Science of Sintering, 50 (2018) 217-223

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doi:https://doi.org/10.2298/SOS1802217G

UDK 549.73; 53.086

Inflence of Cadmium Substitution in Magnesium Ferrites on
Structral and Mechanical Properties

Satyappa Laxman Galagali1, Rahul Annasaheb Patil2, Raju Basappa

Adaki2, Chidanandayya Shivayya Hiremath2, Shridhar Narasinhmurthy
Mathad3*), Rangappa Basappa Pujar2
1
Department of Physics, R. L. Sciencce Institute, Belagavi.India
2
P. G. Studies in Physics, P. C. Jabin Science College, Hubballi, Karnataka, India
3
Department of Physics K. L. E. Institute of technology, Hubballi 580030, India.

Abstract:
This work had the objective of studying the detailed structural properties cadmium
doped of Magnesium ferrite (MgFe2O4) obtained, which was prepared by low-cost solid-state
Method and characterized by XRD and SEM techniques. The X-ray analysis confirms the
formation of single phase cubic spinel structure. The crystallite size, Texture coefficient
[TC(hkl)], dislocation density (ρD), hopping lengths and mechanical properties are also
reported.SEM images reveals agglomerated non-uniform grains with grain size varies from
0.7031 µm to 1.1158 µm.
Keywords: Magnesium-cadmium ferrites; XRD; Texture coefficients; Dislocation density;
Strain; SEM.

1. Introduction

Ferrites are the well-known ferrimagnetic materials with chemical compound formula
of AB2O4 (where A and B represent metal cations). Ferrites are widely used in high-frequency
applications, because an alternating current (AC) field does not induce undesirable eddy
currents in an insulating material [1]. Electrical and magnetic properties of ferrites can be
used for distinct applications in information storage systems, sensors, telecommunication
devices, magnetic refrigeration, catalysis, magnetic drug delivery, antenna rods, permanent
magnets, recording heads, magnetic liquids, as a microwave absorber [1-5]. MgFe2O4 based
materials are found to be much interest due to applications in microwave devices, computer
memory chips and high density recording media [6], humidity sensor [7], an inorganic
pigment [8], as semiconductor[9]. Ferrites can be synthesized by various chemical and
physical approaches are such as high-energy ball milling [10-11], sol-gel [12], co-precipitate
[13], solid state method [14-15] and sucrose precursor [16].
The objective of work aims to synthesize the cadmium doped MgFe2O4 synthesized
by solid-state method and study structural studies characterized by XRD and SEM technique.
We report the influence of cadmium doping in lattice parameter, crystallite-size, morphology,
dislocation density (ρD), mechanical properties (strain), and Hopping length {tetrahedral site
(LA) and octahedral site (LB)} of Mg-ferrite also reported.
B

_____________________________
*)
Corresponding author: [email protected]
218 S. L. Galagali et al. /Science of Sintering, 50 (2018) 217-223
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2. Experimental

Analytical grade Ferric-oxide (Fe2O3), Magnesium-oxide (MgO), Cadmium-oxide

(CdO) chemicals were used to synthesis the Mg1-x Cdx Fe2O4 (with X=0.2,0.4,0.6 and 0.8) by
standard Solid-state method (shown in Fig.1). The compositional weights of powders were
mixed physically and blended in agate mortar in acetone medium. All the samples were pre-
sintered at 800 °C for 10 hours keeping them in separate alumina crucibles, in a muffle
furnace. The pre sintered powders were subjected to hard milling process in acetone medium
for few hours. Then the pellets were subjected to final sintering by keeping them on a alumina
plate separately at 1000 °C for 15 hours and furnace cooled at the rate of about 80 °C per
hour.Structural characterization of the ferrite powders was carried out on Philips
Diffractometer (XRD), (with Cu-Kα radiation, wavelength, λ= 1.54 Å). The scanning
electron micrographs of all the samples were taken on JEOL JSM 6360 SEM
machine.

Fig.1. Schematic over-view of Magnetism- Cadmium ferrite.

3. Results and Discussion

3.1. X-Ray Diffraction Studies and Mechanical properties

To evaluate the crystal structure of Mg1-xCdxFe2O4 (with X=0.2, 0.4, 0.6 and 0.8)
analysis were carried out and the XRD images of the samples are presented in Fig. 2.

Fig.2. XRD pattern of ferrite samples.

 S. L. Galagali et al./Science of Sintering, 50 (2018) 217-223 219
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The diffraction pattern analysis by using (220), (311), (400), (422), (440), and (110) reflection
planes confirms the cubic spinel structures (JCPDC card #00-001-0114). Miller indices (HKL)
and lattice parameter (a) were calculated and tabulated in Tab. I:

Tab. I Lattice planes, Glancing angle, Interplanar spacing and Lattice constant.
X=0.2 X=0.4 X=0.6 X=0.8
Peak hkl dobs dcal hkl dobs dcal hkl dobs dcal hkl dobs dcal
no. ( Å) ( Å) ( Å) ( Å) ( Å) ( Å) ( Å) ( Å)
1 220 3.01203 3.01435 220 3.03934 3.04172 220 3.06359 3.06598 220 3.08883 3.09124
2 311 2.56381 2.56581 311 2.58829 2.59031 311 2.60855 2.61059 311 2.62934 2.63140
3 400 2.12459 2.12625 400 2.14367 2.14534 422 1.76115 1.76253 422 1.77448 1.77587
4 422 1.73063 1.73198 422 1.74669 1.74805 511 1.65986 1.66115 511 1.67189 1.67319
5 511 1.63169 1.63297 511 1.64607 1.64736 440 1.52388 1.52507 440 1.53488 1.53608
6 440 1.49801 1.49918 440 1.51153 1.51271 620 1.36233 1.36340 620 1.37225 1.37331
7 533 1.29161 1.29262 620 1.35125 1.02622 533 1.31353 1.31455 533 1.32317 1.32420
8 533 1.30327 1.30429

a
d= ……… (1)
(h + k + l 2 )1/ 2
2 2

The lattice parameter (a) found increases from 8.526 to 8.7499 Å with increase in cadmium
doping (x) in accordance with Vegard’s law (Shown in Fig. 3).

Fig. 3.Variation of lattice constant, Volume with cadmium composition (x).

This monotonic variation of lattice parameter with Cadmium content is attributed to the ionic
radii of Mg+2 ions, Cd+2 ion and Fe3+ ion. The radius of Cd (1.03 Å) ion is greater than that of
Mg (0.78 Å) and Fe (0.67 Å) ions. As Cd content increases the amount of Mg and Fe
decreases. As a result lattice parameter increases with Cd content. An increase in x results in
stretches of the cubic unit cell. Such a behavior can be described by using the 2nd order
polynomial (with R2 = 0.999, Regration coefficient)

a = 0.004x2 + 0.365x + 8.453……… (1)

Crystallite size (D) is a measure of the size of a coherently diffracting domain. The averaged
grain size estimation can also be estimated by measuring the peak width at half length of full
maxima. The average crystallite size for the different compositions were calculated by Debye-
 220 S. L. Galagali et al. /Science of Sintering, 50 (2018) 217-223
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Sherrer’s formula [16].

0.9 ⋅ λ
D=
β . cos θ (2)
A dislocation is a crystallographic defect (irregularity) within a crystal structure, which
strongly influences the properties of materials. The dislocation density (ρD) is a measure of
the number of dislocations in a unit volume of a crystalline material. Dislocations are one-
dimensional crystalline defects marking the boundary between a slipped and an unslipped
region of a material [18-19]. This defect distorts the regular atomic array of a perfect crystal.
The amount of the defects in the as deposited film was resolved by evaluating the dislocation
density [16] calculated by,
Dislocation density (ρD) =1/D2, ………… (3)
micro-strain (ε) =βcosθ/4 (4)
where ρD is dislocation density and D is crystallite size.
The distance between magnetic ions (hopping length) in A site (Tetrahedral) and B
site (Octahedral) were calculated by using the following relations [20-21] {(LA and LB)} B

a× 3
LA = ……………… (5)
4
a× 2
LB = ……………… (6)
4
where a is lattice constant.
The lattice parameter (a=b=c), cell volume (V) ,crystallite size (D), Dislocation density (ρD)
micro strain, and Hopping lengths {tetrahedral site (LA) and octahedral site (LB)} of ferrite B

samples are tabulated in Tab. II.

Tab. II Lattice constant, Strain, Volume, Crystallite size, Dislocation-Density and Hopping
lengths of Mg-ferrite.
Hoppling Average Dislocation
Lattice lengths (Å) Crystallite grain density
Sample constant Volume Strain Size(D) diameter Porosity (ρD)
(Å) (Å)3 (ε) LA LBB nm (µm) %
Ga x1014
x=0.2 8.526 619.78 0.04759 3.692 3.014 41.85 0.703 38 5.71
x=0.4 8.6033 636.79 0.04452 3.725 3.041 44.63 0.838 33 5.02
x=0.6 8.6719 652.13 0.04934 3.755 3.066 48.06 0.770 21 4.33
x=0.8 8.7499 669.90 0.04605 3.789 3.094 56.39 1.116 23 3.15

The variation of strain and hopping lengths with cadmium content is shown in Fig. 4.

Fig.4. Variation of hopping lengths, strain with composition (x).

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3.3. Surface morphology Studies

The grain size of the sample was calculated by linear intercept method [22].The
average grain diameter (Ga) was calculated by enumerating the number of grain boundaries
intercepted by a measured length of a random straight line drawn on micrographs.
L
Ga = 1.5 (7)
MN
The scanning electron microscopy studies were undertaken for the samples images
are shown in Fig. 5.

X=0.2 X=0.4

X=0.6 X=0.8

Fig. 5. SEM patterns of Mg-Cd ferrite (X = 0.2,0.4,0.6 and 0.8).

It is evident from the SEM micrographs that, sample seems to be non-uniform with somewhat
agglomeration in the synthesized samples which is unavoidable with size less than 1 μm.
Depending upon the heat treatment the grain size varies from 0.7031 μm to 1.1158 μm. The
maximum grain size is found for X = 0.8, due to unequal diffusion rates porosity develops at
the base of the neck and the neck growth is the consequence of migration of vacancies from
pore or neck to the neck boundary. The mechanism of pore growth along with grain growth
results in the characteristic microstructure of ferrites in which residual porosity appears in
intra granular space. This is closely indicated in the present samples. As cadmium content
increases average grain diameter increases and reaches maximum value at X = 0.8. The
increase in diameter is due to presence of certain amount of metal ion vacancies caused by
oxidation of suiTab. doping. Therefore it can be concluded that diameter of the grain
increases with decrease in porosity and under specific conditions exaggerated grain growth
may occur.
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4. Conclusions

Polycrystalline Mg1-xCdxFe2O4 (with X=0.2, 0.4, 0.6 and 0.8) ferrites has been
successfully synthesized by solid-state method. The X-ray diffraction results for the samples
showed the formation of single phase cubic spinel structure. The lattice parameter (a) found
increases from 8.526 to 8.7499 Å with increase in cadmium doping (x) in accordance with
Vegard’s law. We have also discussed morphology, dislocation density (ρD), mechanical
properties (strain), Hopping length {tetrahedral site (LA) and octahedral site (LB)} of Mg-Cd
B

ferrite is also reported.

Acknowledgements

Dr. S. N. Mathad is very much thankful to Prof. Gloria Albert, Department of

English, for precious English critique proofreading.

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Садржај: У овом раду детаљно су проучавана структурна својства магнезијум

ферита допираног кадмијумом, који је припремљен јефтином методом реакција у
чврстој фази и карактерисаног техникама рендгенске дифракције и скенирајуће
електронске микроскопије. Рендген је показао формирање једне фазе кубичне спинелне
структуре. Такође су приказане величина кристалита, коефицијент текстуре,
густина дислокација и механичка својства. Микрографије указују на агломерисана не-
униформна зрна, са величином зрна од 0,7031 µm до 1,1158 µm.
Кључне речи: магнезијум-кадмијум ферит, рендгенска дифракција, коефицијент
текстуре, густина дислокација, микронапрезање, скенирајућа електронска
микроскопија.

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