International Journal of Advanced Materials Science
ISSN 2231-1211 Volume 8, Number 1 (2017), pp. 17-31
© Research Foundation
http://www.rfgindia.com
Characterization of Multicomponent Perovskite
Oxide La0.8Sr0.2Co 0.9Fe 0.1O3-δ Nanoparticles
for Supercapacitor
G.N. Chaudhari1*, V.V. Deshmukh1 and D.K. Burghate2
1Nanotechnology Research Laboratory, Department of Chemistry
Shri Shivaji Science College, Amravati (Maharashtra) 444602, India. 2Shri Shivaji Science College, Nagpur (Maharashtra) 440012, India.
Abstract
A multicomponent perovskite oxide nanoparticle based on
La0.8Sr0.2Co0.9Fe0.1O3-δ (LSCF) were prepared by a simple sol-gel method. The
as synthesized material have been calcined at 550◦C for single-phase
compound formation and evaluated for their structural and electrochemical
properties. XRD data reveal the presence of well-defined sharp peaks,
indicating the cubic perovskite structure and crystalline size about 10.97nm of
La0.8Sr0.2Co0.9Fe0.1O3-δ compound. Morphological studies of the prepared
sample were done by using SEM and TEM analysis. The elemental
composition of the sample was detected by EDAX analysis. Electrochemical
properties were investigated by cyclic voltammetry and galvanostatic
charge/discharge in 1M Na2SO4 electrolyte. LSCF electrode exhibited
maximum specific capacitance of 715.5 Fg-1 at the scan rate of 10 mV/s from
cyclic voltammetry curve. The La0.8Sr0.2Co0.9Fe0.1O3-δ material was promising
for supercapacitor applications.
Keywords: Supercapacitor, La0.8Sr0.2Co0.9Fe0.1O3-δ, cyclic voltammetry,
galvanostatic charge discharge.
mailto:[email protected]
18 G.N. Chaudhari, V.V. Deshmukh and D.K. Burghate
1. INTRODUCTION
The scarcity of fossil fuels and the increasing awareness of the environmental and
geopolitical problems associated with their use have encouraged significant efforts
towards the development of advanced energy storage and conversion systems using
materials that are cheap, abundant and environmentally benign. A major thrust in
the field of renewable energy has been to develop higher power and more energy-
dense storage devices like supercapacitors [1]. The supercapacitor is a new type of
electrochemical energy storage device having advantages of both the dielectric
capacitors and the rechargeable batteries. The typical dielectric capacitors can
provide high power densities and have very long cycle life, but they have low
energy densities. The typical rechargeable batteries can provide high energy
densities, but have low power densities and short cycling life. Supercapacitor can
meet both the power and the energy requirements for systems such as acceleration
power for electric vehicles, burst power for the generation of electronic devices and
so on and have been studied intensively in recent years [2-4].
Supercapacitor electrodes have to store large amounts of energy in the small volume
which is otherwise called such as double layer capacitors, ultracapacitors, gold
capacitors or power cache, supercap, superbattery, power capacitors and electric
double layer capacitors (EDLC). The supercapacitor having a lot of applications in
electric circuits, UPS systems, power conditioners, welders, inverters, automobile
regenerative braking systems, power supplies, cameras, power generators, power
quality, etc. Supercap properties are quickly charged and discharged than the
batteries, good stability and high power density, however the lagging of energy
density [5].
The mechanisms by which EDLCs store and release charge are completely
reversible, so they are extremely efficient and can withstand a large number of
charge/discharge cycles. They can store or release energy very quickly, and can
operate over a wide range of temperatures [6]. In terms of the chemical
composition, several types of supercapacitor electrode materials have been
investigated intensively, which include electrically conducting metal oxides like,
RuO2 [7], IrO2 [8], MnO2 [9], conducting polymers like, polythiophene [10],
polypyrrole [11-12], polyaniline (PANI) [13-14], and their derivatives, and different
type of carbon materials like carbon aerogel [15-16], activated carbon [17], and
carbon nanotubes [18-19].
In this work, we have synthesized mixed conducting perovskites of the
(La,Sr)(Co,Fe)O3-δ family by sol–gel method and employed as electrode for
electrochemical capacitors and electrochemical performances have been
investigated. LSCFs are considered as good cathode materials due to their ionic and
electronic conductivity at low and intermediate temperatures [20-21]. They also
Characterization of Multicomponent Perovskite Oxide La0.8Sr0.2Co 0.9Fe 0.1O3-δ 19
have high catalytic activity for oxygen reduction reaction due to their good oxygen
surface exchange and self-diffusion properties [22-23]. Badwal et al. [24] have
claimed that due to their mixed conductivity these materials exhibited two important
functions; charge transport through both ions and electronic carriers and efficient
charge transfer at the oxygen/electrode interface. In previous reported research work
LSCFs have been widely studied as cathode materials for solid oxide fuel cells
(SOFCs) [25-26]. We tried highly conductive LSCF composite for supercapacitor
performance because the supercapacitors assembled with LSCF electrodes can show
excellent stability. Our results demonstrate that by synthesizing LSCF material with
an ideal pore size, uniformity, substantially high power density, thermodynamic
stability, good ion accessibility and redox reversibility [27], the performance of
supercapacitors can be revolutionized.
2. EXPERIMENTAL DETAILS
2.1 Materials:
La(NO3)3.6H2O (≥99.0%), Sr(NO3)2 (≥99.5%), Co(NO3)2.6H2O (≥99.0%),
Fe(NO3)3.9H2O (≥99.0%) were purchased from Acros Organics and polyvinilidene
difluoride (PVDF), N-methyl-2-pyrrolidone (C5H9NO) was obtained from SRl
chem., sisco research laboratories pvt. ltd. All chemicals were used as received
without any further purification.
2.2 Synthesis of La0.8Sr0.2Co0.9Fe0.1O3-δ nanomaterial using sol-gel route:
Sol-gel technology is a well-established colloidal chemistry technology, which offers
possibility to produce various materials with novel, predefined properties in a simple
process and at relatively low process cost. The main benefits of sol–gel processing are
the high purity and uniform nanostructure achievable at low temperatures. The
properties of metal nanoparticles depend largely on their synthesis procedures. The
La0.8Sr0.2Co0.9Fe0.1O3-δ composite was synthesized by using sol-gel method. In order
to prepare a sol, stoichiometric amounts of the metal nitrates La(NO3)3, Sr(NO3)2,
Co(NO3)2 , and Fe(NO3)3 was dissolved in alcohol. Then, citric acid was added at a
molar ratio of 2:1. It acts as a chelating agent. The resulting mixture was kept stirring
at 80°C until a wet gel was formed. This gel is kept in pressure bomb at 1300C for
12hrs.The precipitate was formed. Final product was obtained by calcined at 3500C
for 3½ hrs. Further this product was calcined at 5500C for 6 hours for the study of
structural and electrochemical characterization.
20 G.N. Chaudhari, V.V. Deshmukh and D.K. Burghate
2.3 Characterization of La0.8Sr0.2Co0.9Fe0.1O3-δ (LSCF) nanomaterial:
Synthesized powder were characterized by Panalytical X-ray diffractometer (Xpert
pro MPD) equipped with Cu Kα sealed tube (λ=1.5406Aº). The sample was scanned
over 2ϴ ranging from 20 to 80º with a step size of 0.016º. The morphology and
particle size was investigated by scanning electron microscope (ultra plus zeiss
FESEM) and transmission electron microscope (Philips TEM). Energy Dispersive X-
ray(EDX) were coupled to SEM used to analyze the composition of sample.
2.4 Electrode preparation and electrochemical characterization:
The working electrode was prepared by mixing 80 wt% of the synthesized LSCF
nanomaterial, 15 wt% of acetylene black (to ensure good conductivity), and 5 wt% of
binder polyvinylidene difluoride (PVDF) in N-methyl-2-pyrrolidone (NMP). This
mixture was uniformly spread on gold plate by using spatula with area 1mg per square
centimetre and dried at room temperature overnight. The electrochemical performance
of the nanocomposite was evaluated on a CHI6002C workstation for cyclic
voltammetry (CV) and chronopotentiometry (CP) tests by using a three electrode cell
with Platinum foil as the counter electrode and an Ag/AgCl saturated calomel
electrode (SCE) as the reference electrode. All electrochemical measurements were
carried out in 1M aqueous Na2SO4 solution as electrolyte.
The specific capacitance (C, F.g-1) of the electrode was evaluated according to
equation (1) and (2), respectively:
Specific capacitance C = 1
𝑚.𝑆.(𝑉𝑎−𝑉𝑐)∫ 𝐼(𝑉)𝑑𝑉
𝑉𝑐
𝑉𝑎 (1)
Where m(g) is the mass of electroactive material loaded on the electrode, Va, Vc are
the anodic and cathodic peak voltages, s (V. s -1) is the scan rate for the
measurement and ∫ 𝐼(𝑉) dV is the area under the cyclic voltammogram from Va to
Vc.
C = i
−∆V
∆t×m
= i
−slope×m (2)
C is calculated from the galvanostatic charge-discharge (GCD) curves. Where i is the
impressed current, ΔV/Δt is the slope of the discharge curve after the iR drop, m is the
mass of each electrode.
3. RESULTS AND DISCUSSION
3.1 Structural analysis of La0.8Sr0.2Co0.9Fe0.1O 3-δ by X-Ray Diffraction studies :
X-ray diffraction(XRD) was performed on LSCF after calcined at 550°C in order to
check the purity of the crystalline product and to allow estimation of the
Characterization of Multicomponent Perovskite Oxide La0.8Sr0.2Co 0.9Fe 0.1O3-δ 21
crystallite size of the powder. The X-ray diffraction pattern of La0.8Sr0.2Co0.9Fe0.1O3-δ
powder is shown in Figure1. XRD analysis of the sample revealed single perovskite
phase produc with a cubic structure. The XRD peaks are found to be very sharp
indicating the highly crystalline nature of the perovskite and good incorporation into
the lattice of the metal oxides used in the powder synthesis. The major peaks for
sample are indexed to the crystal plane (012) (110) (202), (024), (214), (208) and
(226). Some weak peaks are also found, may be due to the presence of impurity
element such as La-O. Since the standard XRD data for La1-xSrxCo 1-yFe yO3-δ is not
available in the literature, the obtained XRD data were compared with the XRD data
of standard JCPDS pattern for LaCoO3(JCPDS card No. 25-1060 and 48-0123) .The
crystalline size was determined from full width of half maximum (FWHM) of
the most intense peak (110) corresponding to 2ϴ = 33.22° by using Scherer’s
formula,
d = 0.9λ / β cosθ
Where, ‘d’ is the crystalline size, λ is the X-ray wavelength of the Cu Kα source
(λ=1.54059A0), β is the FWHM of the most predominant peak at 100% intensity
(110), θ is the Braggs angle at which peak is recorded. It was found at 10.97 nm.
XRD data is in good agreement with results obtained in literature [28-29].
20 30 40 50 60 70 80
0
50
100
150
200
250
(122) (
226)
(208)
(400)
(018)
(214)
(024)
(202)
(110)
(012)
inte
nsi
ty(a
.u.)
2 (degree)
LSCF
Figure1. XRD pattern of La0.8Sr0.2Co0.9F 0.1O 3-δ.
3.2 Morphological analysis of La0.8Sr0.2Co0.9Fe0.1O3-δ by SEM :
The surface microstructure of La0.8Sr0.2Co0.9Fe0.1O3-δ nanoparticles was studied with
22 G.N. Chaudhari, V.V. Deshmukh and D.K. Burghate
SEM. The SEM photographs of LSCF nanoparticles are shown in Figure 2. SEM
analysis provides the information about the size and shape of the particle and pore.
From the SEM studies, it was found that the sample consists of homogeneously
distributed spherical shaped nano crystals with an average grain size of 300 nm. Also,
few larger particles are also present in the sample.
Figure 2: SEM photographs obtained on La0.8Sr0.2Co0.9Fe0.1O3-δ nanocrystalline
powder in two different magnifications (a) 51.13KX (b) 100.00KX
3.3 EDAX Analysis:
Figure 3 shows the energy dispersive X-ray spectrum of La0.8Sr0.2Co0.9Fe0.1O3-δ. The
EDAX spectra display the characteristic peaks corresponding to the binding energy
state of elements. This was carried out to understand the composition of La, Sr, Co,
Fe and oxygen in the material. No other impurity peaks are detected in the spectra,
Characterization of Multicomponent Perovskite Oxide La0.8Sr0.2Co 0.9Fe 0.1O3-δ 23
which is an indication of the chemical purity of the sample. The elemental
composition data obtained with La0.8Sr0.2Co0.9Fe0.1O3-δ nanocrystalline powder
prepared by sol-gel method is indicated in
Table 1: Sample composition
Element Wt.%
La 17.96
Sr 4.58
Co 20.94
Fe 2.03
O 54.49
Figure 3: EDAX spectra obtained on La0.8Sr0.2Co0.9Fe0.1O3-δ.
3.4 Surface morphological analysis of La0.8Sr0.2Co0.9Fe0.1O3-δ by TEM:
Figure 4 shows the typical morphology of La0.8Sr0.2Co0.9Fe0.1O3-δ nanomaterial.
Figure 4 shows that quasi-sherical LSCF nanoparticles have good dispersibility, and
the average size estimated from TEM is around 20-30nm, which is consistent with
XRD results.
24 G.N. Chaudhari, V.V. Deshmukh and D.K. Burghate
Figure 4: TEM images of La0.8Sr0.2Co0.9Fe0.1O3-δ.
Splitted electron diffraction spots can be observed in Figure 5. Electron diffraction
studies indicated crystalline nature of the sample.
Figure 5: Electron diffraction of La0.8Sr0.2Co0.9Fe0.1O3-δ..
Characterization of Multicomponent Perovskite Oxide La0.8Sr0.2Co 0.9Fe 0.1O3-δ 25
3.5 Electrochemical behaviour of La0.8Sr0.2Co0.9Fe0.1O3-δ.
3.5.1 Cyclic voltammetry:
Cyclic voltammetry is a very versatile electrochemical technique which allows to
probe the mechanics of redox and transport properties of a system in solution. This is
accomplished with a three electrode arrangement whereby the potential relative to
some reference electrode is scanned at a working electrode while the resulting current
flowing through a counter (or auxiliary) electrode is monitored in a quiescent
solution. Usually in cyclic voltammetry the potential is scanned back and forth
linearly with time between two extreme values. It provides considerable information
about the thermodynamics of a redox process, kinetics of heterogeneous electron-
transfer reactions and analysis of coupled electrochemical reactions or adsorption
processes.
The cyclic voltammetry response of the electrode La0.8Sr0.2Co0.9Fe0.1O3-δ at different
scan rates of 10, 20, 30, 40 and 50 mVs-1 is as shown in Figure 6. In this study, the
electrochemical properties of La0.8Sr0.2Co0.9Fe0.1O3-δ was explored in 1M Na2SO4
aqueous electrolyte between -0.2V to 0.4V potential window. A pair of redox peaks
was observed for all the scan rates which indicate that the major type of charge
storage was pseudocapacitive in nature. The oxidation peak occurs at 0.155 V and the
reduction peak at -0.009 V. Some week reduction peaks are observed at the potential
range 0.04V and -0.06V may be attributed to irreversible reduction of some other
complex species present in solution. Redox process was highly fast and reversible
seen from the nearly symmetrical current response even at high scan rates. Current
response increases linearly with the increase in scan rate which is suitable for power
applications. With increase in scan rate there is no much shift in the peak positions
exhibiting lower polarization effect in the electrode material and reason for better
reversibility. Specific capacitance of the material is calculated from the equation1.
Maximum specific capacitance of 715.5 Fg-1 was obtained at the scan rate
of 10m Vs-1. It indicates good performance of nanostructured La0.8Sr0.2Co0.9Fe0.1O3-δ
electrode. With increasing scan rate, the specific capacitance decreases gradually
(Figure7), which can be attributed to electrolytic ions diffusing and migrating into the
active materials at low scan rates. At high scan rates, the diffusion effect, limiting the
migration of the electrolytic ions, causes some active surface areas to become
inaccessible for charge storage. We also observe that the specific capacitance of the
LSCF samples decreases to 371.59 F g−1 as the scan rate increases to 50 mV s−1,
representing only a 48% decrease compared with the specific capacitance at a scan
rate of 10 mV s−1. This result indicates the excellent capacitive behaviour and high-
rate capability of the LSCF electrode.
26 G.N. Chaudhari, V.V. Deshmukh and D.K. Burghate
Figure 6: Cyclic Voltammogram of LSCF
Figure7: Plot of scan rate Vs specific capacitance
3.5.2 Galvonostatic Charge-Discharge analysis:
In order to evaluate the charge storage capacity, durability of cycle lifetime and
various electrical parameters, the galvanostatic charge-discharge analysis of the
LSCF electrode were performed at current density of 2×10 -5A between -0.2 and
0.4V. In this study, the working electrode is submitted to a constant current I (charge
or discharge), and voltage versus time is recorded between minimal and maximal
values. It is observed that, the discharge curves are linear in the total range of
potential with constant slopes, showing perfect capacitive behavior. The discharge
capacitance of the electrodes (C) was calculated from the slope of the
discharge curve by using (equation2) and it is found to be 708.6 F-1g. This result is in
good agreement with the specific capacitance calculated from cyclic voltammery.
Characterization of Multicomponent Perovskite Oxide La0.8Sr0.2Co 0.9Fe 0.1O3-δ 27
Figure 7: Galvonostatic charge-discharge curve of GCD curve of
La0.8Sr0.2Co0.9Fe0.1O3-δ electrode.
3.5.3 Electrochemical impedance spectroscopy (EIS):
Electrochemical impedance spectroscopy (EIS) has been widely used to examine a
complex sequence of coupled electrochemical processes, such as electron transfer and
mass transfer. A very small (5mV) amplitude signal is applied to the testing system
over a range of frequencies from 0.01Hz to 1MHz. By monitoring the current
response, the variation of resistance with frequency can be examined. The main
objective of the EIS measurements is to gain insight of the resistive and capacitive
elements associated with the electrode. The data obtained by EIS measurement is
expressed graphically in a Nyquist plot. A typical Nyquist plot of
La0.8Sr0.2Co0.9Fe0.1O3-δ is shown in Figure 8. The EIS curve consists of a depressed
arc in high-frequency regions and an inclined line in low-frequency regions. Ohmic
resisatnce of the electrolyte and the internal resistance of the electrode material is
denoted as Ri. The interfacial charge transfer resistane Rct and double layer
capacitance Cdl are parallely connected to represent the semicircle in high frequency
region. The determined values for Ri, Rct and Cdl are 1.06Ω, 2.6Ω, 1.348μF etc. As
well, the sloping lines reveal the capacitive character at low frequencies. Different
from the ideal 900 phase angle for pure EDLCs, the straight lines with a slope of 450
might derive from a contribution of pseudo capacitance. And this result is in very
good agreement of the specific capacitance behaviour of LSCF electrode.
28 G.N. Chaudhari, V.V. Deshmukh and D.K. Burghate
Figure 8: A typical Nyquist plot of of La0.8Sr0.2Co0.9Fe0.1O3-δ
4. CONCLUSION
In conclusion, a multicomponent perovskite oxide nanoparticle La0.8Sr0.2Co0.9Fe0.1O3-δ
(LSCF) with diameter of around 11nm were fabricated via a simple sol-gel method.
Its chemical composition and structural characters were survey by XRD, EDAX,
SEM, and TEM measurements. The investigations of CV, GCD, and EIS on the
capacitive behaviour of LSCF nanocomposite reveal its excellent electrochemical
properties for the supercapacitor application, including good reversibility and specific
capacitance value. It can be believed that this kind of composites show great potential
as an electrochemical supercapacitors.
5. ACKNOWLEDGEMENT
The authors are grateful to Nanotechnology Research lab, Department of Chemistry,
Shri Shivaji Science College, Amravati for providing research facilities.
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