World Journal of Nano Science and Engineering, 2011, 1, 99-107
doi:10.4236/wjnse.2011.14016 Published Online December 2011 (
Copyright © 2011 SciRes. WJNSE
Synthesis of Ba0.5Sr0.5Co0.2Fe0.8O3 (BSCF) Nanoceramic
Cathode Powders by Sol-Gel Process for Solid Oxide
Fuel Cell (SOFC) Application
Yousef M. Al-Yousef, Mohammad Ghouse*
Energy Research Institute King Abdulaziz City for Science and Technology (KACST), Riyadh, Saudi Arabia
E-mail: *,
Received June 21, 2011; revised November 10, 2011; accepted November 20, 2011
The nano ceramic Ba0.5Sr0.5Co0.2Fe0.8O3 (BSCF) powders have been synthesized by Sol-Gel process using
nitrate based chemicals for SOFC applications since these powders are considered to be more promising
cathode materials for SOFC. Glycine was used as a chelant agent and ethylene glycol as a dispersant. The
powders were calcined at 850˚C/3 hr in the air using Thermolyne 47,900 furnace. These powders were char-
acterized by employing SEM/EDS, XRD and TGA/DTA techniques. The SEM images BSCF powder indi-
cate the presence of highly porous spherical particles with nano sizes. The XRD results shows the formation
of BSCF perovskite phase at the calcination temperature of 850˚C. From XRD line broadening technique, the
average crystllite size of the BSCF powders were found to be around 9.15 - 11.83 nm and 13.63 - 17.47 nm
for as prepared and after calcination at 850˚C respectively. The TGA plot shows that there is no weight loss
after the temperature around 450˚C indicating completion of combustion.
Keywords: SEM/EDS, XRD, TGA/DTA, Ba0.5Sr0.5Co0.2Fe0.8O3 (BSCF)
1. Introduction
Solid oxide fuel cells (SOFCs) are considered as one of
the most promising energy conversion devices that ex-
hibit advantages such as high efficiency, system com-
pactness and low environmental pollution [1-4]. The
SOFCs are expected to be around 50% - 60% efficient at
converting fuel to electricity. In applications designed to
capture and utilize the system’s waste heat (co-genera-
tion), overall fuel use efficiencies could top 80% - 85%.
Since SOFC operate at very high temperatures ~1000˚C,
it removes the need for precious metal-catalyst, thereby
reducing cost. It allows SOFCs to reform fuels internally,
which enables the use of a variety of fuels and reduces
the cost associated with adding a reformer to the system.
SOFCs are also the most sulfur-resistant fuel cell type;
they can tolerate several orders of magnitude more sulfur
than other fuel cell types. In addition, they are not poi-
soned by carbon monoxide (CO), which can even be
used as fuel. The traditional SOFC operate at around
1000˚C, which causes several problems such as; degra-
dation of performance due to the formation of second
phase, sintering of the electrodes and interfacial diffusion
between electrode and electrolyte. The current status of
the development of a cell unit is based on yttria-stabi-
lized zirconia (YSZ) solid electrolyte and electrodes
consisting of Sr-doped LaMnO3 (LSM-Cathode) and Ni-
YSZ cermet (Anode) [5,6]. The state-of-the art cathode
material for high temperature (1000˚C) operation is LSM
perovskite oxide. However, due to its poor ionic conduc-
tivity, search of alternative cathode materials for inter-
mediate temperature SOFC (IT-SOFC) is necessary.
Therefore, the present trend is to develop reduced tem-
perature SOFC technology which could be operated at
below 800˚C. So much attention is being made for IT-
SOFC in recent years [7-9]. Development of alternative
cathode materials with adequate mixed ionic-electronic
conductivity (MIEC) is needed to make the IT-SOFC
technology successful. In spite of significant efforts have
been put until now by various researchers, fundamental
questions on the mechanism and kinetics of the O2 re-
duction reaction and on the electrode behavior of LSM
materials under fuel cell operation conditions still remain
unsolved. The Table 1 shows the suitable materials for
SOFC components [10].
Kim et al. [11] prepared nano BSCF, LSCF and LSM
Table 1. Suitable materials for SOFC components [10].
Component Requirements Preferred Materials Possible Alternatives
i > 0.05 S·cm–1 ZrO2-Y2O3
(3 - 10 mol%)
CeO2-Gd2O3, (Sm2O3)
Cathode >100 S·cm–1
(electronic/mixed) La1–xSrxMnO3 (La1–xSrx)Co, FeO3
Anode >100 S·cm–1
(electronic/mixed) Ni/ZrO2-Y2O3
Interconnect Inert material, high temp. stabilityHigh temp. alloys
La1–x(Sr,Ca,Mg)xCrO3 -
Manifold Non-volatile, inert Ceramics, metals -
Seal Non-volatile, inert Glass, glass-ceramic,
Metal/ceramic -
cathode powers by glycine-nitrate process (GNP) me-
thod for metal-supported SOFCs and studied their parti-
cle size distribution, SEM, XRD, EIS measurement and
electrochemical performance at 1073 K. The powder den-
sity obtained were 0.91 W·cm–2, 0.77 W·cm–2, 0.69 W·cm–2
for the above powders respectively.
Park et al. [12] studied zinc-doped barium strontium
cobalt ferrite (Ba0.5Sr0.5Co0.2–xZnxFe0.8O3–δ(BSCZF), x =
0, 0.05, 0.1, 0.15, 0.2) perovskite oxide powders for cath-
odes of SOFCs application using the eyhylene diamine
tetraacetic acid (EDTA)-citrate method with repeated
ball-milling and calcining. They were evaluated as cath-
ode materials for SOFC at intermediate temperature (IT-
SOFCs) using XRD, H2-TPR, SEM and electrochemical
tests. It is reported that the lowest doping of 0.05
(BSCZF05) resulted in the highest electrical conductivity
of 30.7 S·cm–1 at 500˚C.
Chen and Shao [13] synthesized BSCF powders by
combined EDTA-citrate complexing sol-gel process. The
powder was calcined in air for 5 hr, ball milled and then
pressed into bar-shaped pellets using a stainless steel die
under a hydraulic pressure of 200 MPa and sintered at
1100˚C and evaluated their properties using XRD, ESEM
and electrical conductivity relaxation (ECR) using Ar
and O2 mixture. Based on chemical bulk diffusion coef-
ficient (Dchem), the calculated ionic conductivity of BSCF
reached 0.07, 0.25 and 0.96 S·cm–1 at 600˚C, 700˚C,
800˚C respectively.
Sun et al. [14] prepared BSCF cathode materials for ce-
ria-composite electrolyte low temperature SOFC application
using sol-gel process with polyacrylicaced (PAA) with ad-
justted pH with ammonia and they were evaluated with
XRD, and electrochemical properties. It is reported that the
maximum power density achieved was about 800 mW·cm–2
at 500˚C with Ni as anode and Sm0.2Ce0.8O2 (SDC)-car-
bonate composite electrolyte and cathode as BSCF.
Recently a new cathode material Ba0.5Sr0.5Co0.8Fe0.8O3
(BSCF) reported [15], which showed excellent perform-
ance as cathode material in conjunction with ceria-based
electrolyte at reduced temperature compared with con-
ventional cathode materials. Generally synthesis of BSCF is
carried out by the traditional solid-state reaction methods
[16] and other wet chemical methods [17-21]. These
methods are time consuming and require high tempera-
ture calcination (>950˚C) and long time to prepare the
precursor, which faces the difficulties in preparing homo-
genous material with good reproducibility. So to overcome
such difficulties a sol-gel process is used generally for
preparing the pure BSCF nano-powder for SOFC cath-
ode application.
The main design requirements for SOFC Cathode Ma-
terials [22] include: 1) High electronic conductivity, 2)
Chemically compatible with neighboring cell compo-
nents (electrolyte), 3) Stable in oxidizing environment, 4)
Large triple phase boundary, 5) High ionic conductivity,
6) Thermal expansion coefficient similar to other SOFC
materials, 7) Relative simple fabrication, 8) Relatively
inexpensive materials.
In the present investigation, nano-crystalline cathode
material of BSCF (5528) powders were prepared by the
Sol-Gel process since it is a simple and more economical
way of making nano powders for SOFC application. While
the physical characterization of the powders were carried
out using SEM/EDS, XRD techniques, the thermal prop-
erties were carried out using TGA/DTA techniques.
2. Experimental Procedure
2.1. Preparation of BSCF Powders
The Ba0.5Sr0.5Co0.2Fe0.8O3 (BSCF-5528) nano ceramic pow-
ders were prepared by modified Sol-Gel Process [23-27]
using Ba(NO3)2 (BDH), Sr(NO3)2 (BDH), Co(NO)3·9H2O
(Fluka), Fe(NO3)3·9H2O, Citric Acid (BDH), Ethylene
Copyright © 2011 SciRes. WJNSE
glycol (BDH), Ammonia Solution and distilled water.
The precursor solution was prepared by mixing individual
aqueous solution of the above chemicals in a molar ratio
of 0.5:0.5 and 0.2:0.8 respectively (Table 2). To the
mixed all nitrate solutions, required citric acid, ammonia
solution and ethylene glycol were added. The citrate/
nitrate ratio used in the present experiments was 0.5. The
solution was heated in a pyrex glass beaker on a hotplate
using magnetic stirrer until a chocolate colored gel was
formed. When heated further, the gel burns to a light and
fragile ash. The ash was calcined at 850˚C/3 hr in air in a
Barnstead Thermolyne 47,900 Furnace (USA). Figure 1
shows the flow sheet for the preparation of Ba0.5Sr0.5Co0.2
Fe0.8O3 powder using the Sol-Gel process. Tab le 2 shows
the batch preparation of nano cathode materials (BSCF-
5528) by the Sol-Gel process.
Figure 1. Flow Sheet for the preparation of Ba0.5Sr0.5Co0.2
Fe0.8O3 Nanoceramic cathode powders by Sol-Gel process [23-
Table 2. Cathode (BSCF-5528) powders prepared by sol-
gel process.
Sample no Cathode Powder With c/n Ratio
#77a,b Ba0.5Sr0.5Co0.2Fe0.8O3 0.50
#78a,b Ba0.5Sr0.5Co0.2Fe0.8O3 0.50
2.2. SEM/EDS Characterization
Small amounts of the samples were spread on adhesive
conductive aluminum tapes attached to sample holders,
coated with thin films of gold and examined with a FEI
Quanta 200 Scanning Electron Microscope. An attached
OXFORD INCA250 Energy Dispersive Spectroscopy
(EDS) unit was used to determine area and spot elemen-
tal compositions. Images at higher magnification were
collected with a FEI Quanta 3DF SEM. Imaging was per-
formed in secondary electron (SEI) mode using an ac-
celerating voltage of 20 keV.
2.3. XRD Characterizatio n
A part of the samples were analyzed with a PANnytical
X’Pert PRO XRD for phase characterization. The X-ray
diffractometry with CuK radiation at 35 kV and 20 mA
was used for phase analysis with a diffraction angle 2
theta range 10˚ - 80˚ and particle size determination from
X-ray line broadening technique using the following
Debye Scherrer Equation [28]:
t 0.9B cos Ø
where t = average particle size in nm, λ = the wave
length (0.15418 nm) of Cu Kα radiation, B the width (in
radian) of the XRD diffraction peak at half of its maxi-
mum intensity (FWHM), Ø the Bragg diffraction angle
of the line, and B is the line width at half peak intensity.
2.4. TGA/DTA Characterization
In order to determine the decomposition behavior of the
BSCF Gel samples, around 7 mg - 8mg of the Gel sam-
ples were loaded in an alumina crucible and put inside
the thermo balance of TG machine (Perkin-Elmer Ther-
mal Analysis Controller TAC7/DX, USA). The thermal
decomposition behavior was studied up to 700˚C that
was raised at a rate of ~10˚C per minute. TGA and DTA
plots were presented.
3. Results and Discussion
3.1. SEM/EDS Characterization
Figures 2-5 show the SEM images and EDS spectra of
Copyright © 2011 SciRes. WJNSE
Figure 2. (a) SEM image of Ba0.5Sr0.5Co0.2Fe0.8O3 cathode
powder as prepared (#77a); (b) SEM image of Ba0.5Sr0.5Co0.2
Fe0.8O3 cathode powder calcined at 850˚C (#77b).
Figure 3. (a) EDS of Ba0.5Sr0.5 Co0. 2Fe0.8O3 #77a (as prepared);
(b) EDS of Ba0.5Sr 0.5Co0.2Fe0.8O3 #77b (calcined at 850˚C).
Figure 4. (a) SEM image of Ba0.5Sr0.5Co0.2Fe0.8O3 cathode
powder (#78a); (b) SEM image of Ba0.5Sr0.5Co0.2Fe0.8O3 ca-
thode powder (#78b).
nano-sized particles of the Ba0.5Sr0.5Co0.2Fe0.8 O3 (BSCF-
5528) powder as prepared samples and calcined at 850˚C/
3 hrs which were prepared with the Sol-Gel process us-
ing metallic nitrates. It is seen in the SEM images that
the particles are homogeneous with the presence of
highly porous spherical particles of nano size with ag-
glomeration. It is noted from the figures that the particle
size of the calcined powders at 850˚C are larger than the
as prepared powders since growth kinetics are favored
and the spherical particles became larger with porous
structure which resembled the typical cathode structure
for SOFC application. The SEM images of BSCF ob-
tained here are similar to the other authors reported [30].
Figures 3 and 5 show the EDS patterns of Ba0.5Sr0.5
Co0.2Fe0.8O3 powders (as prepared and calcined at 850˚C).
The figures show the presence of Ba, Co, Fe, C, O peaks.
The residual C element from the citric acid probably that
Copyright © 2011 SciRes. WJNSE
Copyright © 2011 SciRes. WJNSE
had not been combusted fully yet is shown in EDS in the
as prepared BSCF powder. However, C content has been
reduced in the calcined powders at 850˚C as seen in the
EDS. Also this would further be reduced by increasing
the calcination temperature.
3.2. XRD Characterization
Figures 6 and 7 show the XRD patterns of the as prepared
and calcined powders of Ba0.5Sr0.5Co 0.2Fe0.8O3 at 850˚C
respectively. It is seen that as prepared powder is partly
amorphous in nature. It is seen that the calcined powder
has well crystalline perovskite phase of Ba0.5Sr0.5
Co0.2Fe0.8O3. These results are in agreement with the
other authors reported elsewhere [14,15,19]. However, a
minor amount of BaCoO3 phase is also present in the
powders. This impurity will be disappeared and a single
cubic perovskite structures may form when the calcina-
tion temperature is raised to ~1000˚C [18,19]. Also, this
could be achieved by using pure metal nitrate chemicals
(99.99%). Table 3 shows the average crystallite sizes of
BSCF powders calcined at 850˚C. It is seen that the av-
erage crystllite size of the BSCF powders were found to
be around 9.15 nm - 11.83 nm and 13.63 nm - 17.47 nm
for as prepared and calcined powders respectively. The
results obtained here for BSCF (5528) are in the agree-
ment with the other authors reported elsewhere [29] for
BSCF using glycine/nitrate (g/n) ratio of 0.56. A number
of factors are responsible for the nano size of the result-
ing powders. Before the reaction, all the reactants are
uniformly mixed in solution at atomic or molecular level.
So during combustion, the nucleation process can occur
through the rearrangement and short-distance diffusion
of nearly atoms and molecules. When the combustion
process takes place such a fast rate that sufficient energy
and time are not available for long distance diffusion or
(a) (b)
Figure 5. (a) EDS of Ba0.5Sr0.5Co0.2Fe0.8O3 cathode #78a (as prepared); (b) EDS of Ba0.5Sr0.5Co0.2Fe0.8O3 cathode #78b (cal-
cined at 850˚C).
Figure 6. XRD Patterns of Ba0.5Sr0.5Co0.2Fe0.8O3 cathode powder (#77) (bottom: as prepared; top: calcined at 850˚C).
Table 3. XRD Data to determine the average particle size of the BSCF (5528) powders prepared by Sol-Gel.
Sample no. 2Ø B
Average Particle size,
t (nm)
#77a 24.432 0.680 11.83
#77b 32.08 0.600 13.63
#78a 24.84 0.880 9.15
#78b 31.92 0.468 17.47
Figure 7. XRD pattern of Ba0.5Sr0.5Co0.2Fe0.8O3 cathode powder (#78) (bottom: as prepared; top: calcined at 850˚C).
migration of the atoms or molecules which may result in
crystalline growth. So the initial nano size of the powders is
retained after the combustion reaction in sol-gel process.
The average particle size of BSCF powder obtained here
with c/n of 0.50 are much better than particle sizes ob-
tained for BSCF using combination of PVA and urea as
fuel [30].
3.3. TGA/DTA Characterization
Figures 8(a) and (b) depict the TGA and DTA plots of
the BSCF gels derived from precursor solution in the
temperature range of 25˚C - 650˚C respectively. The
endothermic peak observed for BSCF gel in the DTA
curves at ~130˚C with small weight loss is due to evapo-
ration of residual and hydrated water in the high tem-
perature combustion process. It is seen from 180˚C -
300˚C that two strong exothermic peaks in DTA curves
are observed which seemed to be associated with the
decomposition/oxidation of the metal-chelates producing
oxide phases. No further weight loss is observed after
temperatures reaching around 450˚C in the TGA plots
which indicates the completion of combustion and for-
mation of expected perovskite phase of BSCF. These
results are similar to the other authors reported else-
where [30] for BSCF gels.
4. Conclusions
The following conclusions are drawn from the present
The Ba0.5Sr0.5Co.2Fe0.8O3 (BSCF-5528) nano ceramic
powders for cathodes were successfully prepared by
Sol-Gel process with c/n ratio of 0.50.
SEM images of BSCF powders indicate the presence
of highly porous spherical particles of nano size in
the powders calcined at 850˚C.
XRD patterns show the presence of the perovskite
Ba0.5Sr0.5Co0.2Fe0.8O3 phases.
TGA plot depicts that there is no weight loss after the
temperature of about 450˚C indicating completion of
the combustion and forming oxide phases.
Copyright © 2011 SciRes. WJNSE
Figure 8. (a) TGA plot of Ba0.5Sr0.5Co0.2Fe0.8O3 gel; (b) DTA plot of Ba0.5Sr0.5Co0.2Fe0.8O3 gel.
Copyright © 2011 SciRes. WJNSE
5. Acknowledgements
Authors thank Dr. Naif M. Al-Abbadi, former Director,
Energy Research Institute, King Abdulaziz City for Sci-
ence and Technology (KACST), Riyadh, Saudi Arabia
for his encouragement and support during the course of
this work.
Also, author’s thanks are due to Mr. Mahmoud Al-
Manea, Dr. Shahreer Ahmad, Mr. Waleed Al-Othman and
Mr. Abdul Jabbar Khan, Technology Center (TC), Saudi
Arabian Basic Industries Corporation (SABIC), Jubail,
Saudi Arabia for providing SEM/EDS analysis results of
Cathode powder samples. Also, author’s thanks are due to
Prof. Ahmed Basfer and to his colleagues Mr. Haitham
Al-Gothami Technicians, Atomic Energy Research In-
stitute (AERI) KACST, Riyadh, Saudi Arabia for pro-
viding XRD analysis and TGA/DTA of Cathode powder
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