Powder Technology 203 (2010) 348353

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Powder Technology
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / p ow t e c

Synthesis and characterization of pure single phase NiZn ferrite nanopowders by

oxalate based precursor method
Prita Pant Sarangi a, S.R. Vadera b, M.K. Patra b, N.N. Ghosh a,
a
b

Chemistry Group, Birla Institute of Technology and Science-Pilani, Goa Campus, Zuarinagar-403726, India
Defence Lab, Jodhpur-342011, India

a r t i c l e

i n f o

Article history:
Received 4 January 2010
Received in revised form 19 May 2010
Accepted 25 May 2010
Available online 31 May 2010
Keywords:
nanopowders
X-ray methods
Chemical preparation
Electrical properties
Ferrites

a b s t r a c t
Series of single-phase Ni1 xZnxFe2O4 (x = 0.20, 0.35, 0.50 and 0.60) nanopowders with average particle size
of 35 nm have been synthesized by using oxalate based precursor method. Precursor powders were
synthesized by reacting aqueous solutions of metal nitrates and oxalic acid by using different total metal
ions: oxalic acid molar ratios and then evaporating them to dryness. Pure, single-phase NiZn ferrite
nanopowder was formed by calcining the precursor with total metal ion: oxalic acid ratio of 1:0.125 at a
temperature of 850 C. The synthesized nanopowders were characterized by using X-ray diffraction, Thermogravimetric and Differential Scanning Calorimetric analysis, Transmission Electron Microscope and Scanning
Electron Microscope. Room temperature DC resistivity of the nanopowders was measured with respect to
temperature by the two-probe method and was of the order of 107 cm. Room temperature saturation
magnetization was measured by using Vibrating Sample Magnetometer and it varied between 3449 emu/g
depending on the composition. This aqueous solution based method provides a simple and cost-effective
route to synthesize single phase, NiZn ferrite nanopowders.
2010 Elsevier B.V. All rights reserved.

1. Introduction
NiZn ferrites are magnetically soft materials that possess versatile
properties like high saturation magnetization, low coercivity, high
resistivity and low dielectric losses. These properties make them best
suited for numerous high frequency applications like inductance coils,
transformer cores, antennas, microwave absorbers etc [1,2]. Ferrite
coatings and thin lms are frequently used as the magnetic layer of
magneto-optical recording medium. Nanostructured NiZn ferrite
and their composites have generated a lot of interest in recent years.
This is due to their potential to exhibit certain superior properties that
could lead to novel applications in the eld of high frequencies,
biosensors, targeted drug delivery, catalysts, pigments etc [3,4].
Ferrites are conventionally prepared by the high temperature
solid-state route [1,5]. The method, however, is inappropriate to
synthesize nanostructured ferrites because it results in coarsening of
grains, inhomogeneity, imprecise control of cation stoichiometry etc.
The solid state method is, thus, getting supplanted by several wet
chemical methods like solgel [6], combustion [7], precursor [6,8], coprecipitation [9], reverse micelle [10], hydrothermal [11] etc. We have
critically reviewed several synthetic routes for different ferrite
compositions having ultrane or nanoscale particles and references
are cited therein [12]. The preparation of nanostructured ferrite

Corresponding author. Tel./fax: + 91 832 2580318/2557033.

E-mail address: naren70@yahoo.com (N.N. Ghosh).
0032-5910/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2010.05.027

powders by wet chemical methods has some inherent limitations

including (i) use of costly metal alkoxides, which are difcult to
synthesize, handle, and alcohols as solvents in solgel method, (ii)
strong base, like NaOH, as precipitating agent for co-precipitation
method, (iii) use of high-pressure reactor in hydrothermal method
etc. In order to surmount the limitations associated with the abovementioned methods, we have already developed aqueous solution
based methods to synthesize pure hematite nanopowders [1316].
Shinde et al and Ghodake et al have reported the oxalate precursor
based precipitation method in order to prepare nanosized ferrites
[17,18]. Based on our literature survey, use of oxalate based precursor
method for preparation of NiZn nanoferrites has not yet been well
explored. Moreover, use of water as the solvent in oxalate precursor
based method has been a major challenge until now. Though the
oxalate method seems to be very convenient, it is also associated with
some problems, such as segregation of impurity phase in the nal
product. This is due to the less solubility of metal oxalates in pure
aqueous medium that quite often precipitate out from the reaction
mixture and form small amount of impurity in the form of metal
oxides in the nal product [19]. The purity of synthesized material is
crucial for the accurate measurement of physical properties (such as
electrical and magnetic properties). Rao et al have reported an oxalate
co-precipitation method for synthesis of ferrites using a mixture of
water and alcohol as medium in order to avoid the precipitation of
metal oxalates during synthesis [20]. Apart from this, in oxalate coprecipitation method, during ltration and washing of the precipitates, loss of some micro amount of metal ions may occur. This loss

P.P. Sarangi et al. / Powder Technology 203 (2010) 348353

349

may not be detected by XRD but it might affect the properties.

Therefore, it is vital to determine the appropriate reaction conditions
to obtain pure, single phase, nanostructured ferrites by this method.
In this paper, we have described the synthesis of pure, singlephase Ni1 xZnxFe2O4 nanopowders with x = 0.20, 0.35, 0.50 and 0.60
by using aqueous solution based oxalate precursor method. We have
investigated the effect of total metal ion: oxalic acid ratio on the
purity of nal product and have demonstrated that pure, single-phase
Ni1 xZnxFe2O4 nanopowder can be synthesized when this ratio is 1:
0.125. For this particular ratio, we have compared the resistivity
behavior of unsintered nanopowders with those of sintered samples
and performed room temperature magnetization measurement.
2. Experimental procedure
2.1. Chemical synthesis
The chemicals used were Fe (NO3)3.9H2O (99.9%, Merck, India),
Ni (NO3)2.6H2O (99.9%, Merck, India), Zn dust (99.9%, Merck, India),
and oxalic acid (99.9%, Merck, India) without further purication.
Zn (NO3)2 was prepared by dissolving Zn dust in aqueous nitric acid.
Stoichiometric amounts of metal nitrates were dissolved in distilled
water according to the molar compositions as shown in Table 1.
Aqueous solutions of metal nitrates and oxalic acid were mixed in
a molar ratio ranging from 1: 3 to 1:0.125. The solutions were stirred
for 1 h at room temperature using a magnetic stirrer. It was observed
that for molar ratios 1:3 and 1:2, the reaction mixtures turned turbid
on standing. When the ratio was lowered to 1:1 and further until
1:0.125, the reaction solutions remained clear on standing. Precursors
of various shades of brown and green color were formed when the
mixtures were evaporated to dryness on a hot plate at 125 C. The
precursor powders, prepared using different molar ratio of metal ions:
oxalic acid, were then calcined in air in temperatures ranging from
450 to 1000 C for 2.30 h to obtain NiZn ferrite nanopowders.

Fig. 1. TG-DTG-DSC thermograms of Ni0.50Zn0.50Fe2O4 precursor.

3. Results and discussion

3.1. Thermal analysis
Thermal decomposition behavior of the precursors prepared using
various total metal ions: oxalate ratio as well as different values of
x for Ni (1 x) ZnxFe2O4, was investigated by using TG-DSC analysis.
They exhibited similar decomposition behavior. Here, we have
discussed the thermal decomposition behavior of precursor powder
prepared using molar ratio 1:0.125 and x = 0.50 as a representative
(Fig. 1). From TGA, a total weight loss of 25% was observed when the
sample was heated between 30 to 900 C in air. A weight loss of 9%
occurred between 30 to 150 C that could be assigned to the hydrated
water of oxalate precursor. This weight loss was reected in DSC
thermogram as an endothermic peak at 78 C. Major weight loss of
16% was observed between 150 to 500 C and that could be
attributed to loss of metal coordinated water molecules [21] as well
as decomposition of carbonaceous mass of the precursor. This weight
loss was reected as an endothermic peak in DSC thermogram at
288 C and an exothermic peak at 418 C respectively. It was
observed that beyond 500 C, there was no signicant weight loss
until 900 C.

2.2. Sample characterization

Thermo gravimetric Analysis (TGA) and Differential Scanning
Calorimetric (DSC) analysis were carried out for the precursors by
using Shimadzu DTG-60 and Shimadzu DSC-60 respectively. Room
temperature X-ray diffraction (XRD) spectra of the precursors and the
calcined powders for all compositions were recorded by using a
Rigaku Powder X-ray Diffractometer (Mini Flex II) with Cu K
( = 0.15405 nm) radiation. The particle size for the calcined powder
was determined by using a Field Emission Gun Transmission Electron
Microscope (JEOL JEMS FEG-TEM, -2100). Morphology of the calcined
powders and sintered pellets was studied by using JEOL Scanning
Electron Microscopy (JSM-6360LV). DC resistivity of the as-synthesized
nanopowders and sintered powders was measured with respect to
temperature by the two-probe method by using Keithley Electrometer
(6517A, USA). For this purpose, pellets were coated on both surfaces
with silver for resistivity measurements. Room temperature magnetization measurement was performed for powders calcined at 850 C for
all compositions by using an ADE Vibrating Sample Magnetometer
(VSM) (EV5).

3.2. X-ray diffraction

In order to determine the optimum condition (e.g., total metal ion :
oxalate ratio and calcinations temperature) to generate single phase
NiZn ferrite, room temperature powder XRD analysis of calcined
powders was performed and formation of crystalline phases due to
calcination of different precursors was monitored. It was observed that
for all the calcined powders (Fig. 2) diffraction peaks corresponding to
(111), (220), (311), (222), (400), (422), (511) and (440) diffraction
planes of NiZn ferrite [22] were present. It is important to note that,
for the calcined powders obtained from the precursors, prepared with

Table 1
Molar ratio of starting compounds with varying ratio of total metal ions: oxalic acid for different precursors.
Target composition

Fe(NO3)3.9H2O

Ni(NO3)2.6H2O

Zn

Ni0.80Zn0.20Fe2O4
Ni0.65Zn0.35Fe2O4
Ni0.50Zn0.50Fe2O4
Ni0.40Zn0.60Fe2O4

0.084
0.084
0.084
0.084

0.034
0.027
0.021
0.017

0.008
0.015
0.021
0.025

Moles of oxalic acid used in different reaction mixture (total metal ions : oxalic acid)
1:3

1:2

1:1

1:0.75

1:0.50

1:0.25

1:0.125

0.378
0.378
0.378
0.378

0.252
0.252
0.252
0.252

0.126
0.126
0.126
0.126

0.0945
0.0945
0.0945
0.0945

0.063
0.063
0.063
0.063

0.0315
0.0315
0.0315
0.0315

0.01575
0.01575
0.01575
0.01575

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P.P. Sarangi et al. / Powder Technology 203 (2010) 348353

Fig. 2. XRD spectra of Ni0.80Zn0.20Fe2O4 powders, obtained from precursors with

different total metal ions: oxalic acid ratio (1:3 to 1:0.125) calcined at different
temperatures ranging from 850 to 1000 C. In the gure, (*) denotes the impurity phase
corresponding to pure hematite.

total metal ions and oxalic acid ratio ranging from 1:3 to 1:0.25, peaks
corresponding to -Fe2O3 (hematite) as an impurity phase were also
present. In Fig. 2(af), the peaks for impurity phase are marked as (*)
and correspond to (012), (104), (113), (024) and (300) diffraction
planes of pure hematite [JCPDS 80-2377]. In fact, this impurity was
present even at high calcinations temperature of 1000 C. When the
ratio was lowered to 1:0.125 (Fig. 2 (g)), we observed the formation of
pure single-phase NiZn ferrite at a comparatively lower calcination
temperature of 850 C. In order to conrm that the optimum molar
ratio for formation of pure NiZn ferrite is 1:0.125, we performed X-ray
diffraction for powders (Fig. 3) obtained by calcining various
precursors, with different total metal ions: oxalic acid ratio, at a
temperature of 850 C for 4 h. It clearly shows the absence of impurity
peak for the precursor with 1: 0.125 ratios. After obtaining pure phase
for the ratio 1:0.125, for x = 0.20, we also performed X-ray diffraction
for different compositions for the same ratio 1:0.125. The spectra for
the precursor powders calcined at a temperature of 850 C of series of
NiZn ferrite compositions is shown in Fig. 4. Crystallite size of the

Fig. 3. Room temperature XRD spectra of the calcined powders prepared by calcining
different precursors of Ni0.80Zn0.20Fe2O4 (total metal ion: oxalic acid ratio ranging from
1:3 to 1:0.125) at 850 C. Impurity peaks of hematite marked as (*).

Fig 4. XRD spectra of the Ni(1 x)ZnxFe2O4 powders obtained by using precursors with
metal ion: oxalic acid molar ratio of 1:0.125 and calcined at 850 C. Absence of impurity
phase is clearly observed.

calcined powders for molar ratio 1:0.125, for all synthesized

compositions, was calculated by using Scherrer's equation. It was
found to be in the range of 1530 nm depending upon the calcination
temperature.
Thus, from XRD analysis we observed that pure NiZn ferrite was
obtained by the oxalate precursor method when the metal ions: oxalic
acid ratio was 1:0.125 and the calcination temperature was 850 C.

Fig. 5. TEM micrographs of NiZn ferrite nanopowders calcined at 850 C for

(a) x = 0.50 and (b) x = 0.60.

P.P. Sarangi et al. / Powder Technology 203 (2010) 348353

When the amount of oxalic acid is comparatively less, there is a

probability of formation of chelate complex by bridging different
metal ions where H2O can also get coordinated with the metal atoms
and form a water-soluble complex [23]. Whereas, presence of higher
amount of oxalic acid in the reaction mixture, increases the
probability of formation of metal-oxalate complex with single metal
ion. Generally, the solubility of these pure metal oxalate (e.g., iron
oxalate, zinc oxalate) complexes is less in aqueous medium.
Therefore, they can easily precipitate out from the reaction mixture
and eventually form segregated metal oxides and are present as
impurity in the nal product. This supports the observation that,
during preparation of precursor, turbidity was observed when metal
ion: oxalic acid ratio was 1:2 and 1:3 while the solutions were clear
with lower ratios. Therefore, we can conclude that reducing the
amount of oxalic acid in the reaction mixture used for preparing the
precursor, decreases the probability of preferential precipitation of
water insoluble metal oxalates. This results in the formation of pure
NiZn ferrite phase at a calcination temperature of 850 C.
3.3. TEM analysis
Transmission Electron Microscope was used to investigate the
particle size of the pure NiZn ferrite nanoparticles (prepared from the
precursor, with total metal ions: oxalic acid ratio 1:0.125, at a
calcination temperature of 850 C). The TEM micrographs of NiZn

351

ferrite nanopowder x = 0.50 and x = 0.60 are shown in Fig. 5(a) and
(b) respectively. The nanopowders were of average particle size
35 nm. They were almost spherical in shape and were found to be
loosely agglomerated.
3.4. SEM analysis
SEM was used to investigate the microstructures with change in
sintering temperature and composition of Ni1 xZnxFe2O4 nanopowders. Ni1 xZnxFe2O4 nanopowders used here were obtained by
calcining the precursors, with total metal ions: oxalic acid ratio
1:0.125, at a temperature of 850 C. For this purpose, four sets of
pellets were prepared by using powders calcined at 850 C; (i) one set
of pellet was kept unsintered to investigate the original microstructure of the as synthesized nanopowders. The other three sets of pellets
were sintered at (ii) 1100, (iii) 1200 and (iv) 1300 C for 2 h. SEM
micrographs exhibiting evolution of microstructure with change in
composition and sintering temperature are shown in Fig. 6 (ai) and
discussed below.
SEM micrographs of the as-synthesized samples exhibited uniform,
almost spherical shaped and loosely agglomerated particles of NiZn
ferrite powders (Fig. 6 ac). When sintering was performed at 1100 C,
the grains retained their spherical shape but they grew to micron-size.
They were also found to be agglomerated and exhibited lots of
intergranular porosity (Fig. 6 de). Sintering at 1200 C resulted in

Fig. 6. (a) x = 0.20, unsintered, (b) x = 0.35, unsintered, (c) x = 0.60, unsintered, (d) x = 0.35, sintered at 1100 C, (e) x = 0.50, sintered at 1100 C, (f) x = 0.20, sintered at 1200 C, (g)
x = 0.60, sintered at 1200 C, (h) x = 0.20, sintered at 1300 C, (i) x = 0.60, sintered at 1300 C.

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P.P. Sarangi et al. / Powder Technology 203 (2010) 348353

formation of well-dened, bigger grain sizes (2 m) with reduction in

porosity and lessened amount of agglomeration (Fig. 6 fg). The effect of
increase in Zn concentration (x = 0.60) was well reected in Fig. 6(g)
where densication occurred largely as compared for the sample with
less Zn concentration (x = 0.20, Fig 6(f)). When sintering was
performed at 1300 C, the homogenous microstructure obtained by
sintering at 1200 C was destroyed and one could only observe a
fractured microstructure (Fig. 6(h) and (i)). It should also be noted that,
though sintering temperature was reasonably high (1300 C), Zn loss
was not observed in our samples. Zn loss at this high temperature has
been reported in SEM micrographs in the form of intragranular porosity
[24]. This ensures the maintenance of stoichiometry of the assynthesized samples at very high temperatures.
3.5. DC resistivity
We have recorded the DC resistivity of all compositions for the
unsintered pellets (nanopowders) and pellets (micron-sized powders)
sintered at 1100, 1200 and 1300 C. To measure DC resistivity we have
used the same pellets, which were used to investigate microstructure by
SEM (Section 3.4). This will help us to understand the inuence of
microstructure, particularly grain size, on electrical property of the
Ni(1 x)ZnxFe2O4. A comparative graph indicating the differences in the
nature of curve and magnitude of the resistivity of unsintered and
powder sintered at 1200 C for all values of x in the NiZn ferrite series is
shown in Fig. 7. Fig.8. shows the variation of DC resistivity with
temperature for unsintered and sintered Ni0.8Zn0.2Fe2O4 powders. It was
observed from Fig.7 (A) and (B) that there is a vital difference in the
resistivity behavior of unsintered and sintered samples. The unsintered
samples exhibit the typical nature of ferrites only beyond the
temperature of 100 C, whereas sintered samples exhibited the typical
NTCR (negative temperature coefcient of resistance) behavior of
ferrites [6] starting from room temperature. The increase in resisitivity
of unsintered samples till 100 C might be attributed to the presence of
open porosity, loose agglomeration of powders (as seen in SEM
micrographs, Fig. 6(ac)) and entrapped moisture inside the pores of
the as-synthesized nanopowders [25,26] (humidity recorded in our lab
was 90% at room temperature). Increasing the temperature up to
100 C caused the evaporation of moisture from the samples and
therefore, maximum resistivity was attained (Fig. 7(A)). This maximum
in resistivity corresponds to desorption of moisture from the samples.
After 100 C, the samples exhibited typical NTCR behavior of ferrites.
The samples sintered at 1100 C had bigger grains and reduced porosity
(as seen in SEM micrographs, Fig. 6(de)). Therefore, the impact of

Fig. 7. Variation of DC resistivity with temperature of (A) unsintered pellets of Ni1 xZnxFe2O4
nanopowders and (B) sintered pellets at 1200 C of Ni1 xZnxFe2O4 powders.

Fig. 8. Variation of DC resistivity with temperature of Ni0.8Zn0.2Fe2O4 powder for (a)

unsintered and pellets sintered at (b) 1100 C (c) 1200 C and (d) 1300 C. Left Y-axis
shows the scale for (a) and (b) and right Y-axis shows the scale for (c) and (d).

adsorption of moisture in these samples was also less pronounced in

comparison to the unsintered samples. This was clearly reected on
comparing Fig. 8(a) and (b). Samples sintered at still higher temperature
of 1200 C exhibited typical NTCR behavior of ferrites from room
temperature to 225 C. This is because the microstructures of these
samples revealed a uniform and homogenous microstructure and the
absence of any intergranular porosity especially for higher Zn
concentration (x = 0.60). Sintering the samples at a very high
temperature such as 1300 C resulted in an exceptionally low resistivity
although the behavior was NTCR throughout the temperature range of
measurement. The low resistivity might be due to the fractured
microstructure. Room temperature resistivity was 107 cm for
unsintered samples and was found to decrease with increase in
sintering temperature. This is obvious, as larger grains would imply a
lesser resistance to electron ow.
3.6. Magnetization measurement
Room temperature magnetization for all compositions of
Ni1 xZnxFe2O4 (x = 0.20, 0.35, 0.50, and 0.60) was investigated
and is shown in Fig. 9 for x = 0.20 and 0.60. In this investigation the

Fig. 9. Room temperature hysteresis loops for Ni1 xZnxFe2O4 (a) x = 0.20 and (b) x = 0.60.

P.P. Sarangi et al. / Powder Technology 203 (2010) 348353

Ni1 xZnxFe2O4 nanopowders used were synthesized by calcining the

precursors, with total metal ions: oxalic acid ratio 1:0.125, at a
temperature of 850 C, because these calcined powders possess
single phase NiZn ferrite spinal crystal structure (XRD spectra Fig. 4).
The compositional study of the series showed a decrease in
the saturation magnetization (from 49 to 34 emu/g) with increasing
Zn2+ ion concentration in the compositions. It is well known that
Zn2+ ions have an afnity to occupy tetrahedral (A) sites and Ni2+
ions have a tendency to go into the octahedral (B) sites in the crystal
lattice. It might happen that as the diamagnetic Zn 2+ ions
introduced in the lattice is increased, it starts replacing Fe3+ ions
from the A sites which start migrating towards B sites. The
weakening of AB exchange coupling due to this migration results
in decrease of magnetic moment.
4. Conclusion
Series of Ni1 xZnxFe2O4 (0b b 1) ferrites were synthesized by
oxalate precursor based method. Average particle size was found to be
35 nm. Room temperature X-ray diffraction conrmed the formation
of single-phase NiZn ferrite at 850 C when the total metal ions: oxalic
acid ratio was 1:0.125. The as-synthesized nanopowders were then
sintered in the temperature range of 11001300 C in order to compare
the microstructures. The microstructures of unsintered (nanopowders)
NiZn ferrite consisted of loosely bound agglomerates with large
amount of open porosity while the SEM micrographs of sintered
(micron-sized) NiZn ferrites revealed densied microstructures consisting of large grains (2 m) and almost devoid of porosity. Room
temperature resistivity of unsintered samples was of the order of
107 cm and it decreased with sintering temperature of the samples.
Unlike other reported methods, we did not observe Zn loss in SEM
micrographs in our samples even at high sintering temperatures that
ensure the quality and homogeneity of our as-synthesized samples.
Room temperature magnetization measurement revealed that the
saturation magnetization of the as-synthesized nanopowders lies in
the range of 3449 emu/g depending upon the composition.
The synthesis methodology reported in this paper is technically
simple and cost effective because starting materials are very cheap
and the method does not require any complex equipment and
complicated operation. The method is versatile and can be utilized to
synthesize different multicomponent ferrite nanopowders.
Acknowledgements
N. N. Ghosh gratefully acknowledges support from DRDO (ERIP/
ER/0605042/M/01/929), India. We also express our thanks to Dr.
Rahul Mohan, NCAOR, Goa, India, for recording SEM micrograph of the
samples.
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