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Effect of Annealing Temperature on Magnetic and Mössbauer Properties of

ZnFe2O4 Nanoparticles by Sol-gel Approach

Article  in  Journal of Superconductivity and Novel Magnetism · October 2018

DOI: 10.1007/s10948-018-4610-2

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Journal of Superconductivity and Novel Magnetism
https://doi.org/10.1007/s10948-018-4610-2

ORIGINAL PAPER

Effect of Annealing Temperature on Magnetic and Mössbauer

Properties of ZnFe2 O4 Nanoparticles by Sol-gel Approach
Md. Amir1,2 · H. Gungunes3 · A. Baykal4 · M. A. Almessiere5 · H. Sözeri6 · I. Ercan7 · M. Sertkol8 · S. Asiri4 ·
A. Manikandan9

Received: 4 February 2018 / Accepted: 13 February 2018

© Springer Science+Business Media, LLC, part of Springer Nature 2018

Abstract
In this study, spinel ZnFe2 O4 nanoparticles (NPs) were synthesized by citrate sol-gel route using nickel nitrates, ferric
nitrates and citric acid by annealing at 900, 1000, and 1100 ◦ C. We reported the structural and magnetic properties (including
Mössbauer analysis) for anisotropy ZnFe2 O4 NPs annealed at different temperatures. Fourier transform infrared (FT-IR)
and X-ray powder diffraction (XRD) were utilized to analyze the structural properties of magnetic nanoparticles (MNPs).
Morphological features of resultant MNPs were examined by scanning electron microscopy (SEM). The observed XRD
results displayed that the crystallite size increased from 38.60 to 49.28 nm with increasing the annealing temperature in
a distinct linear trend. The enhancement of saturation magnetization of the uniaxial ZnFe2 O4 NPs was studied and varied
from 1.28 to 1.66 emu/g as the annealing temperature increases. The Mössbauer spectra results show that ZnFe2 O4 ferrites
were paramagnetic in nature at room temperature (RT).

Keywords ZnFe2 O4 · Spinel ferrite · Annealing temperature · Magnetic properties · Hyperfine interactions

1 Introduction telecommunication and microwave frequency region, etc.

Due to the increasing demand and usage of nanosized mag-
netic ferrite materials, they are perceived as the important
things up to date, and there are reaping benefits owing to
their excellent magnetic, optical, electrical, and catalytic
properties, which provide unique services in various fields
of technology such as medical and industry [1–3]. Neverthe-
less, with fast technological developments of spinel ferrite
materials in magnetic storage devices, recording media,
are creating the large market all over the world [4].
By altering the electrical, optical, and magnetic properties
of the ferrite magnetic materials, the above-mentioned devices
can be developed [5, 6]. Therefore, size of the ferrites, cation
distribution of metal ions, and the temperature of the manufac-
turing process are crucial factors to achieve these goals.
ZnFe2 O4 spinel ferrites are made up of soft transition
metals of Zn2+ ions and Fe3+ ions, where iron(III) occupied
the octahedral site (B site), while zinc ions are placed at

 A. Baykal
abaykal@iau.edu.sa
1 Department of Biochemical Engineering and Biotechnology,
Indian Institute of Technology Delhi, Hauz Khas, New Delhi
110016, India
2 Instrument Design and Development Centre (IDDC),
Indian Institute of Technology Delhi, Hauz Khas,
New Delhi 110016, India
3 8
Department of Physics, Hitit University, Çevre Yolu Bulvarı,
19030 Çorum, Turkey
4 Department of Nano-Medicine Research, Institute for Research
and Medical Consultations (IRMC), Imam Abdulrahman
Bin Faisal University, P.O. Box 1982, Dammam 31441,
Saudi Arabia
5
Department of Physics, College of Science, Imam Abdulrahman
Bin Faisal University, P.O. Box 1982, Dammam 31441,
Saudi Arabia
6 TUBITAK-UME-National Metrology Institute, 41470 Gebze,
Kocaeli, Turkey
7 Department of Biophysics, Institute for Research and Medical
Consultations (IRMC), Imam Abdulrahman Bin Faisal University,
P.O. Box 1982, Dammam 31441, Saudi Arabia
Deanship of Preparatory Year, Imam Abdulrahman
Bin Faisal University, Building 450, P.O. Box 1982,
Dammam 31441, Saudi Arabia
9 Department of Chemistry, Bharath Institute of Higher Education
and Research (BIHER), Bharath University, Chennai, Tamil
Nadu 600073, India

the tetrahedral site (A site). Recently, ZnFe2 O4 NPs are
attracted [7] due to their high magnetic permeability, high
electronic conductivity, excellent phase stability, low eddy
current loss, low cost of production and non-toxicity, etc.
As for example, Shivgurunathan et al prepared ZnFe2 O4
nanomaterials via co-precipitate method and annealed
at three different temperatures for the development of
their magnetic and anisotropy uniaxial properties and
enhancement of surface effect of the temperature-dependent
magnetization of ZnFe2 O4 nanomaterials, respectively [8].
ZnFe2 O4 NPs was prepared by Maalam et al. at 500 ◦ C
temperature through chemical combustion method, and
magnetic properties were developed [9]. Nanostructured
ZnFe2 O4 ferrites with different grain sizes were prepared
by high energy ball milling for various milling times
[10]. Therefore, most of the study discussed the effect of
synthesis type on the magneto-optical properties as well as
on the morphology of the spinel ferrites [11–13]. Herein,
we produced very fine ZnFe2 O4 nanoferrites via cost-
effective sol-gel auto-combustion approach at 900, 1000,
and 1100 ◦ C, and their structures and magnetic properties
were reported.
2 Experiment
2.1 Method of Preparation
ZnFe2 O4 NPs were prepared at 900, 1000, and 1100 ◦ C
via sol-gel combustion approach, and citric acid was
used as fuel and chelating agent. Precursor materials
Fig. 1 Flowchart for the
synthesis of ZnFe2 O4
nanoparticles at different
annealing temperatures
J Supercond Nov Magn
Fe(NO3 )3 ·9H2 O and Zn(NO3 )2 ·6H2 O at 4.04 and 2.97 g
were dissolved completely in 80 ml of distilled water
followed by addition of 2 g of citric acid (C6 H8 O7 ) under
constant stirring. The sol was obtained by using magnetic
stirring to mix the nitrate solution with citric acid until
becoming a transparent solution; pH has been adjusted to
7 by adding drop by drop of ammonia solution to the
mixture. After heating at 80 ◦ C for about 4 h, a gel has been
obtained. The sample was dried for 6 h at 75 ◦ C. Finally, the
synthesized product was pressed into small pellets annealed
at 900, 1000, and 1100 ◦ C for 2 h, respectively. Schematic
presentation of preparation of ZnFe2 O4 NPs at different
annealing temperatures is shown in Fig. 1.
2.2 Materials and Instrumentation
All chemicals such as Fe(NO3 )3 ·9H2 O (purity, ≥ 98%),
Zn(NO3 )2 ·6H2 O (purity, ≥ 98%), citric acid (purity,
≥ 99.5%), and NH3 (purity, 25%, v/v) used in the present
study without further purification were obtained from
Sigma Aldrich. The X-ray diffraction measurements (XRD,
Rigaku D/Max-IIIC with Cu Kα radiation) were conducted
in the 2θ range of 20–70◦ . Fourier transform infrared (FT-
IR, Bruker) spectra have been recorded using a spectrometer
in the range of 4000–400 cm−1 by KBr technique. Scanning
electron microscope (SEM, JEOL JSM-6490) equipped
with EDX was used to characterize the surface morpholo-
gies of the samples. For magnetic measurements, a vibrating
sample magnetometer (VSM) (15 kOe) was used, and the
Mössbauer spectra were recorded at RT using a spectrome-
ter 25mCi 57Co (Rh matrix) as radiation source.
J Supercond Nov Magn

3 Results and Discussion Table 1 Refined structural parameters for ZnFe2 O4 samples with
space group Fd-3m (No. 227)
3.1 Structural Study Sample (◦ C) a (Å) V (Å)3 DXRD (nm) ± 0.05 χ 2 (chi2 ) RBragg

The XRD powder pattern for three different products is 900 8.4364(4) 600.45 38.60 2.45 1.36
presented in Fig. 2. The Bragg reflections indexed to the 1000 8.4387(5) 600.94 46.10 2.95 1.10
standard peaks of single cubic ZnFe2 O4 phase are compared 1100 8.4359(4) 600.34 49.28 2.32 1.13
with ICDD PDF: 22-1012 of the following observed Miller
indices (111), (220), (311), (222), (400), (422), (511),
and (440) matched very well with the spinel structure of
sizes of ZnFe2 O4 NPs of all three samples are given in
ZnFe2 O4 NPs. No intermediate phases or peaks of any
Table 1. Thus, the particle size increases as a result of
species (ZnO or Fe2 O3 ) were observed. These results depict
increasing temperature during calcination process.
the XRD pattern of the single-phase crystal structure of
The reason may be due to the enhancement of
ZnFe2 O4 NPs. The Rietveld analysis results are displayed
coalescence process, which takes place at high annealing
in Table 1. The average crystallite size based on [311] peak
temperatures (900, 1000, and 1100 ◦ C) with respect to time,
was estimated to be in the range of 30 to 49 nm using the
in which grain size of the final products increases [15].
Scherrer’s formula [14].
As can be seen from Table 1, the particle size increases
linearly with the annealing temperature. According to the
0.89λ
L= (1) report, annealing temperature generally decreases the lattice
β cos θ defects and strains. However, it has also been reported
that the effect in the coalescence process of smaller grains
where L, λ, θ , and β are crystallite size, X-ray wavelength, results in the increase in the average grain size of the
Bragg diffraction angle, and full width at half maximum nanoparticles [16].
(FWHM), respectively. The calculated average crystallite

Yobs
1100 °C O
Ycalc
1100 C
(311)

Bragg Pos.
(440)

Transmittance % (a.u.)
(511)
(220)

(400)

(422)
(111)

(222)
Intensity (a. u.)

O
1000 C
1000 °C

900 °C O
900 C

10 20 30 40 50 60 70 4000 3500 3000 2500 2000 1500 1000 500

2 (deg.) Wavenumber (cm )
-1

Fig. 2 XRD patterns with Rietveld analysis patterns for ZnFe2 O4 Fig. 3 FT-IR spectra of ZnFe2 O4 samples obtained at different
samples at different annealing temperatures annealing temperatures

3.2 FT-IR Analysis
To further study the complete formation of spinel ZnFe2 O4
ferrite sample FT-IR spectrum was used. The FT-IR result
of ZnFe2 O4 nanostructure is shown in Fig. 3. The peaks
appeared at ∼ 440 and ∼ 550 cm−1 for all three samples
and can be attributed to the metal oxygen (Zn-O and Fe-O)
bonds [11]. It was noted from the FT-IR data of all samples
prepared at 900, 1000, and 1100 ◦ C that the observed
metallic Fe-O vibrational mode was more prominent and
this clearly concludes that a strong Zn doping exists in the
Fe3 O4 NPs [14].
3.3 Morphological Investigation
Figure 4a–c shows the surface morphology of ZnFe2 O4
nanoferrites at three different temperatures examined by
Fig. 4 HR-SEM images of
ZnFe2 O4 samples obtained at
different annealing temperatures
900°C
1000°C
1100°C
J Supercond Nov Magn
SEM analysis. SEM images clearly observed grains,
which are found to be non-spherical and are distributed
inhomogeneously. Furthermore, the effect of temperature on
the particle morphology is shown in Fig. 4a–c. The increase
of annealing temperatures produced the sharpness of the
peaks in the XRD results. Thus, grain size and crystallinity
increase positively with annealing temperature. Due to
the electrostatic magnetic attraction and sintering effect
at high temperature, individual nanoparticles completely
aggregated and the obtained images showed agglomerated
ferrite particles [15]. The found grain sizes in the range of
30–50 nm are obtained from SEM images.
EDX analysis showed that the weight percentage of
elements in products is in good agreement with that of
theoretical (Table 2). In order to obtain a more accurate
analysis, the elemental mapping micrographs of spinel
ZnFe2 O4 ferrite sample annealed at 900, 1000, and 1100 ◦ C
(a) 900°C
1000°C
(b)
(c) 1100°C
J Supercond Nov Magn

Table 2 Weight and atomic percent composition of the constituent are depicted in Fig. 5. These micrographs indicated the
elements of the ZnFe2 O4 NPs obtained at different annealing temperatures chemical homogeneity of products in terms of distribution of
Sample at Tann (◦ C) Element Weight % Theo. Weight % Exp. Zn, Fe, and O atoms across the grain boundaries (Fig. 5a–c).

900 Fe 46.34 41.36 3.4 Magnetic Properties

O 26.54 26.61
Zn 27.12 32.04 Figure 6 shows the distinctive magnetic properties recorded
1000 Fe 46.34 40.89 for ZnFe2 O4 NPs calcinated at three different temperatures.
O 26.54 34.04 The magnetic studies were carried out using vibrating
Zn 27.12 25.07 sample magnetometer (VSM), and applied magnetic field
1100 Fe 46.34 42.77 (Hc) was plotted against saturation magnetization (Ms)
O 26.54 29.13 at RT [17]. The ZnFe2 O4 bulk material exhibits normal
Zn 27.12 28.10 spinel structure, Fe3+ ions occupy octahedral (B) site,
while Zn2+ prefers tetrahedral (A) site and behaves in
a paramagnetic nature at RT. But, the ZnFe2 O4 NPs

Fig. 5 Electromapping (top) and EDX spectra (bottom) of ZnFe2 O4 samples obtained at different annealing temperatures: a 900, b 1000, and c
1100 ◦ C

Fig. 5 (continued)
exhibit a partly inverse spinel structure, i.e., the Zn2+
and Fe3+ cations occupy both A and B sites. Hence, the
magnetic properties depend on cation distribution, synthesis
technique, particle size, annealing temperature, type of
cations between the interstitial sites, etc. [18]. As depicted in
Fig. 6, ZnFe2 O4 smaller NPs show ferromagnetic behavior:
however, with an increase of annealing temperature, which
tends to be paramagnetic in nature [19]. The Ms value
increased with the reduction of particle size similar to those
results reported in the literature [20]. The ferromagnetic
behavior in ZnFe2 O4 NPs occurs, when the Fe3+ ions
migrate to the A site, giving rise to a strong superexchange
interaction between cations at A and B sites [21]. In
another view, we also notice that with the increase of
particle size, i.e., approaching towards bulk ZnFe2 O4 ,
J Supercond Nov Magn
ferromagnetic behavior tends to be paramagnetic. Some
researchers noticed superparamagnetism for ZnFe2 O4 NPs
due to small grain size (≈ 5 nm) for ZnFe2 O4 NPs under
critical size range [22, 23].
It can be stated that ZnFe2 O4 NPs have no saturation,
which implies a paramagnetic behavior reaching a magneti-
zation of around 1.5 emu/g at 1 T. The coercivity (Hc) values
of NPs vary from 150 to 500 Oe, which is the lowest in the
sample sintered at 1100 ◦ C. Depending on the preparation
method and particle size, various saturation magnetization
values were reported such as 82 emu/g (microwave-assisted
ball milling) [24], 30 emu/g (high-energy ball-milling) [25],
12.0 emu/g (surfactant-assisted hydrothermal method) [26],
24.32 emu/g (ultrasonic cavitation-assisted solvothermal
technique) [27], 60 emu/g (advanced combustion route)
J Supercond Nov Magn
Fig. 5 (continued)
[28], etc. On the other hand, superparamagnetic ZnFe2 O4
NPs having crystallite sizes of 4–12 nm appeared to have
Ms values between 1.6 and 3 emu/g [29].
3.5 Hyperfine Interactions
The RT Mössbauer spectra of ZnFe2 O4 NPs of three
samples at different temperatures are shown in Fig. 7.
Important Mössbauer parameters such as isomer shift,
quadrupole splitting, and variation in line width calculated
from the fitting of the spectra are given in Table 3. The
spectrum composed of three components: a sextet and two
doublets for ZnFe2 O4 sample calcined at 900 ◦ C. The sextet
is related to α-Fe2 O3 phase because of the Mössbauer
parameters which is very close to hematite [30]. This phase
is not detected by the XRD analysis. The doublet with a
lower quadrupole splitting can be assigned to the Fe at B
sites [31]. The isomer shift (IS) and quadrupole splitting
(QS) of the B site are 0.348 and 0.335 mm/s, and the A site
are 0.348 and 0.527 mm/s, respectively. The other samples
compose of only quadrupole doublet. These doublets are
related to ZnFe2 O4 . In all calcined temperature, there is no
detected Fe2+ . Moreover, the sharp doublets is an indication
and fact for iron that it is homogeneously distributed and
thus, unique in its environment [32]. The isomer shift and
QS values are not changed with calcination temperature,
which showed that electron charge distribution of Fe3+ ions
and cubic symmetry are not affected by calcination process.
 J Supercond Nov Magn

Fig. 6 Magnetic hysteresis

loops of ZnFe2 O4 samples
obtained at different annealing
temperatures. The two insets top
and bottom of the figure show
the expanded field region
around the origin for clear
visibility of the readers

Fig. 7 Room temperature Mössbauer spectra of ZnFe2 O4 samples

obtained at different annealing temperatures
Table 3 Mössbauer parameters
for ZnFe2 O4 NPs at different Annealing Assignment IS (± 0.003) QS Bhf (± 0.07) W (± 0.01) RA (%)
annealing temperatures temperature of sites (mm s−1 ) (± 0.006) (T) (mm s−1 )
(◦ C) (mm s−1 )

900 Sextet-: Fe2 O3 0.393 − 0.208 51.951 0.248 2.5016

Db-: Fe+3 (A) 0.348 0.527 – 0.303 28.924
Db-: Fe+3 (B) 0.348 0.335 – 0.289 78.575
1000 Db-: Fe+3 (B) 0.351 0.364 – 0.331 100
1100 Db-: Fe+3 (B) 0.351 0.363 – 0.332 100
J Supercond Nov Magn
4 Conclusion
In conclusion, this study demonstrates the preparation of
spinel ZnFe2 O4 nanoparticles via cost effective and simple
chemical sol-gel autocombustion approach at three different
annealing temperatures. The characteristic peaks of XRD
and FT-IR spectra results confirmed the single crystal
structure of ZnFe2 O4 nanoparticles without any minor
impurities. HR-SEM and EDX analyses show roughly
non-spherical crystal morphology with nanosized particles.
The observed experimental details revealed a significant
effect of annealing temperature of the synthesize route
on the particle size and magnetic properties of spinel
ZnFe2 O4 ferrites. The crystallite size of NPs increased with
increasing annealing temperature in a distinct linear trend.
Moreover, there is an enhancement of the magnetization and
magnetic moment of the uniaxial ZnFe2 O4 nanoparticles.
According to the magnetic hyperfine result, the isomer shift
and QS values are not changed, which showed that electron
charge distribution of Fe3+ ions and cubic symmetry are
not affected by the calcination process. The experimental
evidences signify the promising use of these magnetic
nanoparticles in the development of materials for magnetic
storage devices and portable electrochemical sensor system
and magnetic photocatalyst.
Funding Information Deanship of Scientific Research (DSR) and
Institute for Research and Medical Consultations (IRMC) of Imam
Abdulrahman Bin Faisal University is highly acknowledged for
providing financial assistance for this study (application number
(auto): 2017-605-IRMC).
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