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ISSN 1061-3862, International Journal of Self-Propagating High-Temperature Synthesis, 2017, Vol. 26, No. 1, pp. 75–79.

© 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
Department of Physics, GKG College, Kolhapur, 416012 India
K.L.E. Institute of Technology, Hubli, 580030 India
The New College, Kolhapur, 416012 India
Received August 12, 2016

Abstract⎯Magnesium 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 dral LA and octahedral site LB) of synthesized magne-
stand for metal cations, including iron. Ferrites are the sium ferrite.
well-known ferrimagnetic materials that consist
mainly of ferrimagnetic oxides and, therefore, are 2. EXPERIMENTAL
electroinsulating. Ferrites are widely used in high-fre-
Starting materials of analytical grade – MgSO4 ⋅
quency applications, because alternating electric field
does not induce undesirable eddy currents in material 7H2O (99.99% pure, Sd-fine) and FeSO4 ⋅ 7H2O
[1, 2]. Nano ferrites have been investigated because (99.5%, Thomas Baker) – were used to synthesize
their electrical and magnetic properties are attractive MgFe2O4 by standard oxalate coprecipitation method
for application in information storage systems, sen- as illustrated in Fig. 1. The final powdered product was
sors, telecommunication devices, magnetic refrigera- sieved, dried, and sintered first at 400°C for 5 h and
tion, catalysis, magnetic drug delivery, antenna rods, then at 500°C for 4 h. Thus prepared samples were
permanent magnets, recording heads, magnetic liq- characterized by XRD (Philips diffractometer, Cu-Kα
uids, and as a microwave absorber [3–8]. MgFe2O4- radiation, λ = 1.54 Å) and SEM (JEOL JSM 6360
based materials have found much interest due to their apparatus).
applications in microwave devices, computer memory
chips and high-density recording media [9], humidity 3. RESULTS AND DISCUSSION
sensor [10], as inorganic pigment [11], and as semi-
conductor [12]. MgFe2O4 nanoparticles have been
synthesized by various physicochemical methods such 3.1. X-Ray Diffraction and Mechanical Properties
as high-energy ball milling [13], sol–gel technique Figure 2 shows the XRD pattern of synthesized
[14], micellar reactions [15], coprecipitation [16, 17], magnesium ferrite. The diffraction pattern analysis by
and combustion synthesis [18]. using (220), (311), (400), (422), (440), and (110)
This work aimed at the synthesis of MgFe2O4 by reflection planes confirmed the formation of a cubic
oxalate coprecipitatation method and its characteriza- spinel structure. The peaks positions and relative
tion by XRD and SEM, with special emphasis of the intensities match the tabulated values for MgFe2O4
morphology, dislocation density (ρD), mechanical (JCPDC card #00-001-0114). The synthesized mate-
rial belongs to space group Fd3m cubic spinel structure
1 The article is published in the original.
with lattice constant a = 8.31826 Å. Miller indices


26 No. 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. 2. Average crystallite ε were calculated from the formulas [19–21]: size D was calculated by using the Debye–Scherrer formula [19]: ρD = 1/D2. β cos θ d = a . (hkl) and lattice parameter (a) were calculated as shown below and collected in Table 1.76 SHEDAM et al. LB = a 2 (440) 4 4 1100 (422) (220) (400) (511) The results are presented in Table 2. Dislocation density ρD and micro strain maximum of diffraction peaks. counts (311) 1200 LA = a 3 . defined as [19. 1 2017 . The averaged grain size can also the number of dislocations in a unit volume of crystal- be estimated by measuring the half width ah half line material.000 Angle (2theta) XRD SEM Furnace Magnetic stirrer Dried Powder Fig. deg Quantitative data concerning the preferential crys- tal orientation is derived from texture coefficient TC Fig. Schematic diagram of the process for preparation of MgFe2O4. 20] INTERNATIONAL JOURNAL OF SELF-PROPAGATING HIGH-TEMPERATURE SYNTHESIS Vol.9λ . A dislocation is a crystallographic defect (irregular- (h 2 + k 2 + l 2 )1/2 ity) within a crystal structure. Texture Analysis 20 30 40 50 60 70 2θ.2. Intensity 1400 1300 + (311) 1200 1100 (422) (440) Cationic Solution (220) (400) (511) Anionic Solution 1000 900 20 30 40 50 60 70 5 μm ×5. D = 0. 1. ε = βcos θ/4. XRD pattern of synthesized magnesium ferrite. Dislocation density is diffracting domain. which strongly influ- Crystallite size D gives the size of a coherently ences the material properties. 1000 900 3.

014 1.5 TC 1.0 0. 1 2017 .341459 (400) 43.956955 8. (311) 35. Å a. Lattice planes.198 0.67 2.515045 8. 4. glancing angle. The sample is seen to be non-uniform (511) 57.3. Texture coefficient for hkl planes.316309 with some unavoidable agglomerates with a size of below 1 µm.363531 Ga = 1. interplanar spac.084689 8. Agglomerated particles showed a broader (440) 64. Surface Morphology The grain size was determined by using linear inter- Table 1. (a) 50 μm (b) 1 μm Fig.327946 shown in Fig.453334 8. 3. The agglomeration of particles takes INTERNATIONAL JOURNAL OF SELF-PROPAGATING HIGH-TEMPERATURE SYNTHESIS Vol. and lattice constant was calculated by enumerating the number of grain Planes (hkl) 2θ d. The average grain diameter (Ga) ing.279 1.5L/MN.338757 The SEM studies were carried out for the sample (422) 53.5 2. Å boundaries intercepted by a random straight line with length L drawn on micrographs: (220) 30.54 1.600474 8.710 Fig.549 2.37 2. cept technique [23]. 26 No.5 0 220 311 400 422 511 440 TC(hkl) 0.518 0. I ( hkl ) Preferential orientation of crystals (abundance of grains) was found (see Fig. (422) plane. I ( hkl ) 1 ∑ N N I 0 ( hkl ) 3.2 2. 4.699935 8.318216 nanoparticles.221296 size distribution typical of mechanically activated averaged a = 8.89 1. 3) to happen along the I 0 ( hkl ) TC ( hkl ) = .0 TC(hkl) 1. STRUCTURAL AND MECHANICAL PROPERTIES 77 2. SEM images of synthesized magnesium ferrite at different magnification.744 0.

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