Journal of Alloys and Compounds 803 (2019) 964e970

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Cd-doping effect on morphologic, structural, magnetic and electrical

properties of Ni0.6-xCdxMg0.4Fe2O4 spinel ferrite (0
x
0.4)
Nejeh Hamdaoui a, b, *, Yashar Azizian-Kalandaragh c, d, Mouadh Khlifi e, Lotfi Beji a, f
a
Laboratoire des Energies et des Materiaux, LabEM-LR11ES34, Ecole Superieure des Sciences et de La Technologie, Universit
e de Sousse, Rue Lamine Abessi,
4011, Hammam Sousse, Tunisia
b
Institut Superieur des Technologies de L'Informatique et de La Communication, Universit
e de Sousse, Gp1, 4011, Hammam Sousse, Tunisia
c
Department of Physics, University of Mohaghegh Ardabili, P.O. Box.179, Ardabil, Iran
d
Department of Engineering Sciences, Sabalan University of Advanced Technologies (SUAT), Namin, Iran
e
Laboratoire de Physique de La Mati ere Condens
ee et des Nanosciences, Facult
e des Sciences de Monastir, 5019, University of Monastir, Tunisia
f

Departement de Physique, Coll ege des Sciences et des Arts D'Ar Rass, Universit

e Qassim, Ar Rass, Saudi Arabia

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

Article history: The effect of Cd-doping on physical properties of Ni0.6-xCdxMg0.4Fe2O4 spinel ferrite has been investi-
Received 29 March 2019 gated. Scanning electron spectroscopy (SEM) confirms the formation of grain and grain boundaries in
Received in revised form these samples and the presence of all chemical elements introduced was confirmed by EDS. The X-ray
26 June 2019
analyses indicate that all the compounds have the cubic structure with Fd3m space group, cell parameter
Accepted 27 June 2019
Available online 28 June 2019
increase which Cd content. A ferromagnetic state at room temperature for all compounds is detected by a
magnetization measurement of hysteresis loops. We note that the saturation magnetization increases
with Cd content, however, the remnant magnetization, and the corrective field decreases. DC electrical
Keywords:
Ferrite
conductivity analysis shows a semiconductor behavior for all sample. In addition, non-overlapping small
Spinel structure polaron tunneling (NSPT) and the overlapping large polaron tunneling (OLPT) are the dominants con-
Magnetic properties ductions mechanisms in our samples.
Electrical conduction mechanisms © 2019 Elsevier B.V. All rights reserved.

1. Introduction between the different crystallographic sites, the difference in ionic

Spinel ferrites)AFe2O4(, in which A is a divalent element (Ni, Co,
Mg, Mn) attracted the attention of scientific researchers due to their
interesting magnetic and electrical characteristics for example high
saturation magnetization at room temperature, considerable elec-
trical resistance, flexibility and chemical consistency [1e5]. These
ferrites crystallize generally in a cubic symmetry and at the Curie
temperature exhibit a magnetic transition from ferromagnetic (FM)
to paramagnetic (PM) state that is very dependent on the chemical
composition of materials. These properties give the possibility of a
technologic application using some spinel ferrites such as RF de-
vices, nanoelectronics devices, and high-speed digital data recorder
[6,7]. Structural, magnetic and electric properties of ferrites are
strongly related to the type of cations and their distribution
* Corresponding author. Laboratoire des Energies et des Materiaux, LabEM-

de
LR11ES34, Ecole Superieure des Sciences et de la Technologie, Universite
Sousse, Rue Lamine Abessi, 4011, Hammam Sousse, Tunisia.
E-mail addresses: hamdaoui_nejeh@protonmail.com, hamdaoui_nejeh@yahoo.
fr (N. Hamdaoui).
radius, the elaboration method, heating temperature, the micro-
structure and the chemical composition [8,9]. The dielectric char-
acteristics of spinel ferrites are generally studied by the impedance
spectroscopy technique to examine and distinguish between the
contribution of the bulk particle (grain) and the inter-particle
contact (grain boundaries) in the conduction mechanisms
[10e13]. Among spinel ferrites, Ni1-x Mgx Fe2O4 ferrite has
important uses due to its high electrical resistivity, low coercivity
(i.e. soft ferrite), hardness, chemical stability, and cost-effectiveness
that made more enthusiasm to manufacture ferrite materials at a
large scale for industrial applications. The Ni1-x Mgx Fe2O4 ferrites
are also popular for its high-frequency application and magneto-
dielectric properties especially in microwave and radio frequency
region [14]. It was found that among the various compositions of
Ni1-x Mgx Fe2O4 ferrites, Ni0.6Mg0.4 Fe2O4 has relatively high
electrical-magnetic properties [15]. The Ni1-xMgxFe2O4 composi-
tion has been investigated and reported in several research travels
[16e20]. Therefore, many substitutions are made on NieMg ferrite
compound in order to analyze the substitution effect on the electric
and magnetic properties. Many studies investigated the influences

https://doi.org/10.1016/j.jallcom.2019.06.339
0925-8388/© 2019 Elsevier B.V. All rights reserved.
 N. Hamdaoui et al. / Journal of Alloys and Compounds 803 (2019) 964e970 965

of magnetic and nonmagnetic ions such as Co2þ, Zn2þ, and Gd3þ, on

structural, magnetic, electric, and dielectric properties of spinel
ferrite system [21e23]. However, to the best of our knowledge,
there is no report available detailed the impact of different pro-
portion of Cd2þ on the structural, magnetic, dielectric, and electrical
properties of Ni0.6-xCdxMg0.4Fe2O4 materials prepared through
the sol-gel method. Many works have been carried out by the
substitution of Cd ion in other spinel structure of ferrite [24,25].
Saha [26] has reported that there is an increase in the dielectric
constant by 3.5 times when cadmium is substituted in NieCo
perminvar ferrite. This prompted us to carry out the present work
to study the effect of cadmium substitution on the properties of
Ni0.6-xCdxMg0.4Fe2O4 ferrite. Also, Muddassar Naeem et al. [16]
have investigated the dielectric, structural, and magnetic properties
of Ni1xMgxFe2O4 ferrite nanoparticle synthesized by chemical
coprecipitation technique. In addition, Hossain et al. [27] have
studied the magnetic characteristics of Mn-substituted nano-
crystalline Ni0.5-xMnxMg0.5Fe2O4 ferrites prepared by a combustion
route.
In this paper, we have interested in the Cd-doped Ni0.6-
xCdxMg0.4Fe2O4 spinel ferrites prepared by sol-gel technique. A
detailed investigation of structural, morphological and magnetic
characteristics of the prepared materials has been analyzed by XRD,
FE-SEM, EDX, and VSM. The dielectric and electrical parameters are
analyzed using complex impedance spectroscopy technique.

2. Experimental details

The sol-gel method was used to prepare Ni0.6-xCdxMg0.4Fe2O4

ferrites by using Ni(NO3)2.6H2O, Cd(NO3)2.4H2O, Mg(NO3)2.6H2O,
and Fe(NO3)3.9H2O nitrates (all chemicals were of 99.99% purity
and purchased from Sigma Aldrich). The stoichiometric amount of
nitrates and citric acid were dissolved into distilled water to form a
mixed solution. The pH value was maintained at about 7. The mixed
solution was heated on a hot plate under regular stirring at 90  C
followed by the addition of ethylene glycol until a highly viscous gel
formed. The obtained gel was dried in an oven at 250  C for 12 h to
get a porous solid mass, which was ground into powders. Then the
powders were calcined at 600  C (12 h) and 800  C (12 h) respec-
tively. Finally, the powders were pressed into pellets with a diam-
eter of 10 mm and a thickness of about 2 mm and then sintered at
1000  C (24 h). The structural properties are studied using a Philips
X pert, X-ray diffractometer with CuKa1 radiation (l ¼ 1.54 Å). Field
Emission Scanning electron microscopy (FESEM) is employed to
examine the morphological characteristics of the samples and also
EDX analysis was used to check the presence of chemical elements
introduced during the sample preparation using a FESEM, TeScan -
Mira III, Czech Republic. A vibrating sample magnetometer (8600
Series VSM Model lake shore) was employed to study the magnetic
properties of all samples at room temperature. Finally, the electrical
measurements were taken by complex impedance spectroscopy
technique using an N4L-NumetriQ (model PSM1735) in the fre-
quency range of 10 Hz10MHz by varying temperature from room Fig. 1. SEM micrographs for Ni0.6-xCdxMg0.4Fe2O4 for x ¼ 0.00; x ¼ 0.20 and x ¼ 0.40
temperature to 440 K using lake shore model 335 cryogenic tem- samples and their corresponding EDX spectra.
perature controller.

3. Results and discussions
3.1. FESEM and EDX analysis
Fig. 1 shows the FESEM micrograph of Ni0.6-xCdxMg0.4Fe2O4
samples, we can see that all samples are formed by grains and grain
boundary, which reveals a good grain growth during the heat
process. The grains have a polygonal form with average grain size,
which decreases from DSEM ¼ 1 mm to DSEM ¼ 0.3 mm when Cd-
content increases from 0 to 0.4. In addition, the EDX spectra
reveal the presence of all chemical elements (Cd, Ni, Mg, Fe, and O)
introduced along with the elaboration of Ni0.6-xCdxMg0.4Fe2O4
samples, confirming that there is no loss of any integrated element
after the heating process.
3.2. XRD analysis
X-ray diffraction (XRD) analysis is performed to study the
966 N. Hamdaoui et al. / Journal of Alloys and Compounds 803 (2019) 964e970

structural properties. The X-ray pattern (Fig. 2) depicts a super-

position of all the peaks characteristic of all samples, which proves
that they crystallize in the same structure. Rietveld's method is
applied via Fullprof program [28] in order to analyze the data of the
XRD pattern. Fig. 3 depicts the XRD peaks of the studied samples,
we note the presence of very fine peaks confirming the good
crystalline quality of samples. Then, the absence of supplementary
peaks proves the high purity of the synthesized compounds. Riet-
veld refinement shows that all samples have the cubic structure
with Fd3m space group. Moreover, it is obvious that the cell
parameter “a” and the cell volume increases when Cd-amount in-
creases. This increase is explained by the fact that the Cd2þ radius
rCd2þ ¼ 0.95 Å is larger than the Ni2þ one rNi2þ ¼ 0.69 Å [29]. Struc-
tural parameters are summarized in Table .1. The variation of cell
volume as a function of Cd concentration is displayed in Fig. 4.
Finally, the ferrites spinel (AB2O4) structure is characterized by two
sites type: (A-site) tetrahedral site and the (B-site) octahedral site.
In our case, the Ni2þ ions owing to their high crystal field stabili-
zation select octahedral B-site [30], and the Mg2þ ions will occupy
the tetrahedral A-site, and the Fe3þ ions are placed between both A
and B-sites. So, the distribution of the ions between A and B sites for
A
2þ 3þ 2 B
the x ¼ 0.00 composition is: ½Mg2þ 3þ
0:4 Fe0:6  ½Ni0:6 Fe1:4  O4 (Fig. 5).
2þ
On the other hand, with the presence of Cd ions, the tetrahedral A
site will be occupied by these ions [30,31], and the vacancy pro-
duced by replacement of Mg2þ by Cd2þ ions induce the migration of
Fe3þ ions from tetrahedral to octahedral sites. The new cations
2þ 3þ 2þ A 2 B
positions become ½Mg2þ 3þ
0:4 Cdx Fe0:6x  ½Ni0:6x Fe1:4þx  O4 .

3.3. Magnetic properties

Magnetic measurements of Ni0.6-xCdxMg0.4Fe2O4 materials are

performed at room temperature by the magnetic hysteresis loops
under an applied magnetic field ranging between 104 and 104 Oe
(Fig. 6). We note that the magnetization values increases when Cd
content increase, this behavior is explained by the fact of the in-
crease of cadmium concentration ions, which reduces the amount
of Ni2þ ions and increases the amount of Fe3þ ions in B-site.
The inset of Fig. 6 shows the zoom of the hysteresis loop of
x ¼ 0.40 as an example. At lower fields, the magnetization increases

Fig. 3. X-ray diffraction pattern and the corresponding Rietveld refinement. Observed
(Yobs) and calculated (Ycalc) patterns are compared (blue line) for Ni0.6-
xCdxMg0.4Fe2O4 samples. The vertical ticks show the positions of the calculated Bragg
reflections. (For interpretation of the references to colour in this figure legend, the
reader is referred to the Web version of this article.)

rapidly which then increases slowly at higher fields but does not
reach a complete saturation. This behavior confirms the existence
of FM and AFM phases in our compounds, where the FM phases get
responses quickly at the lower fields while the AFM phase responds
slowly even at higher fields.
In order to determine the values of saturation magnetization
and coercive field, a theoretical analysis was performed by fitting
the hysteresis loops using the following equation:
Fig. 2. X-ray diffraction spectrum for all samples.
 N. Hamdaoui et al. / Journal of Alloys and Compounds 803 (2019) 964e970 967

Table 1
Rietveld-refined parameters.

x 0.0 0.2 0.4

Space groupe Fd3m Fd3m Fd3m

a ¼ b ¼ c (Å) 8.348 8.374 8.397
Unit cell volume (Å3) 581.764 587.217 592.069
2þ 3þ A 0,3750 0,3720 0,3741
½Mg 2þ
0:4 Cdx Fe0:6x 
x¼y¼z
B 0,000 0000 0,000
½Ni2þ 3þ
0:6x Fe1:4þx 
x¼y¼z
O x¼y¼z 0,2431 0,2422 0,2461
Rwp(%) 4.20 5.36 4.34
Rp(%) 5.34 6.68 5.12
RF(%) 2.41 2.37 1.51
c2 (%) 2.73 3.13 2.81

Fig. 6. Magnetic hysteresis loop at room temperature for x ¼ 0.00; x ¼ 0.20 and x ¼ 0.40
samples. The inset present a zoom for low field region.

[32,33]. Here MSFM M RFM , Hci are the FM saturation magnetization,

remnant magnetization, and intrinsic coercive field, respectively.
While c is the AFM susceptibility. The fitted curves with both
contributions are shown in Fig. 6 (sold line). The obtained param-
eters from the adjustment are listed in Table 2. The variation of M RFM
and Hci as a function of Cd content is shown in Fig. 7.

3.4. Dielectric analysis

3.4.1. Conductivity analysis

Fig. 4. Cell parameter as a function of Cd content.
Generally, the transport process in spinel ferrites is governed by
the exchange of electrons between the ions of the same elements
present in more than one valence state and distributed randomly
over equivalent crystallographic lattice sites [34]. Precisely, con-
duction in ferrite is attributed to electrons hopping between Fe3þ to
Fe2þ ions [35] that is to say between octahedral and tetrahedral
sites. The number of such ion pairs depends upon the sintering
conditions and amount of reduction of Fe3þ to Fe2þ at elevated
temperatures. The increase in temperature enhances the hopping
of charge carriers resulting in an increase in the conduction process.
Electrical conductivity measurements of Ni0.6-xCdxMg0.4Fe2O4
are performed in the frequency range varying from 10 Hz to
5 MHz at different temperatures (Fig. 7). It is noted that the con-
ductivity increases as a function of the temperature for a given
frequency, which shows that all the samples exhibit a semi-
conducting behavior. In addition, it is clear that at low-frequency
range (DC), the thermally activated hopping process governs the
conduction mechanism. The conductivity sDC follows the Arrhenius
law according to equation (2):
 
Ea
sDC ¼ s0 exp  (2)
KB T

Fig. 5. The unit cell where the positions of all elements are properly identified. where s0 is a pre-exponential factor, Ea is the activation energy, kB
is the Boltzmann constant, and T is the absolute temperature. In
Fig. 8, we present the evolution of Ln (sDC ) as a function of 1000/T
"  !# for the three compounds. Then, a linear fit of these curves allow us
MSFM H±Hci p  MRFM
MðHÞ ¼ 2 tan1 tan þ cH (1) to determine the activation energy values which is found to be
p Hci 2  MSFM Ea ¼ 0.242 eV, Ea ¼ 0.248 eV, Ea ¼ 0.248 eV for x ¼ 0.00, x ¼ 0.20 and
x ¼ 0.40 samples respectively. These values are close to that found
where the first term is related to the FM contributions and the for another similar ferrite [36]. On the other hand, the frequency-
second one represents the linear contribution from the AFM one dependent conductivity increase with frequency to switch from
968 N. Hamdaoui et al. / Journal of Alloys and Compounds 803 (2019) 964e970

Table 2
Parameters extracted from fitting the hysteresis loops of x ¼ 0.00; x ¼ 0.20 and
x ¼ 0.40 compounds.

M SFM (emu/g) M RFM (emu/g) Hci (Oe) c (105 emu/g.Oe)

x ¼ 0.00 40.12 1.89 18.13 1.032
x ¼ 0.20 42.78 1.02 10.02 1.611
x ¼ 0.40 51.36 0.81 7.49 2.083

Fig. 7. Remnant magnetization Mr and the coercive field H casa function of Cd content.

DC to AC state that is characterized by a conductivity increase along

a specific slope for each contribution. The feature of dispersion of
the conductivity is generally examined by using Jonscher's law [37]
which is defined as:

sAC ¼ sDC þ Aun (3)

where u is the angular frequency, A is a constant related to the

internal properties of material and temperature and n is a
frequency-dependent exponent which describes the degree of
interaction between mobile ions and the environments [38,39].
It is evident from Fig. 7 that the conductivity curve is divided
into three areas (region I, region II and region III). The region I
characterized by a DC plateau is followed by two dispersion regions
(II and III) as frequencies increase. This result reveals the existence
of two relaxations in these systems. The first relaxation is associ-
ated with grain boundaries with large capacitance value. The sec-
ond one acts at high frequencies occurred in grain particles, which
is characterized by a smaller capacitance value [40,41]. We
conclude that typical Jonscher formula (Eq. (3)) cannot elucidate
the behavior of the obtained experimental results with a double
slope.
Therefore, the experimental conductivity has been fitted using a
double power law given by Eq (4).

sAC ¼ sDC þ Aun1 þ Bun2 (4)

The obtained values of n1 and n2 parameter are shown in Fig. 9.
It is well known that the evolution of n parameter with tempera-
ture can explain the charge carrier transport in materials [42]. The
n1value relative to the region II decreases from 0.98 to 1.51 when Fig. 8. Electrical conductivity versus angular frequency at different temperatures from
the temperature increases from 300 K to environ 440 K for all 295 K to 440 K for x ¼ 0.00; x ¼ 0.20 and x ¼ 0.40 samples.
samples. On the other hand, n2 parameter in region III decreases
with the increase of temperature for the three compounds. Based
on the above results, we can deduce that at medium frequencies
the increases of n1 with the temperature confirm that the non-
 N. Hamdaoui et al. / Journal of Alloys and Compounds 803 (2019) 964e970
Fig. 9. Variation of the log(sDC) as a function of (1000/T) for all sample. Red solid line is
the linear fit for our data using SPH model. (For interpretation of the references to
colour in this figure legend, the reader is referred to the Web version of this article.)
Fig. 10. Variation of n1 and n2 parameters versus temperature for x ¼ 0.00; x ¼ 0.20 and
x ¼ 0.40 samples. The inset show the variation of WH and WM versus temperature.
969
overlapping small polaron tunneling (NSPT) mechanism is pre-
dominant in our samples [43]. At high frequencies, the decrease of
n2 with temperature shows that the transport process is governed
by the correlated barrier hopping (CBH) model [44] (see Fig. 10).
For the NSPT model, the n1 parameter can be determined by
equation (5) as [44].
4kB T
n1 ¼ 1 þ   (5)
1
WH  kB TLn ut 0
where WH is the polaron hopping energy, ɷ is the angular fre-
quency, and t0 is the carriers relaxation time. Usually, the values of
the WH/kBT is large, and then the exponent n1 can be defined as
[44]:
4kB T
n1 ¼ 1 þ (6)
WH
The WH values are calculated using equation (6), presented
versus temperature for all samples and shown in the inset of Fig. 9
(a). We note that WH decreases with temperature for all samples
confirming that the number of free carriers will be increased. As a
result, this behavior supports that the sAC increases with the
increasing temperature.
Furthermore, the CBH model suggests that the transport process
arises by single or bipolaron hopping mechanism through the
Coulomb barrier occurred between two trap centers. The binding
energy has been calculated from equation (7) as follow:
6kB T
n1 ¼ 1  (7)
WM  kB TLnðut0 Þ
Then for high values of WM/kBT, the parameter n1 can be
reduced as:
6kB T
n1 ¼ 1  (8)
WM
Experimental data of high-frequency n2 exponent is fitted using
equation (8) and then the deduced WM parameter for all of the
Ni0.6-xCdxMg0.4Fe2O4 samples are presented in Fig. 9 (b).
To approve the occurrence of tow contribution which is asso-
ciated to grains and grain boundaries in the transport process, we
presented the Cole-Cole plot (Z00 vs. Z’) at room temperatures
(Fig. 11). Cole-Cole plot indicates the presence of two semicircular
arcs. A small semicircle at a higher frequency and a large semicircle
at a lower frequency. The presence of these semicircles indicates
the existence of two different relaxation processes attributed to the
grains and grain boundaries, which confirms the results discussed
above.
4. Conclusion
Ni0.6-xCdxMg0.4Fe2O4 ferrite was successfully synthesized using
the sol-gel technique. Rietveld method for further analysis of XRD
confirmed that all samples are formed in a crystalline cubic struc-
ture with Fd3m space group. FESEM morphological analysis reveals
the formation of grain and grain boundary with a decrease of grain
size when increasing the Cd-doping rate. A ferromagnetic character
at room temperature is confirmed by the hysteresis loop, which
shows an increase of saturation magnetization with Cd content in
the sample. Furthermore, the electrical conductivity measurement
was used as a function of frequency and temperature ranging from
10 Hz to 5 MHz and from 295 to 440 K, respectively. DC conduc-
tivity analyses allow us to estimate the activation energy, which
970 N. Hamdaoui et al. / Journal of Alloys and Compounds 803 (2019) 964e970
Fig. 11. Nyquist diagrams (Z00 vs. Z0 ) at room temperatures for x ¼ 0.00; x ¼ 0.20 and x ¼ 0.40 samples.
confirms that the electric transport is governed by the polaron
hopping mechanism. In addition, the AC conductivity is charac-
terized using a modified Jonscher's law, and the conductivity pro-
cess is confirmed by NSPT and CBH mechanisms.
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