Materials Research Bulletin 98 (2018) 213–218

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Materials Research Bulletin

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

Effect of Cu dopant on the structural, magnetic and electrical properties of T

Ni-Zn ferrites
⁎
M. Houshiar , L. Jamilpanah
Department of Physics, Shahid Beheshti University, Evin, Tehran 19839, Iran

A R T I C L E I N F O A B S T R A C T

Keywords: Ni0.8-xCuxZn0.2Fe2O4 (x = 0.0, 0.2, 0.4, 0.6) ferrite was synthesized through auto-combustion method. (XRD)
Spinel ferrites patterns confirmed the crystallization of the samples in spinel structure. FESEM showed that the size of ferrite
Ni-Cu-Zn particles are about few hundred nanometers and with increase in Cu concentration (x) in the structure there is
Magnetic and electrical properties increase in particle size. Fourier transform infrared (FTIR) spectrometry indicates that octahedral and tetra-
hedral sites are formed. Vibrating sample magnetometer (VSM) results proved reduction of saturation magne-
tization (Ms) by increasing Cu content, which is explained according to the ferrimagnetic nature of these samples
in which Ni is replaced by Cu at octahedral site. Real part of dielectric constant (ε) and loss tangent (tanδ) of
samples were also studied in frequency range of 100–20000 Hz. Results showed an increase in ε and tanδ of the
sample with x = 0.6 which is considered to be the result of higher density of this sample.

1. Introduction tetrahedral and octahedral sublattices which determine many of their

electrical and magnetic properties. These materials are Ferrimagnetic in
Recently spinel ferrites have gained wide attention in different fields nature. Ferrimagnetic character of spinel ferrites originate from the
of technology and industry, such as medicine and electronics, because antiparallel alignment of magnetic moments of atoms in tetrahedral and
of their excellent mechanical, electrical and magnetic properties [1–6]. octahedral sublattices. Replacing different kind of atoms which have
Characteristics of ferrites depend on their structure, size, atomic mix- different atomic radius, weight and magnetization in these sublattices,
tures, density and many other factors which in turn depend on the allows us to control structural properties which leads to the control of
fabrication method [7]. electrical and magnetic properties of spinel ferrites [17–21]. Therefore,
Low temperature of processing [8] High resistivity [9] and perme- to control the properties of ferrites one can control their structural
ability [10] of Ni-Cu-Zn ferrites have made them suitable for using in properties as they are sensitive to the structural parameters. Cation
multilayer chip inductors (MLCIs) [11] and surface mount devices distribution in spinel ferrites has been investigated by many authors
(SMDs) [12]. The multilayer structure must be processed below the [22–25]. Cation distribution in Ni-Cu-Zn ferrites is known to be as
melting point of the electrode material (961 °C in the case which Ag is follows [26,27]:
used as electrode) to prevent the interfacial diffusion of electrode ma- 2+ 3+ 2+ 2+ 3+ 2−
(Zn 0.2 Fe0.8 )[Ni 0.8 − x Cu x Fe1.2 ] O4 (1)
terial into the ferrite layer. Sintering at low temperature is crucial for
preparation and controlling the stoichiometry of the compositions. There are many reports on the effect of different dopants [28–31],
Several attempts have recently been made for improving the magnetic particle size [7,32] and fabrication method [33–36] on magnetic
properties of these ferrites by substitution of different cations [13–15]. properties of ferrites. Furthermore there are some experimental re-
Addition of copper reduces sintering temperature down to 900 °C. Also searches about the relation between electrical properties and some
copper promotes densification of Ni-Zn ferrites, without degrading the physical properties of ferrites like density and grain size which are in-
dielectric and magnetic properties [16]. Thus using Cu as a dopant in vestigated by many authors through different fabrication methods and
the structure of Ni-Zn ferrites instead of using Ni-Zn ferrites alone leads structural properties [37,38].
to improved process which is possibly due to the structure change and In this work, we have used simple and cost-effective [39] auto
hence electrical and magnetic properties of this kind of spinel ferrite. combustion method to synthesize Ni-Cu-Zn ferrites with different
Ni-Cu-Zn ferrites crystallize in spinel structure and show ferrimag- amounts of Ni and Cu dopants. We have investigated their electrical
netic and semiconducting behavior. Spinel structure has two main and magnetic properties and explained them according to the

⁎
Corresponding author.
E-mail addresses: [email protected], [email protected] (M. Houshiar).

http://dx.doi.org/10.1016/j.materresbull.2017.10.024
Received 28 March 2017; Received in revised form 3 October 2017; Accepted 15 October 2017
Available online 16 October 2017
0025-5408/ © 2017 Elsevier Ltd. All rights reserved.
M. Houshiar, L. Jamilpanah Materials Research Bulletin 98 (2018) 213–218

composition and structure of the synthesized samples. We performed a Table 1

thorough study on the relation between microstructural properties and Lattice constant (a), crystal size (D), saturation magnetization (Ms), density (ρ), dielectric
constant (ε) and tanδ of the Ni0.8-xCuxZn0.2Fe2O4 ferrite samples.
electrical and magnetic properties of Ni-Cu-Zn spinel ferrites. XRD,
FESEM, FTIR, VSM and electrical measurements were used to in- Cu content, x x = 0.0 x = 0.2 x = 0.4 x = 0.6
vestigate the effects induced by microstructural properties. Taking all
these into account, these results seem to be useful towards designing a (Å) 8.3389 8.3501 8.3523 8.3598
D (nm) 23.9 22.9 24.2 32.3
and fabrication of electronic devices like MLCI’s.
Ms (emu/g) 65.78 57.85 54.52 44.85
ρ (gr/cm3) 3.848 3.552 3.686 4.579
2. Experimental ε (f = 100 Hz) 529.68 223.41 310.12 8982.61
tanδ (f = 100 Hz) 1.16 1.54 2.19 10.35

Ni0.8-xCuxZn0.2Fe2O4 (x = 0.0, 0.2, 0.4, 0.6) ferrite was prepared

through auto-combustion method using glycine as fuel. High purity Ni
Scherer equation. Eight sharp peaks of (111), (220), (311), (222),
(NO3)2·6H2O, Cu(NO3)2·4H2O, Zn(NO3)2·6H2O and Fe(NO3)2·9H2O
(400), (422), (511) and (440) were used in these calculations and the
powders were dissolved in deionized water with stoichiometric
averages of (a) and (D) are presented in Table 1. The measured crystal
amounts and then by mixing and stirring at a constant temperature
size of samples (22.9-32.3 nm) show nano crystalline structure of fer-
(60 °C), a homogenized solution was gained. By raising the temperature
rites synthesized by auto combustion method.
to 100 °C all the water evaporated and again by further raising the
As seen in Table 1 the value of lattice constant and crystal size in-
temperature to 250 °C ignition occurred and a fluffy loose powder was
crease by adding Cu to the samples. As can be seen, the lattice constant
formed. To assure crystal formation, all the samples were annealed at increases from 8.3389 to 8.3598 Å for x = 0.0 to x = 0.6 and crystal
900 °C for 3 h in ambient air. X-ray diffraction (XRD) was performed size increases from 23.9 to 32.3 nm. The increase in lattice constant is a
using diffractometer STADI STOE with CuKα (λ=1.54 Å) at the angles consequence of the bigger ionic radius of Cu+2 (0.73 Å) compared to
(2θ) ranging from 10 −70°. The data were analyzed using X’pert soft- Ni+2 (0.69 Å) atom in octahedral site [40,41] which eventually results
ware. Field emission scanning electron microscopy (FESEM) was used in bigger crystal size.
to study the grain formation of the samples. Fourier transform infrared We used FESEM to better study the microstructural properties of the
spectrometry (FTIR) was recorded in the range of 350 to 1000 cm−1. To synthesized samples. FESEM images of all the samples are presented in
perform these measurements, pellets of samples were made mixed with Fig. 2 which show the formation of polygonal shape of particles. These
KBr. Vibrating sample magnetometer (VSM) measurements were per- images indicate that the sizes of ferrite particles are around few hun-
formed up to 20 kg at room temperature to study the magnetic prop- dred nanometers. It can be seen in Fig. 2 that there is a regular variation
erties of the ferrites with different amounts of Cu dopant. For electrical in the size of particles from x = 0.0 to x = 0.6, such that the particle
measurements, powder of the samples were mixed with PVA alcohol size increases by increasing the amount of Cu dopant in the structure.
(5%) as binder and letting them dry at room temperature for 24 h and Especially for x = 0. 6 sample which shows a sudden growth with re-
then made into pellets with 13 mm diameter and 1.5 mm thickness spect to other samples. Also x = 0.4 sample shows a bigger size than
using 5 MPa hydraulic pressure for 20 mins. Then the pellets were x = 0.0 and x = 0.2 sample. This result is in agreement with XRD re-
annealed for 3 h in air at 900 °C. Silver paste was then used on both sults. There are some reports on the grain size growth of ferrites with
sides of each pellet to ensure good electrical contact. LCR meter (model increasing Cu amount in their structure which they have attributed to
GW Instek LCR-821) was utilized to measure electrical parameters of the higher atomic mobility of Cu ions [42,43]. In turn electrical and
the pellets in the frequency range of 100–20000 Hz. magnetic properties of ferrite particles can be affected by particle size.
FTIR measurements were performed, as it helps to understand the
3. Results and discussion formation of bonds and sites (octahedral and tetrahedral) in the
structure of ferrites which play an important role in electrical and
XRD patterns of the samples are plotted in Fig. 1. They show that the magnetic properties of ferrites [44–46]. FTIR results of Ni0.8-
spinel structure of all the samples with fd3 m space group is formed xCuxZn0.2Fe2O4 samples are presented in Fig. 3. Two main bonds in
(JCPDS 008-0234). It can be seen that a little hematite phase in spinel structure are M-O bonds in octahedral and tetrahedral sites,
x = 0.0, x = 0.2 samples is formed, this phase disappears at higher between Oxygen (O) and the doped atom in the structure of ferrite (M)
concentrations of Cu. We conclude that Cu dopant decreases the an- [47–49]. The occupancy of different kinds of atoms in tetrahedral and
nealing temperature of Ni-Zn ferrites. Lattice constant (a) and crystal octahedral sites strongly affects the physical properties of spinel fer-
size (D) of the samples were calculated using miller indices and Deby- rites. Zn atom occupies tetrahedral sites while Ni and Cu atoms can go
either to octahedral or to tetrahedral sites with a much greater tendency
to octahedral site [50]. In FTIR spectrum we see the bands at about 400
and 600 cm−1, related to octahedral and tetrahedral sites respectively.
The band related to octahedral site (at about 400 cm−1) shifts toward
lower wavenumbers with higher Cu concentrations. Due to bigger
atomic weight of Cu compared to Ni, by adding Cu to the samples and
reducing Ni, tensile wavenumber reduces and so we see a peak shift
from 397 cm−1 to 374 cm−1 in octahedral site. There is a slight similar
shift in tetrahedral site band (at about 600 cm−1) too, which can be an
evidence of the replacement of Cu ions in octahedral site rather than
tetrahedral site [51,52]. More experiments like Mössbauer spectroscopy
can disclose the precise distribution of ions in octahedral and tetra-
hedral sites [37].
In order to investigate the magnetic properties of the samples, VSM
measurements up to 20 kg were used (Fig. 4). According to the ferri-
magnetic nature of spinel ferrites, the net magnetization of the cell of
these samples follows the eq. (2) [50]:
Fig. 1. XRD patterns of Ni0.8-xCuxZn0.2Fe2O4 with different concentrations of Cu.

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M. Houshiar, L. Jamilpanah Materials Research Bulletin 98 (2018) 213–218

Fig. 2. FESEM images of Ni0.8-xCuxZn0.2Fe2O4 ferrite samples

with polygonal shape.

Fig. 3. FTIR results of Ni0.8-xCuxZn0.2Fe2O4 ferrite samples and their absorption band shift
towards lower wavenumbers. Fig. 4. Hysteresis loop of Ni0.8-xCuxZn0.2Fe2O4 ferrite samples. Inset shows saturation
magnetization Ms versus Cu content x.

M = MA − MB (2)
data represented in Table 1 it can be seen that the Ms decreases from
In which Mis the net magnetization of the cell, MA and MB are the 65.78 emu/g to 44.85 emu/g as Cu content increases from x = 0.0 to
magnetization of octahedral and tetrahedral sites. As discussed earlier, x = 0.6. All samples have the coercivities below 50 G showing soft
Ni atoms are replaced by Cu atoms in octahedral site and also since the magnetic nature of all the samples.
magnetization of Cu+2 ions is lower compared to Ni+2 ions, the re- As the final investigation, the electrical properties of the synthesized
duction of saturation magnetization (Ms) of the samples is expected as Ni0.8-xCuxZn0.2Fe2O4 ferrites with different amounts of Cu dopant x are
Cu amount increases in the structure. In the inset of Fig. 4 the decrease presented. Real part of dielectric constant (ε) of the pellet of the
of (Ms) can be seen according to the amount of Cu. According to the

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Fig. 5. Dielectric constant (ε) of Ni0.8-xCuxZn0.2Fe2O4 ferrite samples vs frequency.

samples were calculated using the following formula:

C×t
ε=
ε0 × A (2)

where ε0 is the permittivity of free space, C is the real part of capaci-

tance of the pellet, t is the thickness and A is the area of cross section of
the pellet. Dielectric constants ε of the samples versus frequency f are Fig. 7. (a) Crystallite size and density and (b) dielectric constant and tanδ of Ni0.8-
presented in Fig. 5. The reduction of ε with increasing frequency f is xCuxZn0.2Fe2O4 ferrite samples at f = 100 Hz.
seen here. This result is in agreement with Maxwell-Wagner polariza-
tion [53,54] and Koop’s phenomenological theory [55]. This behavior
(ρ) of the samples directly [38]. The values of densities are obtained
occurs when the alternating electric charges lag the alternating external
using the values of weight and volume of the pellets which were made
electric field [56]. Loss tangents (tanδ) of the samples versus frequency
using the sample powders. The values of the density of the pellets are
f are presented in Fig. 6 with a peak appearing in all the samples. This
presented in Table 1 which shows an increase for x = 0.6 sample
peak occurs when the frequency of the oscillating external electric field
compared to other concentrations of Cu. Also crystal sizes are presented
and the natural oscillating frequency of electric charges are equal [57].
in this table which show the similar increase at x = 0.6 sample. In the
For x = 0.6 sample a shift in tanδ peak towards lower frequencies is
explanation of this behavior, we can mention the bigger particle size
observed. This kind of shift was also observed by M. Kaiser et al. with
and lower annealing temperature which is needed for crystallization of
similar samples and they attributed this shift to the increase of [Ni2+-
the samples with higher concentrations of Cu (resulted from SEM and
O2–-Ni2+] interactions, due to the presence of higher concentration of
XRD measurements) and so the density of this sample increased.
Ni in their samples [37]. This shift also has been observed by M.C.
Fig. 7(a) shows the dependence of crystallite size and density and
Dimri et al. in a similar manner [38]. In spinel ferrites the polarization
Fig. 7(b) shows the dependence of ε and tanδ on Cu concentration. An
mechanism at low frequencies (1–105 Hz) occurs through ions existing
anomalous increase is observed in ε and tanδ of the sample with
in octahedral sites with different ionic charges (hopping mechanism)
x = 0.6 Cu content (Fig. 7(b)). Also the same trend is seen in density
[46,50]. For the samples with x = 0.0, 0.2 and 0.4 the orders of values
and crystal size of the samples with a sudden increase for x = 0.6
of ε and tanδ are the same, while for x = 0.6 sample these values in-
sample (Fig. 7(a)). These plots show that the increase in density has
crease dramatically. These values at f = 100 Hz are presented in
caused an increase in ε and tanδ due to higher polarizing species for the
Table 1.
sample with higher density. Also there are some deviations from this
The deterministic parameter which governs the amount of dielectric
dependency of dielectric properties to density. In explaining this be-
constant, is the number of polarizing species which arise from density
havior the effect of other factors on dielectric properties of materials
like dopants, grain and grain boundary size and lattice constant should
be considered which can effect dielectric properties when the density of
material is not varying considerably. For example the particle size from
SEM of x = 0.4 sample is bigger than that of x = 0.0 sample too and
this might cause some variations in grain boundary polarities [58] and
so effecting tanδ. The above results suggest that this relation between
electrical parameters and the microstructure of the samples be studied
for different compositions of ferrites for better understanding of their
nature in response to this microstructural property.

4. Conclusion

The dependency of magnetic and electrical properties on the mi-

crostructure of synthesized samples was studied. The results revealed
indications of strong effect of composition, density and particle size on
Ni0.8-xCuxZn0.2Fe2O4 (x = 0.0, 0.2, 0.4, 0.6) ferrites. Properties of
Fig. 6. Loss tangent (tanδ) of Ni0.8-xCuxZn0.2Fe2O4 ferrite samples vs frequency.
synthesized Ni0.8-xCuxZn0.2Fe2O4 (x = 0.0, 0.2, 0.4, 0.6) ferrite samples

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