Journal of Magnetism and Magnetic Materials 348 (2013) 140–145

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Journal of Magnetism and Magnetic Materials

journal homepage: www.elsevier.com/locate/jmmm

Effect of samarium substitution on structural and magnetic properties

of magnesium ferrite nanoparticles
Smitha Thankachan, Binu P. Jacob, Sheena Xavier, E.M. Mohammed n
Department of Physics, Maharaja's College, Ernakulam, Kerala 681011, India

art ic l e i nf o a b s t r a c t

Article history: Samarium doped magnesium ferrite was prepared (MgSmxFe2 xO4) by sol–gel method. X-ray diffraction
Received 11 December 2012 analysis reveals that the samples are single phasic with crystallite sizes in the 13–25 nm regime. Increase
Received in revised form in lattice parameter with doping concentration suggests the expansion in unit cell with Sm3 þ doping.
8 May 2013
Fourier Transform Infrared Spectrum shows substitution of Sm3 þ ions in octahedral B site. Transmission
Available online 12 August 2013
Electron Micrograph shows the spherical shape of nano-particles. Magnetic measurement shows a
Keywords: decrease in magnetization with doping which is explained using dependence on particle size.
Magnesium ferrite & 2013 Elsevier B.V. All rights reserved.
Sol–gel technique
Sm3 þ doping
Magnetic property

1. Introduction
The unusual magnetic, optical and electrical properties of metal-
oxide nanocrystals have attracted the attention of researchers in
recent years. Technological demand of high performance devices
has triggered the synthesis and research in nano-scale spinel
ferrites. Ferrites have diverged practical applications as high density
magnetic data storage, microwave absorbing materials, magnetic
resonance imaging contrast agents and targeted release of drugs.
Preparation conditions influence the cation distribution which in
turn reflects in the chemical and physical properties of ferrites to a
great extend [1]. Properties of ferrites are highly sensitive to the
substitution of different metal ions in its tetrahedral and octahedral
sites [2]. Magnesium ferrite is a partially inverse spinel with
interesting ferromagnetic property, since Mg2 þ is antiferrimagnetic.
Due to diffusibility of Mg2 þ ions, its distribution in the crystal
lattice site greatly depends on the heat treatment [3,4]. Several
methods are used for synthesizing nanosized spinel ferrites, such
as, co-precipitation, sol–gel, micro-emulsion, hydrothermal and
reverse micelle [5–7]. Good stoichiometric control and production
of ultrafine particles in nano-range at relatively low temperature
has attracted many researchers to choose sol–gel technique as
preparation method [7].
Magnesium ferrite is used as humidity sensor [6], catalyst [7]
and it also have magnetic and gas sensing applications [8,9].
Research on different rare earth substituted ferrites has revealed
to improve its properties [10–12]. But a study on physical, structural
and magnetic properties of samarium doped magnesium ferrite is
not yet reported. So in present work we try to investigate the effect
of samarium doping in structural and magnetic properties of
magnesium ferrite nano-particles. Substitution of large rare earth
ions in place of small iron ions will result in strain which induce
structural distortion and there by modify the properties of samples
in nano-regime [13]. But the percentage of rare earth doping should
be very small to avoid secondary phase formation, which is due to
the difficulty of large rare earth ion to enter into lattice sites.
Gadkari et al. has reported that 5% rare earth ion Y3 þ added
magnesium ferrites show secondary phase of YFeO3 orthoferrite
[32] and in Sm3 þ doped Mg–Cd ferrites they pointed out the
presence of SmFeO3 [19]. Bamzai et al. has reported formation of
DyFeO3phase in addition to cubic phase of MgFe2O4 when it is
doped with 0.5–3.5% of Dy3 þ ions [33]. But all these studies have
employed solid state reactions or high temperature above 800 1C for
preparation of samples. But in our present study we used sol–gel
process and the sintering temperature is at 500 1C so that we have
got pure Sm3 þ doped magnesium ferrite without any secondary
phase even with 15% of doping. But in neodymium doped magne-
sium ferrite a secondary phase was developed [10] in samples with
Nd concentration greater than 10% even if we employed the same
preparation conditions. Objective of our present study is to inves-
tigate the effect of samarium doping on structural and magnetic
properties magnesium ferrite nanoparticles.
2. Experimental
2.1. Synthesis of nanosized Sm3 þ doped magnesium ferrite

n
Corresponding author. Tel.: þ 91 9495315208; fax: þ 91 484 2363038. Sol–gel combustion method was used for preparation of
E-mail address: emmohammed_2005@yahoo.com (E.M. Mohammed). magnesium ferrite nanoparticles. AR grade magnesium nitrate,

0304-8853/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jmmm.2013.07.065
 S. Thankachan et al. / Journal of Magnetism and Magnetic Materials 348 (2013) 140–145
samarium nitrate and ferric nitrate were used as chemical pre-
cursors in ethylene glycol as solvent. Nitrates in the required
stoichiometric ratio were dissolved in minimum amount of ethy-
lene glycol at room temperature and the sol was heated at 60 1C to
obtain a wet gel. This gel was dried at 120 1C, which self-ignites to
form a fluffy product. This is then ground to form fine powder of
magnesium ferrite. A series of samples with formula MgSmxFe2 x
O4 (x ¼0–0.3 at step size 0.05) were prepared. Prepared samples
were sintered at 700 1C for 3 h.
2.2. Characterization
Structural characterization was done using X-ray powder
diffractometer (Rigaku make RINT 2000) with Cu-Kα radiation
(λ ¼1.54059 Å) at 40 kV and 30 mA by performing a scan from 201
to 801 for each sample. The crystal structure, lattice parameter,
crystallite size, X-ray density, bulk density and porosity were
determined from the XRD pattern. The Fourier Transform Infrared
(FTIR) absorption spectra of the samples were recorded using FTIR
spectrometer (Thermo Nicolet, Avatar 370) in the wave number
range 4000–400 cm 1 with Potassium Bromide (KBr) as binder.
Particle morphology was performed using Transmission Electron
Microscope (Philips-CM200) operating at 20–200 kv with resolu-
tion 2.4 Å. Wave length Dispersive X-ray Fluorescence Spectro-
meter (WD-XRF) Make: Bruker, Model: S4 PIONEER was used for
elemental analysis. Magnetic measurements were carried out
using Lakeshore VSM 7410 at room temperature.
3. Results and discussion
3.1. X-ray diffraction studies
The XRD pattern of the prepared samples of the series is shown
in Fig. 1. The XRD pattern confirms the formation of single phase
fcc spinel structure with no extra lines corresponding to any other
crystallographic phase (compared with JCPDS card no.: 73-2211).
Intensity of peak is decreasing with the doping amount of sama-
rium which suggests the difficulty in crystallization with the
addition of rare earth ion with relatively large ion radii. A shift
in prominent peak positions to lower angle with Sm doping is
noted. But extra reflections due to oxides of samarium are not
present in the diffraction pattern.
Fig. 1. XRD pattern of MgSmxFe2 xO4.
141
The interplanar spacing dhkl is calculated using Bragg's equation
which in turn helps to calculate lattice constant ‘a’ using equation
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
2 2 2
a ¼ dhkl h þk þ l ð1Þ
for prominent (311) peak. The average crystallite sizes (D) of all the
samples were calculated from the XRD peak broadening of the
peaks using Scherrer formula corrected for micro-strain using
Hall–Williamson plots [14,15]. All peaks were fitted for Lorentzian
curve to determine the angle θ for maximum intensity and full
width at half maximum (FWHM or β). Instrumental correction in
calculating β was done by applying the formula
β ¼ βobs βins ð2Þ
where βobs is the observed FWHM from the XRD pattern and βinst is
the FWHM of the standard sample taken.
For Lorentzian peak shape
λ
β cos θ ¼ þ 4εstr sin θ ð3Þ
D
where εstr is the strain due to imperfection in crystals. William-
son–Hall analysis was done by plotting graph between β cos θ and
4sin θ for all prominent peaks by applying linear best fitting. From
the graph particle size D is obtained by
λ
D¼ ð4Þ
interscept
and slope gives the strain values.
Lattice parameter obtained for MgFe2O4 (8.43 Å) is larger than
reported value of 8.37 Å [16,17]. The deviation in lattice parameter
can be attributed to the cation rearrangement in the nanosized
MgFe2O4 [6].
Since each primitive unit cell of the spinel structure contains
8 molecules, the value of X-ray density (ρx) was determined
according to the relation [15]
8M
ρx ¼ ð5Þ
Na3
where N is the Avogadro's number and M is the molecular weight
of the sample. Bulk density (ρm) was calculated using formula
m
ρm ¼ ð6Þ
πr 2 h
where m is the mass, r is the radius and h is the thickness of the
pellet.
Porosity(%) P of the samples are calculated using the formula
 
ρ
P ¼ 1 x 100 ð7Þ
ρm
Values of lattice constant, X-ray density, bulk density, porosity
and crystallite size (D) calculated from Hall–Williamson plots for
all the prepared samples are shown in Table 1. Hall–Williamson
plots for samples with x¼0 and x¼0.2 are shown in Figs. 2 and 3,
respectively.
Value of lattice constant is increasing with samarium doping
(expect for sample with x ¼0.05 and 0.15) which shows the
expansion of unit cell with rare earth doping. This is expected
due to substitution of large ionic radius of Sm3 þ ions (0.964 Å)
with small ionic radius Fe3 þ ions (0.645 Å) [18]. Decrease in ‘a’
value with Sm3 þ concentration for sample with x ¼0.05 and 0.15
suggests the occupancy of rare-earth ion in B-sites [19,20].
The crystallite size is decreasing with increase in Sm concentra-
tion, which is similar to the reported results [21,22,23]. Due to the
larger bond energy of Sm3 þ –O2 as compared to that of Fe3 þ –O2
more energy is needed to make Sm3 þ ions enter into lattice and
form Sm3 þ –O2 bonds. So Sm3 þ substituted ferrites have higher
thermal stability relative to pure magnesium ferrites; but more
energy is needed for the Sm3 þ substituted samples to complete
142 S. Thankachan et al. / Journal of Magnetism and Magnetic Materials 348 (2013) 140–145

Table 1 nano-crystals may be due to the tendency of nanoparticles to

Values of lattice constant, X-ray density, bulk density, porosity, crystallite size aggregate to achieve a low surface energy state by reducing the
calculated from Hall–Williamson plots and crystallite size calculated from TEM
specific superficial area by reducing the interfaces with other particles
images for different x value in the series MgSmxFe2 xO4.
[12]. Particle size of particles is determined using the software ‘ImageJ’
x a (Å) ρx (gcm 3
) ρm (gcm 3
) Porosity (%) D (nm) D (nm) and histogram of particle size distribution is drawn. Histogram for
from H–W plot from TEM MgFe2O4 TEM images are shown in Fig. 5. Average particle size
0 8.432 4.430 2.478 44.0 24.9 22 7 3
0.05 8.423 4.549 2.342 48.5 22.8 197 2
0.1 8.441 4.618 2.386 48.3 22.7 –
0.15 8.423 4.758 2.362 50.3 20.5 –
0.2 8.440 4.835 2.191 54.6 17.8 177 2
0.25 8.448 4.924 2.332 52.6 11.9 –
0.3 8.447 5.030 2.287 54.5 12.8 –

Fig. 4. TEM image of MgFe2O4.

Fig. 2. Hall–Williamson plots for MgFe2O4.

Fig. 5. Histogram of particle size distribution of MgFe2O4 particles from TEM image.

Fig. 3. Hall–Williamson plots for sample MgSm0.2 Fe1.98O4.

crystallization and grow grains [22]. X-ray density is increasing with

doping which is due its dependence on molecular weight. Porosity
of samples is increasing with doping concentration which is due to
the substitution of rare earth ion with large ionic radius in place of
Fe3 þ ions with small radius. High porosity is one of the main
requirement for applying ferrites as gas sensors [34], humidity
sensors etc.

3.2. TEM analysis

Figs. 4, 6 and 7 show the TEM images of MgFe2O4, MgSm0.05

Fe1.95O4 and MgSm0.2Fe1.8O4, respectively. Most of the nano-particles
are spherical in shape and are agglomerated. Agglomeration of Fig. 6. TEM image of MgSm0.05Fe1.95O4.
 S. Thankachan et al. / Journal of Magnetism and Magnetic Materials 348 (2013) 140–145 143

calculated from the TEM images are given in Table 1. Values are almost
comparable with the crystallite size obtained from XRD.
3.3. XRF-elemental analysis
The stoichiometry of the powder samples was analyzed using
Wave length Dispersive X-ray Fluorescence Spectrometer (WD-XRF).
The composition of elements present in samples MgFe2O4,
MgSm0.05Fe1.95O4 and MgSm0.2Fe1.8O4 are given in Table 2. From
the table it is obvious that the samples show concentration values of
each element very near to expected stoichiometry. No trace of
impurity was found which indicates the purity of the sample.
MgFe2O4 and MgSmxFe2 xO4 samples with x ¼0.05, 0.1, 0.2, 0.25
are shown in Figs. 9 and 10. Inset of Fig. 10 shows the loops in
applied field of 500 Oe to 500 Oe. Magnetization does not
saturate even at an applied magnetic field of 15 kOe. High
magnetocrystalline anisotropy associated with magnesium ferrite
will be contributing to this type of behavior [35]. The presence of
antiferromagnetic or paramagnetic impurities will also impede the
sample from being saturated. The MS values of all the samples
were calculated by extrapolating the inverse of the field versus
magnetization (MS) graph to 1/H ¼0 [25]. The saturation magne-
tization (Ms), coercivity (Hc), remanance (Mr) and remenant ratio

3.4. FTIR-spectra

Infrared spectra of MgSmxFe2 xO4 ferrite system for x ¼0, 0.1,

0.2 and 0.3 are shown in Fig. 8. Two major absorption bands are
found in the range 600–550 cm 1 and 450–400 cm 1. These two
bands have been reported by Waldron [24] for spinel ferrites. The
higher frequency band (ν1) is due to the stretching vibration of
unit cell of the spinel in the tetrahedral (A) site and lower band
(ν2) is caused by metal-oxygen vibration in octahedral (B) site. In
samples with more Sm3 þ concentration the higher band fre-
quency ν1 does not shift much and only a slight broadening is
observed, while lower band ν2 shifts to the low frequency region
which may be attributed to the substitution of Fe3 þ ions on
octahedral B sites by Sm3 þ ions. The bands corresponding to
3400 cm 1 and 1600 cm 1 represent stretching and bending
vibrations of H–O–H which indicates the presence of free or
absorbed water.

3.5. Magnetic measurements Fig. 8. FTIR spectra of MgSmxFe2 xO4 samples with x¼ 0, 0.1, 0.2 and 0.3.

Magnetic characterizations of the samples were carried out by

vibration sample magnetometer at room temperature with max-
imum applied field of 15 kOe. Typical magnetic hysteresis loops of

Fig. 7. TEM image of MgSm0.2Fe1.8O4. Fig. 9. Hysteresis loop of MgFe2O4.

Table 2
Values of concentration of each elements present in samples MgFe2O4, MgSm0.05Fe1.95O4 and MgSm0.2Fe1.8O4 compared with expected concentration.

Elements Concentration (%) Expected concentration Concentration (%) in Expected concentration (%)in Concentration (%)in Expected concentration (%)
present in MgFe2O4 (%) in MgFe2O4 MgSm0.05Fe1.95O4 MgSm0.05Fe1.95O4 MgSm0.2Fe1.8O4 in MgSm0.2Fe1.8O4

Mg 15.780 12 11.245 11.723 9.905 10.965

Sm Nil 0 3.829 3.672 13.698 13.740
Fe 51.330 56 53.188 53.342 46.867 46.054
O 32.600 32 32.230 31.263 28.787 29.241
144 S. Thankachan et al. / Journal of Magnetism and Magnetic Materials 348 (2013) 140–145

Fig. 10. Hysteresis loop of MgSmxFe2 xO 4 samples.

Table 3 porosity is inversely proportional, while the particle size is directly

Effect of Sm3 þ substitution on magnetic parametersof MgSmxFe2 xO 4 samples. proportional to the magnetization for nano ferrites [29].
Sm3 þ doped samples shows decrease in Ms, Mr and Hc values
x Crystallite size (nm) Ms (emu/g) Mr (emu/g) R¼ Mr/Ms Hc (Oe)
which may be due to the decrease in particle size and accom-
0 24.49 26.65 9.8 0.3677 283.27 panied increase in surface area. So we can tune the magnetic
parameters according to our application with Sm3 þ doping in
1
0.05 22.52 17.15 7.9  10 0.0458 40.08
1
0.1 22.59 16.06 5.8  10 0.0361 31.77 magnesium ferrite. Magnetic moment of Sm3 þ is predominantly
2
0.2 17.77 19.06 8.5  10 0.0044 4.81
0.25 12.81 15.17 6.1  10 2
0.0040 4.64
due to the 4 f electrons and their magnetic dipolar orientation
0.3 12.63 14.88 4.4  10 2
0.0029 3.88 exhibits disordered form at room temperature. Hence Sm3 þ
substitution can be considered as a non-magnetic ion substitution
in spinel site which reduces the exchange interaction between A
(R ¼Mr/Ms) of the samples with different Sm3 þ content and and B sites that results in decrease of magnetization. The existence
crystallite size are shown in Table 3. of random canting of particle surface spins, surface effects and the
The magnetic behavior of pure and Sm doped magnesium occurrence of a glassy state were reported to be playing an active
ferrite particles shows soft ferrimagnetic nature. The saturation role in the decline of magnetization values [21,28,31].
magnetization value obtained for undoped magnesium ferrite Doped samples with concentration x Z0.2 exhibits prominent
(26.6 emu/g) is less than that for bulk MgFe2O4 (33.4 emu/g at decrease in Mr, Hc and so remanence ratio values which indicates
room temperature) [17,26]. Value of Ms obtained for magnesium the limit in doping samarium ions in MgFe2O4 lattice for magnetic
ferrite nanoparticles synthesized by solution combustion synthesis application. Remanence is directly related to the ease of move-
(SCS) at low temperature with crystalline size 9–59 nm was 22– ment of domain walls. Low value of remanence and coercivity
31 emu/g and coercivity (Hc) reported is 69–98 Oe [12]. Coercive indicates that the domains can move in easily response to
field obtained for our undoped sample with size 25 nm is 283 Oe. magnetic fields. So lower value of remanence (R) value implies
Value of saturation magnetization depends on grain size and fewer number of domain walls. Presence of classical lattice defects
preparation temperature [27]. The lower value of Ms may be due in polycrystalline materials, cavities, inclusion of secondary phases
to the surface structural distortions and different cation distribu- and scratches can induce domain walls. So we may conclude that
tion in nano-crystalline magnesium ferrite when compared with samarium doped magnesium ferrite samples prepared is isotropic
bulk counterpart [21,28]. According to stochastic model for varia- in nature. Sm3 þ doping in magnesium ferrite has decreased the
tion in magnetic properties with particle size for nano-magnetic hysteresis loss tremendously. This suggests the feasibility in tuning
particles developed by Chakraverty and Bandyopadhy [30], below the magnetic parameters in nanocrystalline MgFe2O4 by suitable
a critical diameter at room temperature, the increase in coercivity selection of amount of doping for appropriate applications.
with an increase in particle size in the single domain region has
been clarified. A similar variation in Hc is shown by magnesium
ferrite nanoparticles with Sm3 þ doping. The decrease in Hc with 4. Conclusions
decreasing crystallite size (Table 3) is due to thermal effects
observed in particles which behave as single-domain particles. Samarium substituted magnesium ferrite nanocrystals (MgSmx
The saturation magnetization Ms is also decreasing as the particle Fe2 xO4 with x ¼0–0.3 at step size 0.05) were synthesized by sol–
size decreases. This reduction is related to surface to volume ratio. gel technique. XRD analysis revealed that all the prepared samples
Increase in porosity due to Sm3 þ doping may be another reason are single phasic cubic spinel without any secondary phase.
for the reduction in MS with samarium content. It is known that Increase in lattice constant value with samarium doping indicates
 S. Thankachan et al. / Journal of Magnetism and Magnetic Materials 348 (2013) 140–145
the expansion of unit cell. The bulk density, X-ray density and
porosity is found to increase with Sm3 þ ion content in the sample.
But crystallite size is decreasing with doping concentration. TEM
images shows the samples are spherical in shape and agglomer-
ated. The absorption bands in FTIR are found in the expected range
of spinel ferrites. The magnetic behavior of pure and Sm doped
magnesium ferrite particles shows soft ferrimagnetic nature.
Saturation magnetization, remanence and coercivity is decreased
with doping which may be due to the decrease in particle size and
accompanied increase in surface area. Sm3 þ substitution can be
considered as a non-magnetic ion substitution in spinel site which
reduces the exchange interaction between A and B sites that
results in decrease of magnetization. The existence of random
canting of particle surface spins, surface effects and the occurrence
of a glassy state may be playing an active role in the decline of
magnetization values. Low value of remanence ratio implies
isotropic nature of the samples. Moreover decrease in hysteresis
loss with doping suggests that samarium substituted MgFe2O4 can
be tuned for suitable applications with the selection of appropriate
Sm3 þ ion concentration.
Acknowledgments
ST acknowledges the University Grants Commission of India for
providing FIP fellowship. EMM thank DST and UGC for the support
given to department of Physics, Maharajas College, Ernakulam. The
authors acknowledge SAIF-IITM Chennai, CIF-Pondicherry University
and SAIF-CUSAT Kochi for providing facilities for measurements.
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