Journal of Magnetism and Magnetic Materials 393 (2015) 5661

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Journal of Magnetism and Magnetic Materials

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

Nanocrystalline Zn1
x Co0.5xNi0.5x Fe2O4 ferrites: Fabrication via coprecipitation route with enhanced magnetic and electrical properties
Amna Hassan a, Muhammad Azhar Khan a, Muhammad Shahid b, M. Asghar a,
Imran Shakir c, Shahzad Naseem d, Saira Riaz d, Muhammad Farooq Warsi b,n
a

Department of Physics, The Islamia University of Bahawalpur, Bahawalpur 63100, Pakistan

Department of Chemistry, The Islamia University of Bahawalpur, Bahawalpur 63100, Pakistan
c
Deanship of Scientic Research, College of Engineering, P.O. Box 800, King Saud University, Riyadh 11421, Saudi Arabia
d
Centre of Excellence in Solid State Physics, University of the Punjab, Lahore 54590, Pakistan
b

art ic l e i nf o
Article history:
Received 7 March 2015
Received in revised form
30 April 2015
Accepted 14 May 2015
Available online 15 May 2015
Keywords:
Spnel ferrites
Nanoparticles
XRD
FTIR
Magnetic parameters

a b s t r a c t
Co and Ni substituted znic ferrite nanoparticles (Zn1
xCo0.5xNi0.5xFe2O4) (0.00rxZ0.75) were synthesized
by co-precipitation method. X-ray diffraction and Fourier transform infrared spectroscopy conrmed the
single phase spinel structure. The lattice constant decreased with the increased Co and Ni contents. The bulk
density was found less as compared to the X-ray density and this difference was explained in terms of
porosity. The crystallite size was calculated by Scherrer's formula and found in the range 2050 nm. Two
prominent stretching bands were observed in FTIR spectra around 400600 cm
1. These two bands conrmed the spinel structure of the prepared nanoparticles. The saturation magnetization was found to increase upto x0.60 from 1.31 emu/g to 81.2 emu/g then it decreased for x0.75 to the value of 75.1 emu/g.
The coercivity and retentivity were found in the range 35.36226.125 Oe and 0.013519.8 emu/g, respectively. Dielectric parameters were decreased with the increased NiCo contents. About nine fold increase in
the DC-electrical resistivity was obtained for the Zn0.25Co0.375Ni0.375Fe2O4 (2.8979  1010 cm) as compared
to the ZnFe2O4 (0.2974  1010 cm) nanoparticles.
& 2015 Elsevier B.V. All rights reserved.

1. Introduction
Nanomaterials are of great interest in today's world due to their
small size and their most important advantage is super miniaturization. Nanomaterials exhibit completely different properties
from there bulk counter parts. Charge storage capacity, magnetic
properties, color and melting point are few characteristic properties of nanoparticles that are sensitive to small size variation in the
nano-scale regime [1]. Nano-ferrites also show extraordinary
properties as compared to the bulk material [2,3]. Nanocrystalline
ferrites with spinel structure are magnetic in nature at room
temperature. Spinel ferrites exhibit remarkable properties owing
to their structural properties, magnetic properties, high electrical
resistivity, low conductivity and low dielectric loss [46]. These
properties of spinel ferrites are inuenced by method used for the
synthesis, chemical composition and cation distribution [5]. These
properties suggest that spinel ferrites are of great importance for
n

Corresponding author. Fax: 92 62 9255474.

E-mail address: farooq.warsi@iub.edu.pk (M. Farooq Warsi).

http://dx.doi.org/10.1016/j.jmmm.2015.05.033
0304-8853/& 2015 Elsevier B.V. All rights reserved.

several advanced technological and electrical applications e.g.

magnetic recording devices, high quality lters, magnetic resonance imaging enhancement, storage devices, microwave devices, power transformers, electric generators etc. [4,6,7]. Many
researchers have already reported the Zn ferrites and substituted
different elements to enhance their magnetic and electrical
properties. For example Malik et al. [8] substituted cobalt, Rashad
et al. [9], Priyadharsini et al. [10] and Shahane et al. [11] doped Ni
and Khan et al. [2] substituted Tb in Zn ferrite. They used different
methods of synthesis such as micro-emulsion, chemical co-precipitation and combustion method and elaborated the effect of
different dopant elements on structural, magnetic and dielectric
properties of Zn ferrites. In the present work we reported the effect of replacement of Zn from ZnFe2O4 with Ni and Co on various
structural and magnetic parameters. The main reason of selection
of Co2 and Ni2 was to improve the magnetic, dielectric and
electrical parameters of ZnFe2O4. Chemical co-precipitation
method was used to obtain the required compositions of NiCo
substituted ZnFe2O4 nanoparticles. Co-precipitation route is facile
and economic. Further it is low temperature technique and involves the aqueous medium [9].

A. Hassan et al. / Journal of Magnetism and Magnetic Materials 393 (2015) 5661

57

2. Experimental
2.1. Materials used
We have used following chemicals as received without any
further purication for the synthesis of nanoparticles of
Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles: Iron(III) nitrate nonhydrate
(Fe(NO3)3  9H2O, 98%, Sigma Aldrich), Zinc nitrate (ZnNO3), 99%,
Sigma Aldrich), Cobalt acetate ((CH3COO)2Co  4H2O), (99%, Sigma
Aldrich), Nickel Chloride (NiCl2  6H2O), Aqueous Ammonia
(NH4OH), 35 wt%, BDH) and Deionised water.
2.2. Synthesis of Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles
Aqueous solutions of the metal ions having molarity 0.125 M
were prepared by dissolving an appropriate amount of corresponding metal salts in deionized water. Aqueous ammonia solution having concentration 2 M was prepared in deionized water.
Required volumes of metal salts solutions having concentrations
0.125 M were mixed in six different beakers. Then the reaction
mixtures was stirred on magnetic stirrers and the temperature
was raised to 5060 C. The pH was raised from acidic media to
basic media by adding freshly prepared aqueous ammonia solution. The pH of all the reaction mixtures was maintained 910.
After maintaining the pH the reaction mixtures were further
stirred for 5 h continuously at room temperature. The precipitates
thus formed were washed with the help of deionized water to
reduce the pH to neutral level. The precipitates of all the compositions were dried in oven at 100 C then the dried samples were
grinded to a ne powder and then powdered samples were sintered at 700 C for 7 h. The obtained samples were then characterized by using different techniques.

Fig. 1. XRD patterns of Co and Ni substituted Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles

sintered at 700 C.

3. Results and discussion

3.1. XRD analysis
Fig. 1 shows the XRD spectra of the six samples for x 0.0, 0.15,
0.30, 0.45, 0.60, 0.75 of Zn1
xCo0.5xNi0.5xFe2O4 sintered at 700 C.
For all the samples, the XRD powder patterns were recorded on
Philips X Pert PRO 3040/60 diffractometer by using the Cu K as
radiation source. The XRD data of ZnFe2O4 matched with the
standard pattern (ICSD- 00-001-1109 and ICSD-01-089-1011) of
ZnFe2O4 [12,13]. The main reections were observed at: (220),
(311), (222), (400), (422), (511), (440), (533) hkl values and labeled
[8,9,1114]. All the samples exhibited the maximum intensity at
(311) [9,11,14]. Formation of FCC single phase spinel structure for
all compositions was conrmed by the diffraction patterns. Fig. 2
clearly showed the continuous shift in 2 with increasing Co and
Ni concentration. It is also clear from Fig. 2 that the angle shifts
towards higher values. This shift is attributed to decrease in lattice
parameter [15]. The lattice constant (a) was calculated by using the
cell software and further conrmed by following relation.

1
h2 + k 2 + l2
=
2
d
a2

(1)

Where d is the inter-atomic spacing and a is the lattice constant.

The results obtained from cell software and above relation were
same and are given in Table 1.The lattice parameter decreased
with the increase in Ni and Co concentration that is justied by the
substitution of relatively larger ionic radius (0.82 ) Zn2 ions
with smaller ionic radius Co2 (0.74 ) [6,8,16,17] and Ni2
(0.69 ) [16,18,19]. As the ionic radii of Co2 and Ni2 is smaller as
compared with that of Zn2 therefore the substitution of Co2

Fig. 2. Shift in 2 with increasing Co and Ni concentration.

and Ni2 in place of Zn2 attributed to the decrease in lattice

parameter [15,2024].The X-ray density for all compositions is
calculated using the following relation [25,26] (Table 1).

X ray =

ZM
NAVcell

(2)

where X-ray is the X-ray density, M is the molar mass, NA is the

Avogadro number and Vcell is the volume of unit cell. The X-ray
density also decreased with increased Co and Ni contents. Mass
density/bulk density was determined by mass and volume [25,27]
by the following relation.

m =

m
r 2h

(3)

where m is the bulk density m is the mass of the pellet r is the

radius of the pellet and h is the thickness of the pellet. Table 1
showed that the values of X-ray density are higher as compared to
those of bulk density. This result indicated the presence of pores in
the samples. Further it was conrmed by calculating the porosity.

58

A. Hassan et al. / Journal of Magnetism and Magnetic Materials 393 (2015) 5661

Table 1
Lattice constant, cell volume, X-ray density, bulk density, porosity and crystallite size of Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles.
Compositions

Lattice constant ()

Volume (3)

X-ray density (g cm
3)

Bulk density (g cm
3)

Porosity

Crystallite size (nm)

ZnCo0Ni0Fe2O4
Zn0.85Co0.075Ni0.075Fe2O4
Zn0.7Co0.15Ni0.15Fe2O4
Zn0.55Co0.225Ni0.225Fe2O4
Zn0.4Co0.3Ni0.3Fe2O4
Zn0.25Co0.375Ni0.375Fe2O4

8.4194
8.4125
8.4044
8.3974
8.3904
8.3834

596.86
595.35
593.69
592.20
590.72
589.24

5.3658
5.3582
5.35295
5.3456
5.3381
5.3306

3.2934
2.7193
2.9317
2.8604
2.8010
2.8430

38.620
49.248
45.231
46.489
47.528
46.667

26.44
35.52
48.16
39.22
27.87
22.384

The percentage porosity of the samples was determined by the

following relation [25,27].

1
x
P =
100
m

(4)

where P, x and m are the porosity, X-ray density and bulk

density respectively.
Crystallite size was determined by using sherrer formula.

D=

K
cos

(5)

where D is crystallite size is wavelength of X-rays, is the full

width at half maxima, is Braggs angle and K is the constant
(with value 0.9). Table 1 show that the crystallite size varies
between 20 and 50 nm. XRD results showed that the lattice
constant, cell volume and X-ray density decreased with the
increased Co and Ni concentration in Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles that is in agreement with the theoretical predictions.
Literature reveals that the crystallite size less than 50 nm is
suitable to get excellent signal-to-noise ratio in switching applications [28].
3.2. FTIR spectroscopy
Fig. 2 shows the FTIR spectra of Zn1
xCo0.5xNi0.5xFe2O4 nanoferrites for x 0.0 and 0.45. These spectra were recorded in the
range of 400700 cm
1 at room temperature. The FTIR data provides the information about positions taken by ions in the crystal
[2], reaction completion and distribution of cations in spinel
structure [6]. The characteristic vibrations of the crystal lattice
show the bands in the range of 300700 cm
1[29]. The two
samples show the characteristic bands of spinel ferrites around
400 cm
1 and 600 cm
1 which conrmed the single phase cubic
spinel structure [6]. The stretching bands (2) at higher frequency
show the vibration of octahedral site and bands at lower frequency
show the vibration of tetrahedral site [30]. Table 2 shows the vibrational frequencies of two prominent IR bands corresponding to
tetrahedral and octahedral sites. These bands shifted with the
substitution of Ni2 ions and Co2 ions in place of Zn2 ions
(Fig. 3). The position of bands in FTIR conrmed the formation of
ferrite structure i.e. spinel structure [10,19,31,32].

Fig. 3. FTIR spectra for Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles (x 0.0, 0.45).

saturated at higher eld values and these are the characteristics of

ferromagnetic materials [8]. The soft magnetic nature of these
spinel ferrites is conrmed by the narrow curves or low values of
coercivity [6,18]. Table 3 shows the values of different magnetic
parameters i.e. retentivity, coercivity, saturation magnetization
and magnetic moment. The magnetic moment is calculated by
using the following relation [33].

B =

M MS
5585

where M is the molar mass and Ms is the saturation

3.3. Magnetic analysis

The hysteresis loops for all compositions are shown in Fig. 4. It
is clear from the gure that the hysteresis loops are S shaped and
Table 2
FTIR transmittance bands for Zn1
xCo0.5xNi0.5xFe2O4 nano-ferrites sintered at
700 C
Samples

v1 (cm
1)

v2 (cm
1)

x 0.0
x 0.45

509.116, 617.19
524.544, 617.64

424.26, 470.54
431.9776, 478.26

(6)

Fig. 4. Magnetic hysteresis loops for Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles.

A. Hassan et al. / Journal of Magnetism and Magnetic Materials 393 (2015) 5661

59

Table 3
Values of coercivity, retentivity, saturation magnetization and magnetic moment for Zn1
xCo0.5xNi0.5xFe2O4
Compositions

Coercivity Hc (kOe)

Retentivity Mr (emu/g)

Magnetization Ms (emu/g)

Magnetic moment (B)

ZnCo0Ni0Fe2O4
Zn0.85Co0.075Ni0.075Fe2O4
Zn0.7Co0.15Ni0.15Fe2O4
Zn0.55Co0.225Ni0.225Fe2O4
Zn0.4Co0.3Ni0.3Fe2O4
Zn0.25Co0.375Ni0.375Fe2O4

0.040413
0.03536
0.049827
0.10413
0.15567
0.226125

1.35  10
2
5.32  10
2
7.86  10
1
6.48
1.49  101
1.98  101

1.31
4.52
2.61  101
5.22  101
8.12  101
7.51  101

0.0566
0.1944
1.1171
2.2285
3.4515
3.1764

magnetization and B is the magnetic moment. Super exchange

mechanism of the metal ions over A-site and B-site in the spinel
structure of ferrites is the reason of magnetic order. In Zinc ferrite
(ZnFe2O4), Zn2 prefers the tetrahedral site i.e. A-site while Fe3
prefers to occupy the octahedral site. However the CoFe2O4 adopts
the inverse spinel structure i.e. Co2 prefers the octahedral site (Bsite) while Fe3 equally distributes itself between octahedral and
tetrahedral sites [6,8]. Similarly the NiFe2O4 also shows inverse
spinel structure i.e. most of the Ni2 take the octahedral site and
Fe3 occupy both tetrahedral and octahedral site [5,34]. So the
magnetic properties depend upon the type of cations and their
distribution between the two interstitial sites and this cationic
distribution depends upon the method used for synthesis and the
ionic radius of the cations. According to Neel's two sub-lattice
model, the magnetic moment per formula unit can be evaluated
by nding the difference of the magnetic moment of the two sublattices i.e.

M = MA MB

(7)

where MA is the magnetic moment of A-sub-lattice and MB is

magnetic moment of B-sub-lattice. Table 3 shows the values of
different magnetic parameters i.e. coercivity, retentivity, saturation
magnetization and magnetic moment. The improvement in magnetic properties may be attributed to the large magnetic moments
of the Co and Ni i.e. 3 B and 2 B [5] respectively as compared to
Zn which is diamagnetic (zero magnetic moment). Fig. 5 shows the
variation in coercivity, retentivity and saturation magnetization by
increasing Co and Ni concentration. It also shows that the saturation magnetization increased up to x 0.60 then decreased for
x 0.75. This is attributed to the migration of Fe3 from octahedral
site to tetrahedral site. The values of saturation magnetization vary
between 1.31 and 81.2 emu/g and the retentivity ranges from
0.0135 emu/g to 19.8 emu/g. It is observed that the values of
coercivity are smaller and varies between 35.36 Oe and

226.125 Oe. Smaller values of coercivity are useful for switching

applications [18].
3.4. Dielectric properties
Dielectric constant was measured for all compositions of
Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles in the range of frequency of
alternating current up to 3 GHz. The dielectric constant of was
evaluated by using the formula [35].

cd
0A

(8)

As pellets were prepared to determine the dielectric parameters so here c is the capacitence of the pellet, d is the thickness of pellet 0 is the permitivity of free space and A is the
cross-sectional area of the pellet. According to MaxwellWagner
interfacial polarization and Koop's phenomenological theory, the
structure of dielectric is composed of two types of layers. One is
composed of a ne conducting material that is ferrite grains. It is
separated by one more thin layer that is composed of grain
boundries. These grain boundries are poor conducting material
[36]. The dielectric constant curves for all samples against frequency is shown in Fig. 6. The gure clearly shows that the dielectric constant decreased with the increase in frequency (for all
the samples). This decrease in dielectric constant is rapid for small
frequency region however for further increase in frequency it
becomes almost invarient with some resonance peaks. The resonance peaks were observed at higher frequencies due to
matching of the electron hopping frequency with ac-current frequency. There is electron hoping between Fe2 and Fe3 ions. The
local displacement of electrons along the direction of applied eld
is due to the exchange of electrons between Fe2 2Fe3 . As the
frequency increased the polarization decreased. Resonance is
produced at higher frequencies when the applied frequency of the
electric eld matches with the jump frequency of electrons between Fe2 and Fe3 and then peaks are observed [37,38]. The
materials which have high conductivity they usually have high
dielectric losses and which have low conductivity they usually
have low dielectric losses [2]. According to Maxwellwagner theory the two dielectric parameters i.e. dielectric constant and tan
have inverse relation with frequency [39]. As very low values of
dielectric constants were observed for these samples which make
them appropriate to use them at higher frequency [40].
3.5. Electrical resistivity
The
DC-electrical
resistivity
for
all
samples
of
Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles was measured using two probe
station which has Keithley-6487 source meter at room temperature.
The electrical was evaluated by following relation [30].

A
(9)
L
where R is the resistance calculated from IV characteristics, L is
the thickness of the pellet and A is the cross-sectional area of the
=R

Fig. 5. Variations in coercivity, retentivity and saturation magnetization with increasing concentration of Co and Ni.

60

A. Hassan et al. / Journal of Magnetism and Magnetic Materials 393 (2015) 5661

Table 4
Resistivity of Zn1
xCo0.5xNi0.5xFe2O4 nano-ferrites sintered at 700 C.
Compositions

Resistivity (ohm-cm)

ZnCo0Ni0Fe2O4
Zn0.85Co0.075Ni0.075Fe2O4
Zn0.7Co0.15Ni0.15Fe2O4
Zn0.55Co0.225Ni0.225Fe2O4
Zn0.4Co0.3Ni0.3Fe2O4
Zn0.25Co0.375Ni0.375Fe2O4

0.2974  1010
2.0329  1010
2.1809  1010
2.3450  1010
2.6781  1010
2.8979  1010

of these nanoparticles.

Acknowledgment
Authors are thankful to the Higher Education Commission of
Pakistan for nancial support under project no: 2913/R&D/HEC.

Fig. 6. Dielectric constant of Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles as a function of

frequency.

pellet. Fig. 7 and Table 4 show the dc-resistivity values and their
trend against the NiCo contents in Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles. The ZnFe2O4 nanoparticles showed relatively low resistivity, which was enhanced by the replacement of Zn with Ni and
Co contents. The high resistivity materials are important for
advanced technological applications.

4. Conclusion
In the present study Zn1
xCo0.5xNi0.5xFe2O4 nanoparticles were
synthesized by co-precipitation method. Single phase cubic spinel
structure was conrmed by XRD and FTIR. The lattice constant
decreased by the increased NiCo contents. The crystallite size
found in the range between 20 and 50 nm. Saturation magnetization increased upto x 0.60 and then decreased for x 0.75. The
saturation magnetization varied between 1.31 and 81.2 emu/g.
Coercivity and retentivity found to vary between 35.36 and
226.125 Oe and from 0.0135 to 19.8 emu/g, respectively. The decreased dielectric constant and increased DC-resistivity by the
replacement of Zn with NiCo exhibit the promising applications

Fig. 7. Effect of NiCo on DC-electrical resistivity of ZnFe2O4 nanoparticles.

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