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Structural, magnetic and

electrochemical properties of
CoxZn1-x Fe2O4 nanoparticles
synthesized by co-precipitat...
Pubs Gupta
International Journal of Advanced Science and Research

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International Journal of Advanced Science and Research

International Journal of Advanced Science and Research

ISSN: 2455-4227
Impact Factor: RJIF 5.12
www.allsciencejournal.com
Volume 2; Issue 6; November 2017; Page No. 33-41

Structural, magnetic and electrochemical properties of CoxZn1-x Fe2O4 nanoparticles synthesized by

co-precipitation method
K Sathiyamurthy, * P Sivagurunathan
Department of Physics, Annamalai University, Annamalai Nagar, Tamil Nadu, India

Abstract
Cobalt zinc ferrite nanoparticles, CoxZn1-xFe2O4(x=0.3, 0.5 and 0.7), have been prepared by the co-precipitation method and
annealed at different temperatures. The structural and magnetic properties of the samples were determined and characterized by X-
ray analysis showed that the samples were cubic spinel. Enhancement of crystallinity and particle size was observed with the
increase in annealing temperatures. The increase in cobalt concentration in zinc ferrite nanoparticles resulted in the decrease of
lattice parameter, unit cell volume and increase X-ray density were observed. Thermo gravimetric and differential thermal analysis
(TG/DTA) method was used to confirm the formation of cobalt zinc ferrite nanoparticles. FTIR spectra confirm that the presence
of metal oxide stretching vibration is attributed to the formation of cobalt zinc ferrite nanoparticles. The cobalt zinc
ferrite nanoparticles annealed at 600 °C were characterized by using FESEM with EDAX, FETEM with SAED pattern. The
surface morphology of cobalt zinc ferrite nanoparticles studied through FESEM and FETEM indicate that the particles were in
spherical shape. EDAX analysis revealed the presence of Co, Zn, Fe and O content in cobalt zinc ferrite nanoparticles, and it’s
varied with the Co concentration. The M–H curve of cobalt zinc ferrite nanoparticles shows a ferromagnetic behavior at room
temperature. The magnetic measurements showed that the saturation magnetization and coercivity increased with increasing the
cobalt content in zinc ferrite nanoparticles, and it is suitable for magnetic devices. The electrochemical performance of the nickel
zinc ferrite nanoparticles was investigated by CV analysis. The higher capacitance value 449 Fg -1 was observed for the scanning
rate 5mVs-1for Ni0.7Zn0.3Fe2O4 reflecting the good quality of nickel zinc ferrite nanoparticles, and it was suitable for supercapacitor
application.

Keywords: ferrite, cobalt zinc ferrite nanoparticles, magnetic property, super capacitor

1. Introduction Co2+ ions are in the B sites namely tetrahedral and Fe3+ ions
In the recent past, interest on synthesis of nanostructured are accommodated both the A and B sites namely tetrahedral
magnetic materials has developed in various research areas and octahedral respectively [9]. Therefore, cobalt zinc mixed
due to their potential applications. As a result, many ferrite has attracted considerable attention due to their
researchers show extreme interest in the synthesis of potential applications. In recent days, ferrite nanoparticles
conventional materials at the nanoscale. Experimental have been prepared by using various methods, such as
conditions play a vital role in determining the shape, size and hydrothermal treatment [10], micro emulsion [11], solvothermal
[12]
purity of the nanoparticles. Spinel ferrite is one of the most , micro-wave sintering [13], ceramic technique [14], sol–gel
attractive magnetic nanoparticles used in various fields, such synthesis [15], solid state reaction [16] and co-precipitation
as magnetic resonance imaging, heat transfer devices, and method [17]. Among the aforesaid methods, chemical co-
high density magnetic storage devices [1, 3]. Supercapacitors precipitation method is a very resourceful, easy to handle and
and batteries are popular now electrochemical energy storage efficient method for the synthesis of ferrite nanoparticles [18].
system in recent days. The batteries distribute high energy It is interesting to study the different concentrations of cobalt
density and low power density whereas, conventional in zinc ferrite nanoparticles annealed at different temperatures
capacitors deliver high power density and low energy density. providing a useful result. An attempt has been made to
Supercapacitor is attractive because it can afford high power synthesis of CoxZn1-xFe2O4 (x = 0.3, 0.5 and 0.7) nanoparticles
density, high rate capability, and long cycle life [4, 5]. These using chemical co-precipitation method. Prepared samples
supercapacitors have plentiful potential applications such as were annealed at different temperatures (400 °C, 600 °C and
power electronics, electric vehicles, sensor, and computer 800 °C) and its effect on structural, thermal, morphological,
backup etc., [6]. Zinc ferrite nanoparticles added with cobalt magnetic and electrochemical properties were investigated by
modified the properties such as magnetic properties, high XRD, TG/DTA, FTIR, FESEM, FETEM, VSM and CV
corrosion resistivity and chemical stability [7]. Zinc ferrite measurements.
nanoparticles possess normal spinel structure, where all the
Zn2+ ions are occupied at a sites namely tetrahedral, and all the 2. Experimental
Fe3+ ions are occupied at B sites namely octahedral [8]. Cobalt added zinc ferrite (CoxZn1-xFe2O4) nanoparticles
CoFe2O4 nanoparticles is an inverse spinel structure, where (x=0.3, 0.5 and 0.7) were synthesized by using a co-

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International Journal of Advanced Science and Research

precipitation method [19]. All the chemicals were purchased

from Merck (AR grade) of 99% purity used for the present
work without any further purification. For the successful
synthesis of CoxZn1-xFe2O4 nanoparticles, aqueous solutions of
Fe (NO3)3.9H2O, Zn (NO3)2.6H2O, Co (NO3)2.6H2O were
dissolved in 20 ml of de-ionized water separately. Then the
citric acid (C6H8O7) dissolved in de-ionized water and then
added into nitrate solution drop by drop. Appropriate amount
of sodium hydroxide (NaOH) precipitating agent was added to
the nitrates solution in order to obtain the precipitate. After
getting black brown color solution, the resultant solution was
stirred continuously 120 minutes at 60 °C in 750 rpm.
Obtained product was washed several times by acetone and
de-ionized water, and then the precipitate was dried in hot air
oven at 100 °C for 2 hrs. Further, the synthesized
nanoparticles were annealed for 3 hrs at 400 °C, 600 °C and
800 °C respectively.

2.1 Characterization technique

The obtained materials were made to undergo XRD analysis,
which was performed by a Philips X` pert Pro 3040/60
diffractometer with CuKα (λ=1.54060Å) radiation. XRD
pattern was recorded in the range of 20° to 80°. As a result of
using the Joint Committee on Powder Diffraction Standards
(JCPDS) database the phase identification of the prepared
sample was found out. Average crystalline sizes of the
samples have been calculated by Debye-Scherer’s formula [20].

D= (1)

Where D is mean crystalline size, K is a dimensionless shape

factor, with a value close to unity. The shape factor has a
typical value of about 0.9, but varies with the actual shape of
the crystallite, λ is wavelength of radiated X-ray (in Å), θ is
represent Bragg diffraction angle (in radian) and β is full-
width at half maximum subsequent to corrected for
instrumental error. The TG/DTA analysis was carried out
using NETZSCH - STA 449 F3 JUPITER. FTIR spectra were
recorded using Perkin Elmer FTIR model 2000
spectrophotometer from 1000 to 400 cm-1. FESEM with
EDAX was recorded using ZEISS SUPRA 40 VP SEM.
Shape of the particles with micro structural properties were
examined by FETEM JEM 2100F. The selected area electron
diffraction (SAED) patterns were confirmed by dispersing the
sample beyond a carbon covered copper grid. Magnetic Fig 1(a, b & c): XRD Spectra of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7)
measurements were carried out with the Quantum Design nanoparticles as-prepared and annealed at different temperatures
lakeshore model 7407 Vibrating sample magnetometer (VSM)
and parameters saturation magnetization (Ms) and coercive As the prepared sample does not show any peaks which
force (Hc) were evaluated. An electrochemical property of the reveals that the prepared sample is amorphous in nature, so
nanoparticles was investigated by using the cyclic annealing process is essential and it has been carried out for
voltammetry (CV) instrument model CHI 660. further study. For that all synthesized samples were annealed
at 400 °C, 600 °C and 800 °C and the XRD patterns of
3 Results and discussion Co0.3Zn0.7Fe2O4, Co0.5Zn0.5Fe2O4 and Co0.7Zn0.3Fe2O4
3.1 Structural properties nanoparticles having (220), (311), (400), (511) and (440)
The X-ray diffraction pattern of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 planes confirm that the synthesized nanoparticles possess a
and 0.7) nanoparticles annealed at different temperatures cubic spinel structure with Fd3m space group [21]. The peaks
namely 400 °C, 600 °C and 800 °C are shown in Fig. 1(a, b present in the obtained XRD patterns are well matched with
and c). JCPDS card no. 89-1012 (ZnFe2O4) and 22-1086 (CoFe2O4)

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International Journal of Advanced Science and Research

and it may suggest that the synthesized particles are cobalt data using the relation is given by
zinc ferrite nanoparticles. Similar result was observed by
Gozuak et al., [22] for Synthesis and characterization of dx = ZM / Na3 (4)
CoxZn1-xFe2O4 magnetic nanoparticles. XRD analysis
designate that the particle size increased with the increase of Here, dx is the X-ray density (g/cm3), Z is the number of
annealing temperatures reveals the growth of the nanoparticles molecules per unit cell (Z = 8 for spinel system), M is the
is shown in Table 1. molecular weight of the sample, N is the Avogadro’s number,
and 'a' is the lattice parameter. Table 1 indicates that the X-ray
Table 1: Particle size D (nm), Lattice parameter ‘a’ (Å), Unit cell density (dx) are increased with increasing annealed
volume (V) (Å) and X-ray density (dx) of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 temperatures from 400 °C to 600 °C and 600 °C to 800 °C for
and 0.7) nanoparticles annealed at different temperatures a cobalt zinc ferrite nanoparticles. It is interesting to note that
Temperature (D) ‘a’ (V) dx increasing X-ray density with increasing cobalt concentrations
Material ◦
C (nm) (Å) (Å) 3
(gm/cm ) from Co0.3Zn0.7Fe2O4 to Co0.5Zn0.5Fe2O4 and Co0.5Zn0.5Fe2O4
400 ◦C 10 8.453 603 4.14 to Co0.7Zn0.3Fe2O4 in all temperatures are observed. The X-ray
Co0.3Zn0.7Fe2O4 600 ◦C 14 8.445 602 4.15 density depends upon the lattice parameter and molecular
800 ◦C 18 8.425 598 4.18 weight of the sample. This is expected since the lighter cobalt
400 ◦C 11 8.447 602 4.15
ion replaces a heavier zinc ion, in addition to the decrease in
Co0.5Zn0.5Fe2O4 600 ◦C 17 8.439 600 4.16
800 ◦C 21 8.397 592 4.22 lattice parameter [26].
400 ◦C 13 8.420 597 4.18
Co0.7Zn0.3Fe2O4 600 ◦C 22 8.419 596 4.19 3.2 TG/DTA
800 ◦C 26 8.376 587 4.24 The TG/DTA curves of the dried precursor sample of
Co0.5Zn0.5Fe2O4 nanoparticles from 35 °C to 850 °C are shown
The particle size of the Co0.3Zn0.7Fe2O4 at 400 °C, 600 °C and in Fig. 2.
800°C are 10, 14 and 18 nm respectively. The increases in
particle size with annealing confirm the growth of cobalt zinc
ferrite nanoparticles. Similar trend is noticed for
Co0.5Zn0.5Fe2O4 and Co0.7Zn0.3Fe2O4 nanoparticles. The
particle size of Co0.3Zn0.7Fe2O4, Co0.5Zn0.5Fe2O4 and
Co0.7Zn0.3Fe2O4samples annealed at 400 °C are 10, 11 and 13
nm respectively. An identical result has been observed for the
cobalt zinc ferrite nanoparticles annealed at 600 °C and 800
°C. The increasing particle size with increasing cobalt
concentration is observed in the present study is close
agreement with Mehran et al., (23) for the synthesis of CoZn
ferrite nanoparticles. This could be ascribed to the smaller
covalent radius of Co cation (1.26 Å) than Zn cation (1.25 Å)
[24]
. Structural parameters such as, lattice parameter (a) of the
annealed CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) nanoparticles
have been calculated by using this relation is given by

(2)
Fig 2: TG/DTA analysis of Co0.5Zn0.5Fe2O4 nanoparticles
Here, `a` is the lattice parameter, d is the interplanar spacing,
The first stage of weight loss is observed in TGA curve at a
and h, k, and l are the Miller indices of the crystal planes. The
temperature below 99 °C (2%) due to desorption of water
interplanar spacing d can be calculated by using the Bragg law
vaporization of hydroxyl group. The second weight loss is
of X-ray diffraction. The unit cell volume is calculated by
observed in the range from 99 °C to 210 °C (6 %) as a result
using the following equation, which depends on the lattice
of decomposition of organic templates. The final weight loss
Parameter.
of (7%) is observed in between 210 °C and 391 °C due to
crystallization of the final product. No weight loss is observed
Volume of the unit cell V=a3 (Å) (3) beyond 391 °C indicating the formation of cobalt zinc ferrite
nanoparticles. The TG curve shows that there is a continuous
The lattice parameter and unit cell volume decreased with and gradual weight loss up to about 391 °C and no weight loss
increasing the annealing temperatures of CoxZn(1-x)Fe2O4 is recorded for further increasing of temperature [27]. The DTA
(x=0.3, 0.5 and 0.7) nanoparticles are shown in Table 1. The curve shows the presence of one endothermic peak and one
decrease lattice parameter and unit cell volume with increase exothermic peak at 281 and 326 °C respectively. The
in Co concentration is observed in the present study suggest endothermic peak come out due to loss of absorbed water and
the configuration of a homogeneous solid solution [25]. the exothermic peak at 326 °C is accompanied with the
The X-ray density (dx) values are calculated from the XRD decomposition of the metal hydroxides [28].

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International Journal of Advanced Science and Research

3.3 Functional group analysis been obtained in the frequency range of 1000-400 cm-1 is
FTIR spectra of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) shown in Fig. 3(a, b and c).
nanoparticles annealed at 400 °C, 600 °C and 800 °C have

Fig 3(a, b & c): FTIR spectra of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) nanoparticles annealed at different temperatures

There are two strong absorption bands are observed in the Table 2: FTIR spectra of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7)
FTIR spectra of Co0.3Zn0.7Fe2O4, Co0.5Zn0.5Fe2O4 and nanoparticles annealed at 400 °C, 600 °C, and 800 °C
Co0.7Zn0.3Fe2O4 samples. The higher absorption band ν1 has Temperature
400 °C 600 °C 800 °C
°C
been observed in the range of 594-578 cm-1 corresponds to
ѵ1 ѵ2 ѵ1 ѵ2 ѵ1 ѵ2
intrinsic stretching vibration of the tetrahedral position of Co- Samples
(cm−1) (cm−1) (cm−1) (cm−1) (cm−1) (cm−1)
O/Zn-O and lower absorption band is observed in the range of Co0.3Zn0.7Fe2O4 562 420 568 424 572 427
420-464 cm-1 is assigned due to octahedral position of Fe- Co0.5Zn0.5Fe2O4 572 424 574 428 579 430
Co0.7Zn0.3Fe2O4 577 426 580 430 586 432
O/Co-O stretching vibration of the ferrite nanoparticles [29, 30].
The absorption bands of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) 3.4 Field emission scanning electron microscope (FESEM)
samples annealed at different temperatures are summarized in with EDAX
Table 2. The morphology of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7)
nanoparticles annealed at 600 °C have been studied by means
of the FESEM image is shown in Fig.4(a, b and c).

Fig 4(a, b & c): FESEM image of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) nanoparticles annealed at 600 °C

36
International Journal of Advanced Science and Research

The morphology can be able to identify the agglomeration in

spherical nanoparticles, which is attributed due to the
interaction between magnetic ferrite nanoparticles [31]. The
EDAX spectrum of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7)
nanoparticles annealed at 600 °C are shown in Fig.4 (d- f).
From EDAX spectra of the elements present in the samples
are identified as Co, Zn, Fe and O and it is shown in Fig.4 (d-
f). The quantitative results of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and
0.7) nanoparticles annealed at 600 °C are shown in Fig.4 (g-i).
It is seen from the figure shows that the weight and atomic
percentage of the cobalt ions increased from Co0.3Zn0.7Fe2O4
to Co0.5Zn0.5Fe2O4 and Co0.5Zn0.5Fe2O4 to Co0.7Zn0.3Fe2O4,
whereas the reverse trend is observed for zinc content confirm
the Co2+ ions replacing the Zn2+ions. Similar result was
observed by Anshu Sharma et al., [32] for cobalt doped zinc
ferrites nanoparticles using metallo-organic decomposition
technique.

3.5 Field emission transmission electron microscope

(FETEM) with SAED
Fig 4(d, e & f): EDAX spectra of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and FETEM images of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7)
0.7) nanoparticles annealed at 600 °C and (g, h and i) corresponding nanoparticles intend morphology is shown in Fig. 5(a, b and
Quantitative results
c).

Fig 5 (a, b & c): FETEM image of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) nanoparticles annealed at 600 °C and (d) (e), (f) resultant SAED.

The FETEM images of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) observation made by XRD. The resultant selected area
nanoparticles annealed at 600 °C which confirms the particles electron diffraction pattern (SAED) of spherical shaped
are agglomerated with spherical shape [33]. From Fig. 5(a, b CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) is shown in Fig. 5(d, e
and c), the average particle size is found to be 14.2, 17.8 and and f). From the SAED pattern rings match well with standard
23.4 nm for the samples Co0.3Zn0.7Fe2O4, Co0.5Zn0.5Fe2O4 and powder diffraction information of spinel CoFe 2O4 and
Co0.7Zn0.3Fe2O4, respectively. This is well agree with those ZnFe2O4 samples. The figure shows a SAED patterns reveals

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International Journal of Advanced Science and Research

the ordered structure of cobalt zinc ferrite nanoparticles which field (Hc) at room temperature for the samples Co xZn(1-x)Fe2O4
is in good agreement with XRD results showing the good (x=0.3, 0.5 and 0.7) nanoparticles annealed at
crystalline nature of cobalt zinc ferrite nanoparticles [34]. 600 °C shows a clear M-H curves as shown in Fig.6(a, b and
c). The saturation magnetization (Ms) and coercivity (Hc) of
3.6 Magnetic properties CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) annealed at 600 °C are
The variation of magnetization (Ms) as a function of applied provided in Table 3.

Fig 6(a, b & c): Room temperature M-H curves for CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) nanoparticles annealed at 600 °C

Table 3: Saturation magnetization (Ms) and Coercivity (Hc) value of structure of spinel ferrites, the magnetic order is mainly
CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) nanoparticles annealed at 600 °C constructed due to super exchange interactions between metal
Material Ms (emu/g) Hc (G) ions of sub-lattices A and B sites. In ZnFe2O4, Zn2+ preferably
Co0.3Zn0.7Fe2O4 21.2 323.7 occupies the tetrahedral (A) sites and Fe3+ prefers the
Co0.5Zn0.5Fe2O4 35.3 337.5 octahedral sites (B). CoFe2O4 has an inverse spinel structure
Co0.7Zn0.3Fe2O4 41.2 341.3 in which Co2+ occupies B site and Fe3+ ions equally taken A
and B sites, with their spins in the opposite direction [36]. The
The low field region of the magnetization increases with magnetic moments of Fe3+ are mutually compensated, and the
increasing applied magnetic field. It can be seen that all the resulting moment of the ferrite is due to the magnetic
magnetization curves are saturated at higher field region and moments of bivalent cations Co2+ in the B positions.
the hysteresis curves for cobalt zinc ferrite nanoparticles Replacement of Co2+ with Zn2+ leads to introduction of non-
resulting an S shaped hysteresis curve and suggesting the magnetic Zn2+ ions into A sites, thus increasing the saturation
ferromagnetic behavior of the material at room temperature magnetization, Ms, leading to an increased magnetization [37].
[35]
. From Fig. 6, it is observed that Co 0.3Zn0.7Fe2O4 obtained a
saturation magnetization value of 21.2emu/g and the 3.7 Cyclic Voltammetry (CV)
coercivity value of 323.7 G. While increasing the The cyclic voltammetry study for CoxZn(1-x)Fe2O4 (x=0.3, 0.5
concentration of Co content Co0.5Zn0.5Fe2O4 and and 0.7) nanoparticles annealed at 600 °C electrode is carried
Co0.7Zn0.3Fe2O4, the values of both the saturation out, and it is recorded at different scan rates 5, 10, 20, 30, 50,
magnetization and the coercivity get increased. In a cubic and 100 mVs-1 shown in Fig.7 (a, b and c).

38
International Journal of Advanced Science and Research

Fig 7(a, b & c): CV pattern of CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) nanoparticles annealed at 600 °C

Ideal rectangular shape is observed in the CV sure for 5 mVs - cathodic charges on each scanning, m specifies the mass of the
1
. The pseudo-capacitive nature is confirmed for the CoxZn(1- electrode material (mg) and ∆v means the scan rate (mVs-1)
x)Fe2O4 (x=0.3, 0.5 and 0.7) samples annealed at 600 °C as the fixed in examining, tetra butyl ammonium perchlorate 0.2 M
CV pattern changes with increasing scan rate. The specific with a standard three electrode configuration consisting of a
capacitances (CS) values of our desired synthesized material sample (working electrode), an Ag/AgCl (reference electrode)
cobalt zinc ferrite electrode can be calculated using the and a high platinum wire (counter electrode) is taken during
relation [38]. electrochemical measurements [39]. Different scan rate starting
from 5 mVs-1 to 100 mVs-1 is done and their equivalent
(5) specific capacitance value decreased as the scan rate increase
which is illustrated in Table 4
Here, Cs is the specific capacitance, Q signifies the anodic and

Table 4: The specific capacitance of the CoxZn(1-x)Fe2O4 (x=0.3, 0.5 and 0.7) samples annealed at 600 °C for different scan rates
Different Scan Rate specific capacitance Fg-1
(mVs-1) Co0.3Zn0.7Fe2O4 Co0.5Zn0.5Fe2O4 Co0.7Zn0.3Fe2O4
5 300 344 376
10 186 220 272
20 74 96 98
30 42 55 57
50 21 25 29
100 3 7 9

A higher capacitance value of 376 Fg-1 is recorded for detected for higher scan rates specify that the ionic diffusion
Co0.7Zn0.3Fe2O4 samples than Co0.3Zn0.7Fe2O4 and takes place only for outer surfaces [40]. The greater specific
Co0.5Zn0.5Fe2O4. The present study reveals that the better capacitance value detected in the present study confirms the
concentration as Co0.7Zn0.3Fe2O4 samples, exhibiting higher better crystallinity of the Co0.7Zn0.3Fe2O4 nanoparticles, and it
specific capacitance. Higher specific capacitance value at low helps to attain a better super capacitor.
scan rate has been detected in the present study i.e.,5 mVs-1
propose that the ionic diffusion takes place in, both inner and 4. Conclusions
outer surfaces depict lower specific capacitance values Cobalt zinc ferrite nanoparticles have been synthesized by

39
International Journal of Advanced Science and Research

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