
200
300
400
Temperature C
1.8x10
1.6x10
(d)
1600
1400
1200
1000
1.4x10
1.2x10
1.0x10
8.0x10
Z''
Z''
600
700
1800
Z''
(c)
500
Temperature C
6.0x10
Z''
800
600
4.0x10
400
2.0x10
200
0.0
-2.0x10
100
200
300
400
500
600
700
Temperature C
-200
0
100
200
300
400
500
600
700
Temerature C
Fig (6) Variation of imaginary part of impedance (Z) with temperature at four different frequencies(a) 1KHz (b) 10KHz (c) 100KHz and
(d) 1MHz
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Biographies of authors
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 35 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.
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