Journal of Magnetism and Magnetic Materials 398 (2016) 2025

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Journal of Magnetism and Magnetic Materials

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

Effect of zinc concentration on the structural and magnetic properties

of mixed CoZn ferrites nanoparticles synthesized by sol/gel method
M. Ben Ali a,b,n, K. El Maalam a,b, H. El Moussaoui a, O. Mounkachi a, M. Hamedoun a,nn,
R. Masrour d, E.K. Hlil c, A. Benyoussef a,b
a

MAScIR Foundation, Institute of Nanomaterials and Nanotechnologies, Materials & Nanomaterials Center, B.P., 10100 Rabat, Morocco
Laboratory of Magnetism and the Physics of the high Energies, URAC 12, Department of Physics, B.P. 1014, Faculty of Science, Mohammed V University,
Rabat, Morocco
c
Institut Nel, CNRS-UJF, B.P. 166, 38042 Grenoble Cedex, France
d
Laboratory of Materials, Processes, Environment and Quality, Cady Ayyed University, National School of Applied Sciences, PB 63 46000, Sa, Morocco
b

art ic l e i nf o

a b s t r a c t

Article history:
Received 21 April 2015
Received in revised form
20 June 2015
Accepted 23 August 2015
Available online 25 August 2015

Synthesization of zinc-substituted cobalt ferrites nano-particles Co1
xZnxFe2O4 (x 0.00.3) has been
achieved by the sol/gel method. The characterization of the synthesized nano-particles has been done by
X-ray diffractometry (XRD), transmission electron microscopy (TEM) and Fourier transform infrared
spectroscopy (FITR). The relation between the composition and magnetic properties has been investigated by Magnetic Properties Measurement System (MPMS). The results revealed that the nanoparticles size is in the range of 1128 nm. It was found that the zinc substitution in cobalt ferrite increases saturation magnetization from 60.92 emu/g (x 0) to 74.67 emu/g (x 0.3). Nevertheless, zinc
concentrations cause a signicant decrease in coercivity.

Keywords:
Magnetic properties
Mixed ferrites
Sol/gel method

& 2015 Elsevier B.V. All rights reserved.

1. Introduction

Corresponding author at: MAScIR Foundation, Institute of Nanomaterials and

Nanotechnologies, Materials & Nanomaterials Center, B.P., 10100 Rabat, Morocco.
nn
Corresponding author.
E-mail addresses: m.benali06@gmail.com (M. Ben Ali),
m.hamedoun@mascir.com (M. Hamedoun).
http://dx.doi.org/10.1016/j.jmmm.2015.08.097
0304-8853/& 2015 Elsevier B.V. All rights reserved.

Magnetic nano-particles are of great technological importance

because of their use in various hi-tech applications. Spinel ferrites
(AB2O4; a tetrahedral and B octahedral sites) are one of the most interesting Magnetic nano-particles because of their applications in
various elds, such as high-frequency systems, electronic circuits,

M. Ben Ali et al. / Journal of Magnetism and Magnetic Materials 398 (2016) 2025

power delivering devices, electromagnetic interference suppression,

and in biotechnology [1]. In recent years, cobalt ferrite (CoFe2O4) is
largely studied in the search for improved properties and new applications; this is due to its high coercitivity, moderate saturation magnetizations and large magnetostrictive coefcient [24]. These properties make it a very promising magnetic material for a variety of
applications in new technological areas, such as magnetic drug delivery, hyperthermia treatment, microwave device and high-density
information storage [57]. Several preparation techniques have been
used for the synthesis of ferrites nano-particles, which exhibit novel
properties. Gyergyek et al. [8] has reported the synthesis method effect
on particles sizes and magnetic properties in Cobalt ferrite using three
different techniques: co-precipitation, microemulsion method and
thermal decomposition. The results show a signicant variation of
saturation magnetization and coercitivity. The magnetic properties can
be modied either by varying the size of the nano-particles [9], or by
tuning the concentration of magnetic phases in this ferrite [1013]. In
this context, Zinc substituted mixed ferrites is widely treated by several authors, Veena Gopalan et al. [14] have reported a study on Mn
Zn mixed ferrite and found that the magnetization decreases with zinc
substitution and have supposed an existence of a metastable cation
distribution with possible surface effects. Sanjeev Kumar et al. [15]
have synthesized NiZn ferrite by the inverse microemulsion technique and found changes in magnetic behavior due to cation distribution and interparticles interactions.
In this work, we have synthesized Co1
xZnxFe2O4 (x0, 0.05, 0.1,
0.2 and 0.3) using a sol/gel process. The obtained nanoparticles have
many potential applications, including their use for the preparation of
ferrouid, for the energy conversion application utilizing the magnetically induced convection for thermal dissipation. The effect of zinc

21

substitution on the structure and magnetic properties of mixed CoZn

ferrite has been investigated by diffraction XRD, transmission electron
microscopy (TEM), and superconducting quantum interference device
(SQUID). All results will be presented and discussed.

2. Experiments
Iron(III) nitrate nonahydrate (Fe(NO3)3, H2O), Cobalt(II) nitrate
hexahydrate (Co(NO3)2, 6H2O), Zinc(II) nitrate hexahydrate (Zn(NO3)2,
6H2O), citric acid and ethanol were the precursors used to synthesize
Co1
xZnxFe2O4. The chemicals were all of analytical reagent grade
or equivalent and they were used as received without further
purication.
The samples were prepared according to the sol/gel route. Initially, a stoichiometric amount of nitrate precursors were dissolved in 50 ml of ethanol under constants stirring at room temperature for 30 min, an amount of citric acid (stabilizing agent) is
added into the reactive mixture with maintaining a molar ratio of
1:2 between metal nitrates and citric acid. The solution was then
sonicated using an ultrasonic processor for 60 min at a temperature of 60 C; the solution was thereafter heated to evaporate the
solvent excess, concentrated and transformed into a gel. Finally,
the samples were calcined at a temperature of 400 C for 6 h.
All samples were analyzed by X-ray diffraction (Model: D8
Discover Bruker AXS) using Cu K radiation (Cu 1.5407 ). The
magnetic properties of the samples were studied in by Magnetic
Properties Measurement System (MPMS-7XL), with a Quantum
Design XL-SQUID magnetometer. The morphology and particle
size of the as prepared samples were determined by transmission
1,6

100

2,0

100

1,5

80

1,4

0,5
40
0,0

1,0
0,8

60
0,6
0,4

40

0,2
0,0

20

-0,2

20
200

300

400

500

600

100

700

200

300

Temperature (C)

400

500

Temperature (C)
1,0

100
0,8

80

0,6

0,4

60

0,2
40

Deriv. Weight (%/C)

100

0,0
20
200

400

600

800

Temperature (C)
Fig. 1. Thermogravimetric analysis for Co1
xZnxFe2O4 (x 0.0, 0.2 and 0.3).

600

700

Deriv. Weight (%/C)

60

Weight (%)

1,0

Weight (%)

Weight (%)

80

Deriv. Weight (%/C)

1,2

22

M. Ben Ali et al. / Journal of Magnetism and Magnetic Materials 398 (2016) 2025

511

400

14000

440

311

3. Results and discussion

220

16000

intensity

12000
10000
8000
6000
4000
2000
0
20

30

40

50

60

70

2
Fig. 2. X-ray diffraction patterns of Co1
xZnxFe2O4 samples sintered at 400 C with
x varied from 0.0 to 0.3.
Table 1
The values of lattice constant, particles sizes and IR absorption bands (1,2) of
Co1
xZnxFe2O4 (x 0; 0.1; 0.2) samples at room temperature.
Composition

Lattice const ()

DXRD (nm)

1 (cm
1)

2 (cm
1)

CoFe2O4
Co0.95Zn0.05Fe2O4
Co0.9Zn0.1Fe2O4
Co0.8Zn0.2Fe2O4
Co0.7Zn0.3Fe2O4

8.497
8.477
8.468
8.522
8.521

11.7
21.3
23.7
22.1
28.5

540.3
550.0
545.2
548.4
542.0

323.4
330.7
318.7
331.2
300.8

electron microscopy (TEM) observations with an accelerating

voltage of 200 kV. The infrared ABB-Bomen FTLA 2000 was performed over the range 4000250 cm
1.

Thermogravimetric Analysis (TG/DTA, TA InstrumentsPfeiffer

Vacuum) equipment was used to determine the thermal decomposition and weight loss of the precursor powder, by varying the
temperature from 25 C up to 800 C with a heating rate of 10 C/
min. Fig. 1 shows the TGA curve. The rst weight loss step is in the
temperature range of 150230 C. It corresponds to the decomposition of acetates [16]; and the exothermic peak at 300350 C
in the DTA curve is presumed to be associated with the crystallization of spinel phase. In order to have comparable samples we
decided to anneal all the samples at a temperature of 400 C.
X-ray diffraction of cobalt zinc ferrite samples with x 0; 0.05,
0.1, 0.2 and 0.3 are shown in Fig. 2, the patterns reveal the presence of peaks characteristic of the cubic phase of spinel ferrite in
all samples, the observed diffraction peaks perfectly match with
those of CoFe2O4 (JCPDS Card no 22-1086). The absence of any
additional peaks related to impurities indicates the high purity of
our samples. The lattice parameter was calculated using the following relations,

a = [d2 h2 + k 2 + l2 ]2

The lattice constant was found in the range of 8.498.52 (Table 1). The values of lattice parameters change with zinc concentration, this behavior could be attributed to the substitution of
Co cation (of radius 0.75 ) by a larger cation which is Zn2 (of
radius 0.82 ) [17,18]. A similar type of variation is also observed
in the case of Cu1
xZnxFe2O4 [19] where the lattice parameter
increases with increasing Zinc content. The particles size was
calculated from the most intense peak 311 using the well known
Scherrer formula [20].

DDRX =

0.9
cos

where is the wavelength (Cu Ka), is the full width to halfmaximum (FWHM) of line broadening and is the Bragg angle of
diffraction. The particles size calculated are listed in Table 1, the
particles sizes of the prepared samples were obtained between 11

Fig. 3. TEM image of (a) CoFe2O4, (b) Co0.9Zn0.1Fe2O4, (c) Co0.8Zn0.2Fe2O4, (d) Co0.7Zn0.2Fe2O4, samples.

M. Ben Ali et al. / Journal of Magnetism and Magnetic Materials 398 (2016) 2025

23

70

70
60

60

number of particles

number of particles

50
40
30

50
40
30

20

20

10

10

0
0

10

20

30

40

10

15

20

grain size (nm)

25

30

35

40

45

grain size (nm)

60
40

50

35
30

number of particles

number of particles

40

30

20

25
20
15
10

10
5
0

0
0

10

20

30

40

grain size (nm)

10

20

30

40

50

60

70

grain size (nm)

Fig. 4. Curve of grain size distribution of (a) CoFe2O4, (b) Co0.9Zn0.1Fe2O4, (c) Co0.8Zn0.2Fe2O4, (d) Co0.7Zn0.2Fe2O4, samples.

and 28 nm.
To reveal the local microstructure of the particles, Transmission
electron microscopy analysis was carried out. Fig. 3 present the
results for Co1
xZnxFe2O4 samples with x 0, 0.1, 0.2 and 0.3. The
image reveals that particles are in nanometer range with spherical
shape and good dispersion. The particles sizes have been estimated using Image analysis algorithm (Fig. 4), the tted curve
indicates the presence of a population of particles centered around
17, 20, 16 and 30 nm for CoFe2O4, Co0.9Zn0.1Fe2O4, Co0.8Zn0.2Fe2O4,
and Co0.7Zn0.2Fe2O4, respectively. These values are in good agreement with the size obtained from the DRX patterns.
The FTIR analysis was performed at room temperature in the
range of 2503000 cm
1 for detecting chemical bonds present in
the samples and ensuring the formation of ferrite phase.
Generally, there are two main characteristic absorption peaks
in FTIR spectra of the spinel ferrites, which are related to intrinsic
stretching-vibrations of the oxygen bonds with metal cations in
positions A and B [21,22]. Where The rst band in the range of
500650 cm
1 corresponds to the stretching vibrations of the
metal at the tetrahedral site (M[4]2O). The other band appeared
around 300450 cm
1 is attributed to the octahedral-metal
stretching (M[6]2MO).
The infrared spectra of all the mixed cobaltzinc ferrites are

shown in Fig. 5. It can be seen from the gures that the IR spectrum of mixed cobaltzinc ferrites exhibit the two expected bands
in a spinel structure, 1 with the higher wavenumber observed in
the range of 540550 cm
1 and 2 with lower wavenumber observed in the range of 300300 cm
1. The band positions of the
investigated samples are tabulated in Table 1. It is clear from Table 1, that the frequency band shift with the variation of Zinc
concentration, this may be due to the re-distribution of cations;
Co, Fe and Zn on both sites [15]. The same observation has been
made by Azhar Khan et al. [23] in the case of cobalt doped
terbium.
Cobalt ferrite exhibits a hard magnetic behavior [24] with a
relatively high coercivity and high magnetization [2]. However,
magnetic properties of this spinel ferrite depend strongly on the
particle size [25,26], cation distribution [27] and doping [28].
In our work, the magnetic measurement of mixed Co1
xZnxFe2O4
nanoparticles, with varied x from 0 to 0.3, was done by Magnetic
Properties Measurement System. The hysteresis loops at 300 K for
these samples are shown in Fig. 6. The saturation magnetization (Ms)
was obtained from hysteresis loop at H60000 Oe. The positive remanent magnetization (Mr) was obtained from hysteresis loop at
H0 Oe. The coercivity eld was obtained from hysteresis loop at
M0. The saturation magnetization (Ms), remanent magnetization

24

M. Ben Ali et al. / Journal of Magnetism and Magnetic Materials 398 (2016) 2025

Table 3
Values of the coercitif eld (Hc) of CoFe2O4 by several synthesis methods.

100

Intensity

80

60

Synthesis method

Hc (Oe)

Reference

Co-precipitation
Co-precipitation
Co-precipitation in reverse microemulsion
Thermal decomposition
Combustion
Sol/gel (citrate method)

800
850
700
1900
2002
2000

[8]
[30]
[8]
[8]
[30]
This work

80

2250

40

2000
75
1750
70

0
800

700

600

500

400

300

1500
1250

65
1000
60

Hc (Oe)

Ms (emu/g)

20

750

-1

500

Wavenumber (cm )

55

Fig. 5. FTIR band of Co1
xZnxFe2O4 ferrite nanocrystals with x varied from 0.0 to
0.3.

250
50

0,00

0,05

0,10

0,15

0,20

0,25

0,30

x
80

Fig. 7. Variation of magnetization and Hc values with zinc concentration.

60

M(emu/g)

40
20
0
-20
-40
-60
-80
-6

-5

-4

-3

-2

-1

H (T)
Fig. 6. Room temperature magnetization cures of Co1
xZnxFe2O4 samples sintered
at 400 C with x varied from 0.0 to 0.3.

Table 2
The values of the saturation magnetization (Ms) and the coercitif eld (Hc) for each
sample.
Composition

Ms (emu/g)

Hc (Oe)

CoFe2O4
Co0.95Zn0.05Fe2O4
Co0.9Zn0.1Fe2O4
Co0.8Zn0.2Fe2O4
Co0.7Zn0.3Fe2O4

60.92
63.99
68.01
72.17
74.67

2000
1600
800
220
170

(Mr) and coercivity (Hc) are listed in Table 2.

The hysteresis curves show that for the undoped cobalt ferrite
the coercivity is about 2000 Oe, this value may be due to the high
anisotropy constant of the Cobalt ferrite (Table 3) [29]. However,
several authors associate the high value of coercitivity to the

synthesis method. In the studies of Saso Gyergyek et al. [8], the

coercitivity value varies from 700 to 1900 Oe by changing the
synthesis method, according to the authors this variation is attributed to the difference of cation distribution in the samples.
Similar studies were reported by Houshiar et al. [30]. It was also
observed that the value of coercivity shows a signicant decrease
from 2000 Oe to 170 Oe with increasing the zinc substitution, the
decrease in coercivity with zinc concentration is reported in Fig. 7.
This variation can be attributed to the reduction of domain wall
energy caused by the weak magnetocrystalline anisotropy of the
zinc [31].
The saturation magnetization (Ms) for x 0 is about 60,92 emu/
g with an average grain size of 11.7, while the value reported in the
literature for bulk sample is about 81 emu/g [32]. However, the
substitution of cobalt by zinc shows an increase in saturation
magnetization up to reach 74.67 emu/g for x 0.3 (Fig. 7). According to Blanco-Gutierrez et al. [33], the bulk ZnFe2O4 has an
antiferromagnetic behavior with normal spinel structure
(Zn2 )Td[Fe3 Fe3 ]OhO24
in which all the Zn2 cations are located in tetrahedral sites (A) and Fe3 cations are in octahedral
sites (B) with antiparallel moments. Thereby the substitution of
nonmagnetic ion which has a preferential A site occupancy results
in the reduction of the exchange interaction between A and B sites.
Hence by varying the degree of zinc substitution it is possible to
vary magnetic properties of the ne particles.
Similar studies were reported by Nandapure et al. [10] in the
case of ZnNi mixed ferrite, were saturation magnetization increases due to the addition of Zn content in NiFe2O4. In this sense,
the substitution of Zn2 ions at tetrahedral sites (A) in place of
Fe3 ions into an inverse cobalt ferrite [34] lead to the decrease of
magnetic moment in tetrahedral A-site. However, A-site magnetic
moment is less than B-site magnetic moment and the net magnetic moment increases up to 74.67 emu/g for x 0.3. However,
the magnetization decreases after a certain zinc concentration due
to Yafet-Kittel arrangement [35]. In this context a lower magnetizations value was reported by Yadav et al. for Co1
xZnxFe2O4

M. Ben Ali et al. / Journal of Magnetism and Magnetic Materials 398 (2016) 2025

with x 0.5 [36].

[16]

4. Conclusions
[17]

Particles of zinc-substituted cobalt ferrites have been successfully prepared by sol/gel methods; the spinel crystalline structure
was veried by DRX, the addition of the zinc does not change the
crystalline phase of the particles and the results matches perfectly
with the standard reported data. Therefore, there are signicant
changes in other physical properties. It was found that the particles size calculated from DRX results were between 1128 nm; and
that the lattice constant varies with zinc concentration. The
coercivity shows a signicant decrease from 2000 Oe to 170 Oe
with increasing the zinc amount while the saturation magnetization increases with the addition of a small concentration of Zinc.

[18]

[19]

[20]

[21]
[22]

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