J Solid State Electrochem
DOI 10.1007/s10008-013-2355-1
ORIGINAL PAPER
Preparation and electrochemical performance
of porous hematite (α-Fe2O3) nanostructures
as supercapacitor electrode material
S. Shivakumara & Tirupathi Rao Penki &
N. Munichandraiah
Received: 24 October 2013 / Revised: 29 November 2013 / Accepted: 2 December 2013
# Springer-Verlag Berlin Heidelberg 2013
Abstract Porous α-Fe2O3 nanostructures have been syn-
thesized by sol–gel route. The effect of preparation
temperature on the morphology, structure, and electro-
chemical stability upon cycling has been studied for
supercapacitor application. The discharge capacitance
of α-Fe2O3 prepared at 300 °C is 193 F g−1, when
the electrodes are cycled in 0.5 M Na2SO3 at a specific
current of 1 A g−1. The capacitance retention after
1,000 cycles is about 92 % of the initial capacitance
at a current density of 2 A g−1. The high discharge
capacitance as well as stability of α-Fe2O3 electrodes is
attributed to large surface area and porosity of the
material. There is a decrease in specific capacitance
(SC) on increasing the preparation temperature. As iron
oxides are inexpensive, the synthetic route adopted for
α-Fe2O3 in the present study is convenient and the SC
is high with good cycling stability, the porous α-Fe2O3
is a potential material for supercapacitors.
Keywords Iron oxides . Porous nanostructures .
Supercapacitors
S. Shivakumara (*) : T. R. Penki : N. Munichandraiah
Department of Inorganic and Physical Chemistry, Indian Institute of
Science, Bangalore 560012, India
e-mail: elessk@gmail.com
Introduction
Electrochemical capacitors (ECs) have attracted interest in
recent years because of their high power density, excellent
reversibility, and long-cycle life [1]. Research efforts have
been underway in developing supercapacitors with both
high energy density as well as high power density by
exploring novel electrode materials [2–4]. Various elec-
trode materials including carbons [5, 6], conducting poly-
mers [7] and metal oxides [8] have been widely consid-
ered for ECs. Pseudocapacitive metal oxides, such as
RuO2 [9], NiO [10–12], Co3O4 [13–15], MnO2 [16, 17],
Fe3O4 [18–23], and Fe2O3 [24–29], have been studied as
active electrode materials. Among them, ruthenium oxide
[9] has been demonstrated with excellent pseudocapacitive
performance. However, a high cost of RuO2 limits its
commercial application. Efforts have been devoted on
investigations of inexpensive alternative materials with
good capacitance characteristics similar to RuO2. Among
the metal oxides, iron oxides are of particular interest due
to their easy synthesis, low cost, good structural stability,
and environmental friendliness.
Hematite (α-Fe2O3) has been investigated for applica-
tions in lithium batteries, sensors, and catalysts [30–36]. It
is also one of the promising materials for supercapacitors
[27–29]. The specific capacitance (SC) of iron oxide
electrodes is strongly influenced by the surface morphol-
ogy, surface area, porosity, etc. [28]. Recently, porous α-
Fe2O3 nanostructures with SC of 138 F g−1 are reported
[27–29]. This value is the highest reported till now for

Fig. 1 Powder XRD patterns of
(a) as-prepared, (b) F200, (c)
F300, (d) F400, (e) F500, and
(f) F-600
iron oxides. Preparation of α-Fe2O3 with appropriate
morphology, surface area, and porosity for achieving
high SC is a challenging task. Synthetic routes to pre-
pared to porous α-Fe2O3 nanostructures include chemical
precipitation, forced hydrolysis, sol–gel processes, etc.
[37–40]. Among these routes, chemical precipitation and
sol–gel methods are widely used to prepare α-Fe2O3
nanoparticles with a high yield. Simple synthesis routes
for porous α-Fe 2 O 3 nanostructures and studies on
supercapacitor properties are rarely reported.
In the present work, porous, high surface area α-Fe2O3
nanostructures are prepared by a sol–gel method followed by
heating at several temperatures between 200 and 600 °C. The
electrochemical capacitive behaviors of α-Fe2O3 nanostruc-
tures are studied in an aqueous 0.5 M Na2SO3 solution. The
sample annealed at 300 °C exhibits good electrochemical
performance with high discharge capacitance and good cy-
cling stability.
Experimental
Synthesis of porous α-Fe2O3 nanostructures
All chemical used were of analytical grade and they were
used as received. In a typical synthesis, 3 g of FeCl3·6H2O
was dissolved in 100 ml of double distilled water at room
temperature. To the above solution, 5 ml of ethylene glycol
was added slowly and continued stirred for 1 h. A red
J Solid State Electrochem
transparent colloidal suspension appeared. 1 M NaOH so-
lution was added dropwise to increase the pH to 9. The
contents were stirred for 6 h. Iron hydroxide formed was
filtered, and washed with distilled water several times
followed by ethanol. The product was dried at 100 °C for
12 h. Samples were heated at several temperatures for 3 h
between 200 and 600 °C in a muffle furnace under air
atmosphere. The sample prepared at 200, 300, 400, 500,
and 600 °C, respectively, are referred to F200, F300, F400,
F500, and F600.
Characterization methods
Powder X-ray diffraction (XRD) patterns were recorded
u s i n g B r u k e r D 8 a d v a n c e d i ff r a c t o m e te r w i t h
monochromatized Cu Kα (λ =1.5418 Å) incident radiation
as the source. Surface area and pore size distribution of the
samples were measured using micromeritics surface area
analyzer model ASAP 2020. The microscopy studies were
conducted by using FEI model Sirion scanning electron
microscope (SEM) and transmission electron microscope
(TEM) model JEOL JEM 2100 F.
Preparation of electrodes and electrochemical characterization
The electrodes were fabricated on a high-purity stain-
less steel (SS) foil as a current collector. The SS was
polished with successive grades of emery paper and
washed thoroughly with detergent and distilled water.
J Solid State Electrochem
Fig. 2 SEM micrographs of a as prepared, b F200, c F300, d F400, e F500, and f F600
For fabrication of electrodes, α-Fe2O3 (75 wt.%), con-
d u c t iv e c a r b o n ( K e t j e n b l a c k , 1 5 w t . % ) , a n d
polyvinylidene fluoride (10 wt.%) were mixed in a
mortar. A few drops of N -methyl pyrrolidone were
added to form a syrup. The syrup was coated on the
pretreated SS foil with a geometrical surface area of
1 cm2 and dried at 100 °C under reduced pressure.
Coating and drying steps were repeated to get the mass
of active material 0.5–0.6 mg cm−2. The electrodes
were finally dried for 12 h. Electrochemical cell was
assembled using α-Fe 2 O 3 -coated SS, Pt foils, and
saturated calomel electrode (SCE) as the working,
counter, and reference electrodes, respectively in a
glass container. All potential values reported are
against SCE reference. The electrolyte was aqueous
0.5 M Na2SO3 solution. Cyclic voltammetry (CV) and
galvanostatic charge–discharge cycling were measured
by a Biologic SA multichannel potentiostat/galvanostat
model VMP3. The electrochemical impedance spectros-
copy (EIS) measurements were carried out in the fre-
quency ranging from 0.01 Hz to 100 kHz with an
alternating current perturbation of 5 mV by Solatron

a sample and the sample heated at 200 °C are nearly
b sample (F300), crystalline particles (Fig. 3b) are seen
0.37 nm
(012)
Fig. 3 (a) TEM images of a as prepared (inset SAED patterns) and b
F300 sample (top inset HRTEM and bottom inset SAED patterns)
frequency response analyzer model 1255B and Solatron
electrochemical interface model 1287. The galvanostatic
charge–discharge cycling tests between −0.8 and 0.0 V
were performed, and the discharge SC was calculated
using the following equation:
SC ¼ It ðΔEmÞ
where I is current, t discharge time, ΔE potential window
(0.8 V), and m mass of the active material on the working
electrode.
Results and discussion
Figure 1 shows powder XRD patterns of samples pre-
pared at different temperatures. Pattern of the as-prepared
J Solid State Electrochem
identical (Fig. 1a and b), indicating amorphous nature.
The samples prepared at ≥300 °C (Fig. 1c–f) exhibit
crystalline nature with rhombohedral structure of α-Fe2O3
(JCPDS 33–0664). Morphology significantly influences the
properties of the material for supercapacitor properties. In
the SEM image of the as-prepared sample (Fig. 2a), particles
are not clearly seen. On increasing the temperature of prepa-
ration, particles progressively clear as observed in Fig. 2b–f
for the samples F200–F600, respectively. Worm-like particles
of size less than 100 nm are observed for F600 sample
(Fig. 2f).
TEM image and corresponding selected area electron
diffraction (SAED) pattern of the as-prepared sample are
shown in Fig. 3a, SAED pattern shows diffused pattern
characteristics of an amorphous phase. For the heated
and well-defined circles are present in the SAED pattern
(Fig. 3b inset). Also the lattice fringes seen in high-
resolution TEM (HRTEM) image (Fig. 3b inset) with
interspacing distance of 0.37 nm correspond to the
(012) plane of α-Fe2O3.
To evaluate the surface area and porous nature of the
α-Fe2O3 nanostructures, N2 adsorption–desorption iso-
therms were recorded (Fig. 4a). The specific surface
area was calculated using the Brunauer–Emmett–Teller
(BET) method from adsorption branch of isotherm in p /
p o range of 0.1–0.2 (Table 1). The isotherms of all
samples resemble type IV isotherm with hysteresis in
the p /p o range of 0.5–0.99 [41]. The adsorption–desorp-
tion loop indicates the presence of mesopores in the
samples. Barreett–Joyner–Halenda (BJH) curves from
desorption branch of isotherms are presented in
Fig. 4b. The sample F300 exhibits pores with a pore
size distribution of 8.3 nm. The BET surface area is
74 m2 g−1 highlighting the overall formation of nano-
structure. The pore volume and surface area of α-Fe2O3
samples decrease with an increase of preparation tem-
perature. Consequently, the pore diameter increases as
the temperature increases.
Electrochemical studies of α-Fe2O3 were reported in
several electrolytes, and it was found that an aqueous
solution of Na2SO3 is the most suitable in the view of
the maximum SC measured [18, 19, 21, 22, 24, 29].
Accordingly, 0.5 M Na2SO3 solution is used for electro-
chemical characterization in the present studies also.
Figure 5a shows typical CVs of α-Fe2O3 electrodes in
the potential range from −0.8 to 0.0 V at 25 mV s−1. CVs
of F300 at different scan rates (5–200 mV s−1) are shown in
Fig. 5b. The shape of CV curves suggests the pseudocapacitance
characteristic of α-Fe2O3, which is distinguishable from
J Solid State Electrochem

Fig. 4 a N2 adsorption–
desorption isotherms and b BJH
pore-size distribution curves of
α-Fe2O3 annealed at different
temperatures

rectangular shape of the electric double-layer capaci- (Fig. 5b). As suggested by Wu et al. [18], the capaci-
tance [42]. There is a decrease in current of CV for tance of α-Fe2O3 in Na2SO3 aqueous solution arises
α-Fe2O3 samples prepared with increasing temperature from the surface redox reaction of sulfur in the form
(Fig. 5a). The current increases with increasing scan rate of sulfate and sulfite anions. Furthermore, the possible

Table 1 Structure type, surface

area (S BET), and specific capaci- Sample BET surface Average pore Cumulative pore Specific capacitance
tance (F g−1) of α-Fe2O3 nano- area (m2 g−1) diameter (nm) volume (cm3 g−1) (F g−1) at 1 A g−1
structures at different
temperatures F-300 74 8.3 0.017 193
F-400 39 25.3 0.012 100
F-500 27 37.6 0.004 60
F-600 19 56.8 0.003 37

Fig. 5 Cyclic voltammograms of
α-Fe2O3 nanostructures a at
25 mV s−1 for samples annealed
at different temperatures and b at
different scan rates (5–100 mV
s−1) for the sample F300 in 0.5 M
Na2SO3
redox reaction between FeII and FeIII is accompanied by
adsorption of sulfite ions for charge balance on iron
oxide [21, 22].
Galvanostatic charge–discharge curves of α-Fe2O3
electrodes (F300) at different current densities are pre-
sented in Fig. 6a. The shape of the charge and dis-
charge curves also indicates capacitive behavior of α-
Fe2O3, in agreement with the data of CV curves. The
SC values of F300 sample evaluated from the discharge
curves are 193, 120, 109, 97, and 90 F g−1 at specific
current of 1, 2, 3, 4, and 5 A g−1, respectively. These
values are high in comparison with the values reported
J Solid State Electrochem
in the literature [27–29] for Fe2O3 samples. For in-
stance, Wang et al. [27] reported SC of 116 F g−1 for
mesoporous α-Fe2O3 nanostructures. Recently, Xie et al.
[28] reported a value of 138 F g−1 for α-Fe2O3 nano-
tube arrays. Very recently, we reported an SC of
127 F g−1 for porous flower-like α-Fe2O3 nanostructures
[29]. Thus, an SC of about 193 F g−1 measured in the
present study for α-Fe2O3 is quite attractive. Figure 6b
presents the SC as a function of different discharge
current densities for samples annealed at different tem-
peratures. The SC decreases with the increase of the
discharge current density. A high SC (63 F g −1 )
J Solid State Electrochem

Fig. 6 a Charge–discharge
curves for porous α-Fe2O3
nanostructures (F300) measured
at different current densities and b
specific capacitance as a function
of different discharge current
densities for samples annealed at
different temperatures

obtained at a high current density (12 A g−1) indicates a
high-power capability of α-Fe2O3 of sample F300 pre-
pared in the present study. There is a decrease in SC
with an increase in preparation temperature due to a
decrease in surface area and pore volume. The SC
values for α-Fe2O3 samples are listed in Table 1.
The α-Fe2O3 electrode made of F300 sample was
subjected to long-cycle test (Fig. 7). Galvanostatic
charge–discharge cycling data for the first few cycles
at a current density of 2 A g−1 are also shown in Fig. 7
(inset). The SC slightly decreases from 120 F g−1 at the
beginning of cycling to 110 F g −1 at the end of
1,000 cycles. Thus, the capacity retention after 1,000 cy-
cles is about 92 %. These results demonstrate that α-
Fe2O3 electrodes exhibit excellent cycling stability and
high degree of reversibility on repetitive charge–dis-
charge cycling. The capacitance retention upon electro-
chemical cycling is strongly attributed to the nature of
porous α-Fe2O3 possessing high surface area and utili-
zation of electrode material.
EIS is employed to study the electrochemical behav-
ior of the electrode. Figure 8 shows the Nyquist imped-
ance plot of the α-Fe2O3 electrode in the frequency
range from 100 kHz to 0.01 Hz with an excitation
 J Solid State Electrochem

Fig. 7 Average specific

capacitance versus cycle number
at galvanostatic charge–discharge
at a constant current density of 2
A g−1 and the inset shows first
few charge–discharge cycles
curves at a current density of 2
A g−1

signal of 5 mV at open circuit potential (−0.34 V). The
equivalent circuit used for fitting the spectrum is shown
as inset. The high-frequency intercept with the real axis
and depressed semicircle correspond to the electrolyte
resistance (R s) and interfacial charge-transfer resistance
(R ct ), respectively. The double-layer capacitance is
replaced by a constant phase element (CPE 1) because
of a depressed semicircle. CPE 2 represents capacitor
behavior at low-frequency region. The sample F300
has minimum R ct value, suggesting that α-Fe2O3 pre-
pared at 300 °C is superior to the other samples as a
supercapacitor material.

Fig. 8 Nyquist plots of the α-

Fe2O3 nanostructures electrodes.
The inset is the equivalent circuit
J Solid State Electrochem
Conclusions
Porous α-Fe2O3 nanostructures were prepared and the effect
of preparation temperature on the morphology, electrochemi-
cal and structural properties, and stability upon cycling
was studied for supercapacitor application. The α-Fe2O3
sample prepared at 300 °C exhibits better capacitance
performance than those prepared at higher temperatures.
There was a gradual decrease in SC for the samples
prepared at higher temperatures due to a decrease in
surface area and pore volume.
Acknowledgments S S and T R P acknowledge the financial support
from the University Grant Commission (UGC), Government of India,
under Dr. D.S. Kothari fellowship program [Ref. No. F.4-2/2006(BSR)/
13-626/2012(BSR)] and senior research fellowship, respectively.
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