ISSN 1061-3862, International Journal of Self-Propagating High-Temperature Synthesis, 2017, Vol. 26, No. 1, pp. 7579.

Allerton Press, Inc., 2017.

Structural and Mechanical Properties of Nanograined Magnesium

Ferrite Produced by Oxalate Coprecipitation Method1
R. M. Shedama, A. B. Gadkaria, S. N. Mathadb,*, and M. R. Shedamc
a
Department of Physics, GKG College, Kolhapur, 416012 India
b
K.L.E. Institute of Technology, Hubli, 580030 India
c
The New College, Kolhapur, 416012 India
*e-mail: physicssiddu@gmail.com
Received August 12, 2016

AbstractMagnesium ferrite (MgFe2O4) was prepared by simple low-cost oxalate coprecipitation method
and characterized by XRD and SEM. The X-ray analysis confirmed the formation of a single-phase cubic
spinel structure. The product revealed a non-uniform morphology and some certain extent of agglomeration.
Crystallite size, texture coefficient, dislocation density, hopping length, and mechanical properties of the
product are also reported.

Keywords: oxalate co-precipitation method, sintering, magnesium ferrite MgFe2O4 texture coefficients, dis-
location density, strain
DOI: 10.3103/S1061386217010113

1. INTRODUCTION properties (strain), and hopping length (for tetrahe-

Ferrites of general formula AB2O4, where A and B
stand for metal cations, including iron. Ferrites are the
well-known ferrimagnetic materials that consist
mainly of ferrimagnetic oxides and, therefore, are
electroinsulating. Ferrites are widely used in high-fre-
quency applications, because alternating electric field
does not induce undesirable eddy currents in material
[1, 2]. Nano ferrites have been investigated because
their electrical and magnetic properties are attractive
for application in information storage systems, sen-
sors, telecommunication devices, magnetic refrigera-
tion, catalysis, magnetic drug delivery, antenna rods,
permanent magnets, recording heads, magnetic liq-
uids, and as a microwave absorber [38]. MgFe2O4-
based materials have found much interest due to their
applications in microwave devices, computer memory
chips and high-density recording media [9], humidity
sensor [10], as inorganic pigment [11], and as semi-
conductor [12]. MgFe2O4 nanoparticles have been
synthesized by various physicochemical methods such
as high-energy ball milling [13], solgel technique
[14], micellar reactions [15], coprecipitation [16, 17],
and combustion synthesis [18].
This work aimed at the synthesis of MgFe2O4 by
oxalate coprecipitatation method and its characteriza-
tion by XRD and SEM, with special emphasis of the
morphology, dislocation density (D), mechanical
1 The article is published in the original.
dral LA and octahedral site LB) of synthesized magne-
sium ferrite.
2. EXPERIMENTAL
Starting materials of analytical grade MgSO4
7H2O (99.99% pure, Sd-fine) and FeSO4 7H2O
(99.5%, Thomas Baker) were used to synthesize
MgFe2O4 by standard oxalate coprecipitation method
as illustrated in Fig. 1. The final powdered product was
sieved, dried, and sintered first at 400C for 5 h and
then at 500C for 4 h. Thus prepared samples were
characterized by XRD (Philips diffractometer, Cu-K
radiation, = 1.54 ) and SEM (JEOL JSM 6360
apparatus).
3. RESULTS AND DISCUSSION
3.1. X-Ray Diffraction and Mechanical Properties
Figure 2 shows the XRD pattern of synthesized
magnesium ferrite. The diffraction pattern analysis by
using (220), (311), (400), (422), (440), and (110)
reflection planes confirmed the formation of a cubic
spinel structure. The peaks positions and relative
intensities match the tabulated values for MgFe2O4
(JCPDC card #00-001-0114). The synthesized mate-
rial belongs to space group Fd3m cubic spinel structure
with lattice constant a = 8.31826 . Miller indices

75
76 SHEDAM et al.

Intensity
1400

1300
+
(311)
1200

1100 (422) (440)

Cationic Solution (220) (400) (511)
Anionic Solution
1000

900
20 30 40 50 60 70 5 m
5.000
Angle (2theta)

XRD SEM

Furnace

Magnetic stirrer

Dried Powder

Fig. 1. Schematic diagram of the process for preparation of MgFe2O4.

D = 0.9 .
(hkl) and lattice parameter (a) were calculated as
shown below and collected in Table 1. cos

d = a . A dislocation is a crystallographic defect (irregular-

(h 2 + k 2 + l 2 )1/2
Crystallite size D gives the size of a coherently
diffracting domain. The averaged grain size can also
be estimated by measuring the half width ah half
maximum of diffraction peaks. Average crystallite
size D was calculated by using the DebyeScherrer
formula [19]:
ity) within a crystal structure, which strongly influ-
ences the material properties. Dislocation density is
the number of dislocations in a unit volume of crystal-
line material. Dislocation density D and micro strain
were calculated from the formulas [1921]:
D = 1/D2, = cos /4.

The distance between magnetic ions (hopping

1400 length) in site A (tetrahedral) and site B (octahe-
dral) were calculated by using the following rela-
1300
tionships [22]:
I, counts

(311)
1200
LA = a 3 , LB = a 2
(440) 4 4
1100 (422)
(220) (400) (511) The results are presented in Table 2.
1000

900 3.2. Texture Analysis

20 30 40 50 60 70
2, deg Quantitative data concerning the preferential crys-
tal orientation is derived from texture coefficient TC
Fig. 2. XRD pattern of synthesized magnesium ferrite. defined as [19, 20]

INTERNATIONAL JOURNAL OF SELF-PROPAGATING HIGH-TEMPERATURE SYNTHESIS Vol. 26 No. 1 2017

 STRUCTURAL AND MECHANICAL PROPERTIES 77

2.5

2.0
TC(hkl)
1.5

TC
1.0

0.5

0
220 311 400 422 511 440
TC(hkl) 0.518 0.279 1.549 2.198 0.744 0.710

Fig. 3. Texture coefficient for hkl planes.

(a) 50 m (b) 1 m

Fig. 4. SEM images of synthesized magnesium ferrite at different magnification.

I ( hkl ) Preferential orientation of crystals (abundance of

grains) was found (see Fig. 3) to happen along the
I 0 ( hkl )
TC ( hkl ) = . (422) plane.
I ( hkl )
1

N N I 0 ( hkl )
3.3. Surface Morphology
The grain size was determined by using linear inter-
Table 1. Lattice planes, glancing angle, interplanar spac- cept technique [23]. The average grain diameter (Ga)
ing, and lattice constant was calculated by enumerating the number of grain
Planes (hkl) 2 d, a,
boundaries intercepted by a random straight line with
length L drawn on micrographs:
(220) 30.2 2.956955 8.363531
Ga = 1.5L/MN.
(311) 35.67 2.515045 8.341459
(400) 43.37 2.084689 8.338757 The SEM studies were carried out for the sample
(422) 53.89 1.699935 8.327946 shown in Fig. 4. The sample is seen to be non-uniform
(511) 57.54 1.600474 8.316309 with some unavoidable agglomerates with a size of
below 1 m. Agglomerated particles showed a broader
(440) 64.014 1.453334 8.221296 size distribution typical of mechanically activated
averaged a = 8.318216 nanoparticles. The agglomeration of particles takes

INTERNATIONAL JOURNAL OF SELF-PROPAGATING HIGH-TEMPERATURE SYNTHESIS Vol. 26 No. 1 2017

78 SHEDAM et al.
Table 2. Lattice constant, strain, volume, crystallite size, dislocation density, and hopping lengths of magnesium ferrite
a, V, 3 D, nm
8.31826 0.23115 575.5566 35.10
place because they experience a permanent magnetic
moment proportional to their volume [24, 25].
4. CONCLUSIONS
Synthesized nano-crystalline MgFe2O4 is single
phase and has a cubic spinel structure (lattice constant
a = 8.31826 , crystallite size D = 35.10 nm) with pref-
erential orientation of grains along the (422) plane.
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