Materials Chemistry and Physics 162 (2015) 332e339

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Materials Chemistry and Physics

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

Studies on structural and magnetic properties of ternary cobalt

magnesium zinc (CMZ) Co0.6-xMgxZn0.4 Fe2O4 (x 0.0, 0.2, 0.4, 0.6)
ferrite nanoparticles
Manpreet Kaur*, Palak Jain, Mandeep Singh
Department of Chemistry, Punjab Agricultural University, Ludhiana 141 004, India

h i g h l i g h t s

 Ternary doped cobalt magnesium zinc ferrite nanoparticles are synthesized.

 FT-IR displayed red shift in tetrahedral stretching band on Zinc doping.
 Expansion of lattice and enhancement of spinel phase purity on zinc doping.
 The variation in saturation magnetization (Ms) on doping is explained.

a r t i c l e i n f o a b s t r a c t

Article history: In this paper we report the variation in structural and magnetic properties of ternary ferrite nano-
Received 2 October 2014 particles (NPs) having stoichiometery Co0.6-xMgxZn0.4 Fe2O4 (x 0.0, 0.2, 0.4, 0.6) and pure spinel ferrites
Received in revised form MFe2O4 (M Mg, Co). NPs with average particle diameter of 25e45 nm were synthesized employing
22 May 2015
self-propagating oxalyl dihydrazide - metal nitrate combustion method. The products were characterized
Accepted 29 May 2015
Available online 8 June 2015
using X-ray diffraction (XRD), Vibrating sample magnetometer (VSM), Transmission electron microscopy
(TEM) and FT-IR spectroscopy. FT-IR spectral analysis revealed two bands centered at 560 and 440 cm1
for tetrahedral and octahedral metaleoxygen bond stretching. Zinc doping caused red shift in the fre-
Keywords:
Magnetic materials
quency band of tetrahedral MO stretching. XRD powder diffraction patterns conrmed the formation of
Nanostructures spinel ferrite nanoparticles, expansion of the lattice on zinc doping and enhancement of spinel phase
Chemical synthesis purity in the doped ferrites. Cobalt ferrite displayed lowering of the magnetic parameters on zinc doping
FT-IR which further decreased in ternary ferrites Co0.6-xMgxZn0.4Fe2O4 on replacing cobalt ions with non-
Magnetic properties magnetic magnesium ions up to x 0.4. At x 0.6 reverse trend was observed and Ms was
enhanced. Magnesium zinc ferrite Mg0.6Zn0.4 Fe2O4 with high value of Ms was obtained. Combustion
process employed in the present studies serves as a low temperature facile route for the synthesis and
structural analysis of ternary doped ferrite nanoparticles.
2015 Elsevier B.V. All rights reserved.

1. Introduction
Magnetic spinel ferrites are the key materials used for elec-
tronic devices and they have varied applications as magnets, cat-
alysts, humidity sensors, phase shifters and insulators etc [1e5].
They have excelled over the pure metals as magnets owing to their
high specic resistance and remarkable exibility in tailoring the
magnetic properties. Ferrites are the mixed metal oxides having
* Corresponding author.
E-mail address: manpreetchem@pau.edu (M. Kaur).
Fe2O3 as their main component. Nano ferrites have an edge over
conventionally synthesized ferrites owing to little or no hysteresis
loss which is an essential requirement for the high frequency
magnetic devices. The unusual magnetic properties exhibited by
nanoparticles such as strong decrease in saturation magnetization
and enhancement of coercivity have attracted much interest in the
recent years [6]. Conventional ceramic method employed for the
bulk synthesis of ferrite involves solid state reaction of metal ox-
ides/carbonates at elevated temperature (>1000  C). It yields
product in micrometer regime and agglomeration owing to
inherently slow reaction kinetics is unavoidable [7]. Various soft
chemical routes are gaining interest of the scientic community

http://dx.doi.org/10.1016/j.matchemphys.2015.05.075
0254-0584/ 2015 Elsevier B.V. All rights reserved.
 M. Kaur et al. / Materials Chemistry and Physics 162 (2015) 332e339
world over for the synthesis of nano ferrites as they yield high
purity product with desired stoichiometery and greater composi-
tional control is achievable. In the recent past different methods
such as sol gel, precursor, combustion and co-precipitation have
been employed for low temperature synthesis of nano ferrites
[8e11]. Combustion process is based on the principle of fuel
chemistry. The equivalence ratio 4 (ratio of oxidizer/fuel) at which
the combustion completes is kept unity [12]. Exothermic redox
reaction takes the system to high temperature and the reaction
becomes self sustained. The ash that emerges out after completion
of combustion is the oxide material having varying applications.
Cobalt ferrite is well known magnetic material with high coer-
civity and moderate magnetization and is used in audio video
tapes and high density digital recording disks [13] similarly
magnesium zinc ferrite is used as electro magnet in transformer
cores and serves as a low cost potential substitute material for
nickel zinc ferrite as nickel containing compounds have been
identied as human carcinogens by US department of Health and
Human services [14]. Magnetic properties of ferrites are strongly
inuenced by preparation methodology and they can be radically
altered by doping and cation distribution. Moreover doped ferrites
are well suited for the cores in inductive components at high
frequencies because the electrons are scattered at the grain
boundary of nanostructure material which reduces eddy current
losses in electric applications [15]. FT-IR and XRD serve as two
important non destructive tools for qualitative analysis of the
structural details of these crystalline materials. XRD provides in-
formation regarding the formation of spinel phase and predicting
the phase purity where as IR helps in studying the formation and
structure of spinel system, as presence of other ions invariably
affect the IR parameters [16]. Inuence of zinc doping on magnetic
and structural properties of pure magnesium ferrite has been
studied extensively. Structural and magnetic properties of NieCo
substituted magnesium ferrite (synthesized by micro emulsion
method) have been reported and value of coercivity is observed to
be low [17] which is a necessary condition for the recording media
[18]. Inuence of Zn, Cu and Ce substitution on the magnetic and
structural properties of nano ferrites is reported in the literature.
However relatively few literature reports are available on the
characterization of ternary doped cobalt ferrite. We have earlier
synthesized and characterized cadmium and zinc doped magne-
sium nano ferrites [19,20]. In continuation, the present work is
focused on the comparative analysis of morphological, structural
and magnetic properties of ternary ferrite nanoparticles having
zinc, cobalt and magnesium in different stoichiometric ratios i.e.
Co0.6-xMgxZn0.4Fe2O4 (x 0.0, 0.2, 0.4, 0.6) with pure magnesium
and cobalt ferrite. The synthesized samples are characterized by
XRD, TEM, VSM and FT-IR spectroscopic techniques and inuence
of stoichiometery on the structural and magnetic parameters is
evaluated.
2. Experimental
Polycrystalline ferrites having magnesium, cobalt and zinc in
different stoichiometric ratio Co0.6-xMgxZn0.4Fe2O4 and pure fer-
rites MFe2O4 (M Mg, Co) were synthesized using oxalyl dihy-
drazide - metal nitrate combustion method. All the chemicals of AR
grade were used.
2.1. Synthesis of ferrites from oxalyl dihydrazide (ODH-metal
nitrates)
Details of the method employed for synthesis of oxalyl dihy-
drazide (ODH) is reported elsewhere [19]. It was recrystallized
using dimethyl sulphoxide and identied by elemental analysis and
333
FT-IR spectroscopy. Stoichiometric amounts of metal nitrates
(oxidizer) were mixed with ODH (fuel) in a silica crucible (keeping
oxidizer/fuel ratio unity) and the mixture was heated in a mufe
furnace at 300  C for 3 hr.
Synthesis of pure ferrites by the redox reaction is represented in
Scheme 1
MNO3 2 2FeNO3 3 4C2 H6 N4 O2 /MFe2 O4 8CO2 12N2
12H2 O Where M Mg=Co
Scheme 1
Synthesis of doped ferrites by the redox reaction is represented
in Scheme 2
0:6  xCoNO3 2 xMgNO3 2 0:4ZnNO3 2 2FeNO3 3
4C2 H6 N4 O2 /Co0:6x Mgx Zn0:4 Fe2 O4 8CO2 12N2
12H2 O Where x 0; 0:2; 0:4; 0:6
Scheme 2
2.2. Characterization techniques
FT-IR spectra were recorded on Perkin Elmer, Model RX-1 FT-IR
Spectrophotometer. X-ray diffraction measurements were carried
out using CuKa radiation (l 1.5404A ) with a Panlytical X'pert
Pro. Magnetic properties of ferrite powder samples were studied by
vibrating sample magnetometer Model PAR-155. Transmission
electron micrographs (TEM) were recorded by employing Trans-
mission Electron Microscope model Hitachi Hi-7650 at 100 kV ac-
celeration voltages in HC mode using water as a dispersion
medium.
3. Results and discussion
3.1. Experimental density
Archimedes principle was employed to evaluate experimental
densities (dexp) of the nanoferrite samples using xylene as a me-
dium [21]. Doping with zinc resulted in an increase in dexp from
1.508 g/cc to 1.724 g/cc and 2.478e2.945 g/cc for MgFe2O4 and
CoFe2O4 nanoparticles respectively (Table 1). The observed trend
can be attributed to greater mass to volume ratio of zinc in com-
parison to magnesium and cobalt. Similar trend has been observed
in the cadmium doped magnesium ferrites. Further doping of co-
balt zinc ferrite with magnesium Co1-xMgxZn0.4 Fe2O4 (x 0.0, 0.2,
0.4, 0.6) resulted in decrease in the density as magnesium has lower
atomic weight as compared to cobalt. Lower value of density of
powdered samples as compared to compressed pellets is attributed
to the less porosity of the later which elevates the density of the
pelletized powder.
3.2. XRD studies
The lattice constant or lattice parameter (a) was calculated
employing the following relationship:
 1=2
a d h2 k2 l2
The XRD density was calculated by formula:
8M
dXRD
Na3
Where
334 M. Kaur et al. / Materials Chemistry and Physics 162 (2015) 332e339

Table 1
XRD parameters of ferrite nanoparticles.

Composition Lattice constant (A ) X-Ray density (g/cc) Physical density (g/cc) %Age porosity Average Particle diameter (nm)

MgFe2O4 8.308 4.632 1.508 10.96 25.65

CoFe2O4 8.297 5.401 2.478 27.36 31.48
Co0.6Zn0.4Fe2O4 8.356 5.456 2.945 35.64 15.39
Co0.4 Mg0.2Zn0.4Fe2O4 8.339 5.274 2.234 23.39 28.31
Co0.2 Mg0.4Zn0.4Fe2O4 8.4002 5.006 2.069 21.10 14.79
Mg0.6Zn0.4Fe2O4 8.380 4.885 1.724 14.91 43.98

M Molecular weight of the sample

N Avogadro's number

Average particle size (D) was estimated with Scherrer's rela-

tionship [22]:

l
D
dCosq

where d is full width at half maximum.

The percentage porosity for all the compositions was calculated
by using the equation:

dexp
1  100
dXRD
X-Ray diffraction patterns and Miller indices (hkl) for ferrite
nanoparticles were in agreement with the reported values [23,24].
The diffraction pattern of magnesium ferrite and cobalt ferrite
(Figs. 1a and 2a) consisted of peaks corresponding to crystallo-
graphic planes (220), (311), (400), (410) (422), (511) and (440)
which were also conrmed by matching with ASTM Data Card No.
17e465 and 3e864 for MgFe2O4 and CoFe2O4 respectively. Traces of
a-Fe2O3 were also detected and corroborated with ASTM Data Card
No. 33-0664. Presence of a-Fe2O3 indicated decomposition of ferric
nitrate into a-Fe2O3 prior to the solid state reaction leading to
formation of spinel ferrite. Lattice constant (a) was calculated using
the most intense (311) peak. Lattice parameters are given in Table 1.
Doping with zinc resulted in lattice expansion of the synthesized
ferrites owing to preference of large zinc ions for the tetrahedral
site thus increase in lattice constant. Similar trend has been
observed in CoeZn and MneZn ferrite NPs prepared by co-
precipitation method [8]. In the ternary doped ferrites with stoi-
chiometery Co1-xMgxZn0.4 Fe2O4 (x 0.0, 0.2, 0.4, 0.6) on increasing
x the lattice constant rst decreased because of the replacement of
cobalt ions but further addition of magnesium ions caused lattice
expansion and at x 0.6 lattice constant displayed slight decrease
indicating effect of replacing magnesium ions with cobalt ions. Zinc
Fig. 2. XRD patterns of (a) CoFe2O4 (b) Co0.6Zn0.4Fe2O4 (c) Co0.4Mg0.2Zn0.4Fe2O4 (d)
Co0.2Mg0.4Zn0.4Fe2O4.
doping also resulted in growth of spinel phase in the crystallites as
no peaks corresponding to a-Fe2O3 were detected in zinc doped
ferrites (Figs. 1b and 2b and c). Similar results have been reported
during synthesis of cobalt zinc ferrite and manganese zinc ferrite by
co-precipitation method [24]. Zinc doping of 0.4 was observed to be
a region of spinel phase purity. Sharpening of the peaks with
doping and reduced full width at half maximum was associated
with increased average particle size. The dXRD increased on zinc
doping from 4.632 to 4.885 g/cm3 in magnesium ferrite and from
5.401 to 5.456 g/cm3 in cobalt ferrite. This is owing to the greater
mass volume ratio of Zn as compared to Mg and Co. In ternary
doped ferrites with stoichimetery Co1-xMgxZn0.4 Fe2O4 (x 0.0, 0.2,
0.4, 0.6) on increasing the value of x there was regular decrease in
the density because of replacement of cobalt ions with magnesium
ions of lower atomic weight (Fig. 3). The values dexp were lower
than corresponding dXRD values because samples in powder form
were porous in nature. The porosity values increased with zinc
doping and decreased on replacing cobalt ions with magnesium
ions in cobalt zinc ferrite (Table 1). Trend followed was similar to

Fig. 3. Variation of XRD density and lattice constant with x for Co1-xMgxZn0.4 Fe2O4
Fig. 1. XRD patterns of (a) MgFe2O4 (b) Mg0.6Zn0.4Fe2O4. (x 0.0, 0.2, 0.4, 0.6).
 M. Kaur et al. / Materials Chemistry and Physics 162 (2015) 332e339
Fig. 4. FT-IR patterns of (a) CoFe2O4 and (b) Co0.6Zn0.4Fe2O4(c) MgFe2O4 and (d)
Mg0.6Zn0.4Fe2O4.
the dXRD and dexp as the value of porosity was calculated from these
two parameters.
3.3. FT-IR study
FT-IR spectra of magnesium and cobalt ferrites displayed two
bands in the region 370e600 cm1. The higher frequency band (n1)
located in the region 600-550 cm1 corresponds to stretching
Fig. 5. TEM micrograph of (a) CoFe2O4 and (b) histogram.
Fig. 6. TEM micrograph of (a) MgFe2O4 and (b) histogram.
335
vibrations of metal ions in the tetrahedral sites whereas the second
lower frequency band (n2) observed in the region 370e450 cm1
was due to the stretching vibrations of metal ions in the octahedral
site [25]. The difference in band position was caused by difference
in MO distance in tetrahedral and octahedral sites. The range of
absorption band obtained are in good agreement with the reported
in literature values [26e28]. Absence of extra peaks indicate that
the prepared samples were free from anionic impurities and any
organic residue. In cobalt ferrite the tetrahedral stretching fre-
quency band n1 displayed a clear shift in the band position from
570.3 cm1 to 560.9 cm1 on zinc doping which conrms presence
of zinc ions in the octahedral site. (Fig. 4a and b) This red shift i.e.
lowering in frequency of absorption is attributed to the inverse
relation of force constant and the reduced mass. Zinc has prefer-
ence for the tetrahedral site and there is an increase in the reduced
mass on zinc doping, causing lowering of the force constant and
hence frequency of absorption displayed red shift. Similar trend
was observed on zinc substitution in magnesium zinc ferrite (Fig. 4c
and d).
3.4. TEM study
TEM images taken by water dispersion method clearly depict
the formation of ultra ne, well dispersed spherical ferrite NPs.
Cobalt ferrite and magnesium ferrite (Figs. 5a and 6a) displayed
smaller crystallite size as compared to the doped ferrite nano-
particles (Figs. 7ae10a). The particle size distribution histograms
for the former (Figs. 5b and 6b) show that the maximum fraction of
particles have size between 20e30 nm. Figs. 7e10 display TEM
336 M. Kaur et al. / Materials Chemistry and Physics 162 (2015) 332e339

Fig. 7. TEM micrograph of (a) Co0.6Zn0.4Fe2O4 and (b) histogram.

Fig. 8. TEM micrograph of (a) Co0.4Mg0.2Zn0.4Fe2O4and (b) histogram.

micrographs for the doped ferrite samples. Larger particle diameter
owing to the growth in crystallinity was clearly observed for the
doped ferrites with maximum fraction of particles having size
ranging from 30 to 50 nm (7b-10b). These results are corroborated
with the XRD ndings where sharpening of peaks on doping
conrmed increase in particle size (Fig. 11).
3.5. Magnetic studies
VSM results revealed effect of varying stoichiometery on mag-
netic parameters of the ferrite samples (Table 2). Hysteresis plots
showing the variation of magnetization (M, emu/g) as a function of
applied magnetic eld (H, Oe) were plotted for the prepared ferrite
samples (Figs. 11e13). All the samples displayed normal (s shaped)
narrow hysteresis loops. Magnetic parameters like saturation
magnetization (Ms), remnant magnetization (Mr) and coercivity
(Hc) of the samples were compared which in turn depend upon
number of factors viz. density, anisotropy, grain growth and AeB
exchange interactions. Narrow loop indicated low coercively values
ranging from 9.00 Oe to 330.00 Oe. Lowering of coercivity indicates
that the prepared sample can be demagnetized easily (Fig. 14).
Pure cobalt ferrite displayed Ms Mr and Hc values of 41.12 emu/g,

Fig. 9. TEM micrograph of (a) Co0.2Mg0.4Zn0.4Fe2O4 and (b) histogram.

 M. Kaur et al. / Materials Chemistry and Physics 162 (2015) 332e339 337

Fig. 10. TEM micrograph of (a) Mg0.6Zn0.4Fe2O4 and (b) histogram.

Fig. 11. Magnetic hysteresis loops of MgFe2O4 and Mg0.6Zn0.4Fe2O4.

Fig. 13. Magnetic hysteresis loops of Co0.4Mg0.2Zn0.4Fe2O4 and Co0.2Mg0.4Zn0.4Fe2O4.

16.22 emu/g and 330.00 Oe respectively. Presence of Zn2 ions in

the A sites in case of cobalt zinc ferrite lowered the value of these
parameters (Table 2). This reverse trend is attributed to replace-
ment of magnetic cobalt ions with non magnetic zinc ions. Cobalt
ferrite has inverse spinel structure in which Co2 ions are present in
B sites whereas Fe3 ions are distributed between A and B sites.
Cobalt zinc ferrite is formed by replacing Co2 ions from B sites and
simultaneously addition of non magnetic zinc ions in the A sites.
Doping cobalt zinc ferrite with non magnetic magnesium ions
resulted in further lowering in Ms values to 33.35emu/g and
13.27emu/g respectively for Co(0.6-x)MgxZn0.4Fe2O4 nanoparticles
having x 0.2 and 0.4 respectively. Similar trend was observed by
Arulmurugan et al. [8] in the cobalt zinc ferrites prepared by co-
precipitation method and they have attributed it to the number
of factors such as formation of dead layer at the surface, existence of
random canting of particle surface spin, non saturation effects due
to random distribution of particle size and deviation from normal
cationic distribution. At x 0.6 there was enhancement of Ms in the

Fig. 14. Variation of saturation magnetization and coercivity for ferrites with
Fig. 12. Magnetic hysteresis loops of CoFe2O4 and Co0.6Zn0.4Fe2O4. composition Co1-xMgxZn0.4 Fe2O4 (x 0.0, 0.2, 0.4, 0.6).
338 M. Kaur et al. / Materials Chemistry and Physics 162 (2015) 332e339
Table 2
Magnetic parameters of ferrite nanoparticles.
Composition Saturation magnetization Ms (emu/g)
MgFe2O4 13.17
CoFe2O4 41.12
Co0.6Zn0.4Fe2O4 40.38
Co0.4Mg0.2Zn0.4Fe2O4 33.35
Co0.2Mg0.4Zn0.4Fe2O4 13.27
Mg0.6Zn0.4Fe2O4 42.29
prepared samples. Mg0.6Zn0.4 Fe2O4 displayed the values of Ms and
Mr 42.29 emu/g and 6.348 emu/g respectively. Similar trend was
observed by Diagle et al. in the magnesium zinc ferrite synthesized
by co-precipitation method [29]. On the contrary pure magnesium
ferrite displayed Ms Mr and Hc values of 13.17 emu/g, 0.975 emu/g
and 70.00 Oe respectively Increase in saturation magnetization at
this stage can be attributed to Neel's theory of ferrimagnetism [30].
For small concentration of non magnetic ions, saturation magne-
tization is represented by the relationship:
Ms jMB  MA j
Where MB and MA denote magnetization of A and B site ions
respectively. Increase in saturation magnetization on doping is
attributed to the non magnetic nature of Zn2 ions [31]. Due to
polarization effects, they prefer tetrahedral sites and presence of
non magnetic zinc ions in these sites results in lowering of MA and
consequently enhancement of Ms values. Preference of Zn2 ions
for A sites also facilitates the migration of Fe3 ions into B sites
which give rise to anti parallel spin coupling resulting in weakening
of AeB exchange interactions, thus causing increase in saturation
magnetization value.
4. Conclusion
Ternary doped ferrites having composition Co0.6-xMgxZn0.4
Fe2O4 (x 0.0, 0.2, 0.4, 0.6) and pure spinel ferrite MFe2O4 (M Mg,
Co) nanoparticles with average crystallite size of 30 nm were suc-
cessfully synthesized by oxalyl dihydrazide - metal nitrate com-
bustion route at 300  C The temperature of ferrite formation is
lower as compared to co-precipitation or conventional ceramic
method. Spectral and XRD analysis revealed spinel structure of
these nano ferrites. Although synthesis conditions were the same
but difference in cationic composition had denite impact on the
magnetic and structural parameters. XRD patterns clearly
conrmed that doping enhanced spinel phase purity. Presence of
zinc in the samples caused lattice expansion. Cobalt ferrite dis-
played lowering of the magnetic parameters on zinc doping which
further decreased in ternary ferrites Co0.6-xMgxZn0.4 Fe2O4 on
replacing cobalt ions with non magnetic magnesium ions. At
x 0.6 reverse trend was observed and Ms was enhanced. Mag-
nesium zinc ferrite Mg0.6Zn0.4 Fe2O4 with high Ms value indicated
its potential application in the preparation of ferrouid. Combus-
tion process serves as low temperature facile route for the synthesis
and structural analysis of ternary doped ferrite nanoparticles.
Acknowledgment
Authors are thankful to Electon microscopy and Nanoscience
Laboratory, PAU for providing imaging facilities.
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