Journal of Materials Science: Materials in Electronics (2020) 31:5738–5745

https://doi.org/10.1007/s10854-020-03142-y

Microwave combustion synthesis of tin oxide-decorated silica

nanostructure using rice husk template for supercapacitor
applications
R. Vijayan1,4 · G. Suresh Kumar2 · Gopalu Karunakaran3 · N. Surumbarkuzhali4 · S. Prabhu5 · R. Ramesh5

Received: 12 November 2019 / Revised: 13 February 2020 / Accepted: 17 February 2020 / Published online: 28 February 2020
© Springer Science+Business Media, LLC, part of Springer Nature 2020

Abstract
Supercapacitors are emerged as leading energy storage device and developing new electrode materials for supercapacitors
has received much scientific interest from the researchers. In this study, we have synthesized tin oxide-decorated amorphous
silica ­(SnO2@RH-SiO2) nanostructures using rice husk template as a silica source via simple microwave combustion method
for supercapacitor applications. XRD, FT-IR, and EDX studies obviously characterize that silica is present in amorphous
form along with crystalline ­SnO2 having a rutile tetragonal structure in the prepared ­SnO2@RH-SiO2 sample. Further, TEM
observation indicates that prepared sample is consisting of amorphous silica nanospheres decorated with agglomerated tin
oxide nanoparticles having size of 5–10 nm. Cyclic voltammetry and galvanostatic charge/discharge studies characterize the
supercapacitive behavior of working electrode fabricated from prepared S ­ nO2@RH-SiO2 nanostructure. The specific capaci-
tances of ­SnO2@RH-SiO2 nanostructure are about 448, 330, 275, 240, 225, and 200 F/g with the current density value of 1, 2,
4, 6, 8, and 10 A/g, respectively. The presence ­SnO2 species in ­SnO2@RH-SiO2 nanostructure can provide reactive surfaces
for the adsorption/desorption charges and it facilitates the charge storage at the surface of sample. The above results sug-
gested that the prepared ­SnO2@RH-SiO2 nanostructure has potential application for making electrochemical supercapacitors.

1 Introduction device that can be mostly used in hybrid electric vehicles,

Energy crisis and global warming have triggered the devel-
opment of new energy storage systems. In recent years,
supercapacitors are emerged as leading energy storage
* G. Suresh Kumar
gsureshkumar1986@gmail.com
* N. Surumbarkuzhali
nsurumbar_kuzhali@yahoo.co.in
1
Department of Physics, Padmavani Arts and Science College
for Women, Salem, Tamil Nadu 636 011, India
2
Department of Physics, K.S. Rangasamy College
of Arts and Science (Autonomous), Tiruchengode,
Tamil Nadu 637 215, India
3
Biosensor Research Institute, Department of Fine Chemistry,
Seoul National University of Science and Technology
(Seoul Tech), Gongneung‑ro 232, Nowon‑gu, Seoul 01811,
Republic of Korea
4
Department of Physics, Government Arts College
(Autonomous), Salem, Tamil Nadu 636 007, India
5
Department of Physics, Periyar University, Salem,
Tamil Nadu 636 011, India
memory devices, uninterruptible power supply (UPS), light
emitting diode (LED), flashlights owing to their unique fea-
tures like fast charge and discharge rate, long cycle life, high
power density, high reliability, etc [1–3]. Supercapacitors
can be categorized into two types based on charging mecha-
nism: First one is pseudocapacitor and it is working based
on Faradaic reactions at the surfaces of electrode materials
and the second one is electrical double-layer capacitors that
store the energies via reversible ion adsorption at the elec-
trolyte and electrode surface [3, 4]. Specific characteristics
of the electrode materials will play an important role on
the performance of supercapacitor [2, 3]. Hence, developing
new electrode materials with enhanced performance rela-
tive to conventional materials has received much scientific
attention from the researchers. Last few decades, much inter-
est is focused on nanotechnology where the materials are
manipulated at nanoscale to acquire novel properties over
the conventional materials. Various nanostructures materi-
als such as metal nitrides, metal oxides, carbon, graphene,
carbon nanotube (CNT), metal-organic frameworks, con-
ducting polymers, and so on have been attempted in order
to produce the supercapacitors with enhanced performance

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Journal of Materials Science: Materials in Electronics (2020) 31:5738–5745
[1–4]. Owing to advantages like non-toxic, lower-cost, better
chemical stability, suitable band gap, and favorable electro-
chemical performance, tin oxide (­ SnO2) has received much
attention from researchers for making the electrodes for
supercapacitors [5, 6]. Also, tin oxide nanoparticles have
potential applications in catalyst, lithium-ion batteries, solar
cells, sensors, and so forth [6–10]. Tin oxide crystallizes in
the tetragonal rutile structure at ambient condition and its
applications in above are mainly depending on particle size,
morphology, and composition [6]. Recently, tin oxide-based
nanocomposites such as polyaniline/SnO2 [11], ­SnO2/gra-
phene [12, 13], CNT/tin oxide [14], tin oxide/carbon [15],
and manganese oxide/SnO2 [16] systems have been widely
investigated to prepare electrode for supercapacitors with
improved performance.
On the other hand, rice husk-derived silica-based materi-
als have been focused for making Li-ions batteries, catalyst,
refractory, and biomedicine due to bioavailability, non-toxic-
ity, and low costs [17–20]. Also, it is considered as potential
material for making electrode towards supercapacitor appli-
cations. Leonard et al. reported that capacitance of carbon
electrodes was improved when silica nanoparticles used as
fillers in carbon matrix [21]. Wei et al. prepared silica-doped
nanopolyaniline-based electrode with better cycling stabil-
ity [22]. However, very few articles are available on silica
nanoparticles for making supercapacitor electrodes owing
to its poor electron transfer reactions on the surface and
wide band gab. Joshi et al. developed a facile approach to
generate active sites (oxygen vacancy) in silica nanostruc-
tures to attain electrode with enhanced energy storage [23].
Also, silica-decorated carbon, silica@manganese silicate,
and ­Co3O4/SiO2 systems were studied for making superca-
pacitor electrode [24–26]. Consequently, the present work is
focused on the synthesis of tin oxide-decorated amorphous
silica nanostructures using rice husk as silica source for
supercapacitor applications.
Fig. 1  Schematic for synthesis
of tin oxide-decorated amor-
phous silica nanostructure using
rice husk template-assisted
microwave combustion method
5739
2 Materials and methods
2.1 Preparation of tin oxide‑decorated silica
nanostructure using rice husk template
Chemicals such as tin chloride ­(SnCl2) and ammonia solu-
tion ­(NH4OH, 25%) were procured from Merck, India. Dou-
ble distilled water was employed to prepare the solutions
from above chemicals for reaction. Tin oxide-decorated
amorphous silica nanostructure was prepared using rice
husk template-assisted microwave combustion method as
follows. Briefly, 100 ml of 1M of tin chloride solution was
prepared using double distilled water and 10 g of rice husk
was added with the prepared tin chloride solution under con-
stant stirring. Then, ammonia (­ NH4OH) solution was added
dropwise with stirring in the above mixture until it reaches
pH 10. After stirring for 1 h, the prepared precipitate was
transferred into 2.2 KW microwave furnace and heated at
500 °C for 5 h using microwave irradiations. Then, obtained
product was named as ­SnO2@RH-SiO2. The schematic for
the synthesis of tin oxide-decorated amorphous silica nano-
structure using rice husk template-assisted microwave com-
bustion method is shown in Fig. 1. Moreover, 10 g raw rice
husk was heated in the microwave furnace at 500 °C for 5 h
for comparison and it was named as RH-SiO2.
2.2 Characterization of samples
The crystalline nature of prepared samples was analyzed via
X-ray diffraction (XRD) on a PANanalytical X’Pert PRO
instrument attached with Cu-Kα X-ray source (λ = 1.5406
Å). Fourier transform infrared (FT-IR) spectrum of KBr-
supported samples in pellet form was recorded in the
4000–400 ­c m −1 region using BRUKER TENSOR 27
spectrometer. Nanoscale characteristics of prepared sam-
ples were analyzed JSM JEOL-2100 transmission electron
microscope (TEM). Elemental composition was obtained
13
5740
using energy-dispersive X-ray (EDX) analyzer attached in
TESCAN VEGA3 scanning electron microscope (SEM).
2.3 Electrochemical studies
The electrochemical performance of the prepared ­SnO2@
RH-SiO2 electrode was evaluated using a software-con-
trolled conventional three-electrode electrochemical work-
station (BioLogic SP-150 Science Instruments, France) at
room temperature. Pt wire was utilized as the counter elec-
trode whereas Ag/AgCl was employed as reference elec-
trode. 0.5M N­ a2SO4 was used as electrolyte. S ­ nO2@RH-
SiO2-coated Ni foam was employed as a working electrode.
The working electrodes were prepared as follows: Briefly,
­SnO2@RH-SiO2 (80 wt%), polyvinylidene fluoride (10 wt%
), and carbon black (10 wt%) were mixed well with 2 ml of
ethanol using morter with pestle to get fine slurry. Then, the
obtained slurry was pasted on Ni foam and dried for 12 h
at 80 °C in a vacuum oven. The cyclic voltammetry (CV)
­ nO2@RH-SiO2 electrode was studied
behavior of prepared S
in between 0 and 1V with 5–100 scan rates. Galvanostatic
charge–discharge (GCD) behavior of S ­ nO2@RH-SiO2 elec-
trode was analyzed between 1 and 10 A g­ −1 with 0 to 0.8 V
potential window. Electrochemical impedance was analyzed
from 0.1 Hz to 100 kHz at 5 mV open circuit potential.
3 Results and discussion
Figure 2a revealed the XRD pattern of the prepared rice husk
ash, which clearly shows a broad diffraction peak in between
15 and 30°. It indicates that the rice husk ash is constituted
of amorphous silica [27, 28]. Figure 2b presents the XRD
Fig. 2  XRD pattern of prepared samples (a) Rice husk ash (RH-SiO2)
and (b) S­ nO2@RH-
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Journal of Materials Science: Materials in Electronics (2020) 31:5738–5745
pattern of the prepared S ­ nO2@RH-SiO2 sample. The 2θ
values of diffraction peaks were compared with Joint Com-
mittee on Powder Diffraction Standards (JCPDS) data of
­SnO2 (JCPDS file No. 41-1445). XRD pattern shows (110),
(101), (200), (211), (220), (002), (221), (112), (301), (320),
and (321) Miller’s planes of ­SnO2 at 2θ values of 26.77°,
34.17°, 38.17°, 52.02°, 55.02°, 58.27°, 62.12°, 64.97°,
66.17°, 71.72°, and 79.12°, respectively [7–10]. It clearly
characterizes that crystalline phase present in the ­SnO2@
RH-SiO2 sample is S ­ nO2 having rutile tetragonal structure.
The calculated unit cell parameters for S ­ nO2 present in the
­SnO2@RH-SiO2 sample is a = 4.729 Å, c = 3.186 Å, and
V = 71.27 Å3 , which is well matched with literature data
[7–10]. It is important to mention that a broad hump between
15 and 30° owing to the presence of amorphous silica nano-
particles is not visible due to the high crystalline nature of
­SnO2 nanoparticles formed on the surface of amorphous
silica nanoparticles [27, 28].
The FT-IR spectrum of rice husk ash (RH-SiO2) is pre-
sented in Fig. 3a. A band located between 1056 and 1078
­cm−1 is attributed to the O–Si–O asymmetric stretching
vibration. A peak between 790 and 800 ­cm−1 is ascribed to
the O–Si–O symmetric stretching vibration. A peak located
around 440–450 ­cm−1 is owing to the Si–O bending vibra-
tion. These three peaks revealed the presence of silica in rice
husk ash [29–32]. The broad band located between 3000 and
3700 ­cm−1 is ascribed to the stretching vibration of water
molecules. A strong peak observed at 1640 ­cm−1 is due to
the bending vibration of water molecules [7, 9, 10]. The
peaks located at 2844 and 2918 ­cm−1 are due to the symmet-
ric and asymmetric C–H bonds, respectively. The peaks at
1375 ­cm−1 (C–O), 1450 ­cm−1 (C–H), and 2350 ­cm−1 (C–O)
are originated from organic residue present in the sample
[29–32]. Hence, FT-IR spectrum clearly confirms that H ­ 2O
Fig. 3  FT-IR spectrum of prepared samples (a) Rice husk ash (RH-
SiO2) and (b) ­SnO2@RH-SiO2
Journal of Materials Science: Materials in Electronics (2020) 31:5738–5745 5741

and organic residue may be present in rice husk ash. The behavior of S ­ nO 2@RH-SiO 2 nanostructure [11–16, 33,
FT-IR spectrum of ­SnO2@RH-SiO2 sample is presented in 34]. This behavior is due to the presence of ­SnO2 species
Fig. 3b. It shows a peak at 638 c­ m−1 along with above peaks in ­SnO2@RH-SiO2 nanostructure that can provide reactive
[7–10]. It revealed that silica is present in amorphous form surfaces for the adsorption/desorption charges on working
along with ­SnO2 in the prepared ­SnO2@RH-SiO2 sample. electrode in neutron electrolyte as follows [33].
Figure 4a shows the EDX spectrum rice husk ash (RH-
SiO2). It clearly indicates that rice husk ash is abundant of (SnO2 ) surface + Na + + e− ↔ (SnO−2 - Na + ) surface
silicon (40.10%) and oxygen (52.90%) with carbon (7%)
The above reactions can facilitate the charge storage at
impurity. The EDX spectrum of ­SnO2@RH-SiO2 sample is
­SnO2@RH-SiO2 sample. The GCD of the working elec-
shown in Fig. 4b, which clearly illustrates the presence of
trodes at different current density is shown in Fig. 6b. It
tin (22.30%), silicon (28.80%), and oxygen (45.90%) with
clearly indicates that charge/discharge curves are asym-
carbon (3%) impurity. Elemental mapping is shown as inset
metric and it represents a typical electric double-layer
in Fig. 4, which evidently demonstrates the elemental dis-
(EDLC) behavior of electrode material. The specific
tribution in RH-SiO2 and ­SnO2@RH-SiO2 nanostructure.
capacitances (Cs) of S
­ nO2@RH-SiO2 electrode were deter-
TEM images of rice husk ash (RH-SiO2) at different
mined from GCD curve using the below relation [11–16]
magnifications are shown in Fig. 5a and b. It shows loosely
agglomerated silica nanospheres with different circumfer- IΔt
Cs =
ence. The size of nanosphere was approximately calculated mΔV
as 30 ± 10 nm. Figure 5e shows the SAED pattern of RH-
Here, m is the mass of S ­ nO2@RH-SiO2 nanostructure
SiO2, which evidently indicated that rice husk-derived silica
in working electrode (g), I indicates the charge–discharge
nanospheres are amorphous in nature. Figure 5c and d shows
current (A), ΔV is the electrochemical potential window,
TEM images of S ­ nO2@RH-SiO2 sample. It is important to
and Δt represents discharged time (s). The correlation
note that silica nanospheres were decorated with agglomer-
of specific capacitance and current density is shown in
ated tin oxide nanoparticles having size of 5–10 nm. SAED
Fig. 6c. The specific capacitances are about 448, 330,
pattern shown in Fig. 5f illustrates the polycrystalline nature
275, 240, 225, and 200 F/g at 1, 2, 4, 6, 8, and 10 A/g,
of individual S­ nO2 nanoparticles formed on surface of amor-
respectively. The specific capacitance was decreased when
phous silica nanosphere.
the current density increased which may be due to poor
Figure 6a illustrates the CV profile of the S ­ nO2@RH-
electrochemical reaction at high current density [11, 12,
SiO2 nanostructure at the different scan rate with 0 to 1 V
32–34]. Recent progress in the synthesis of ­SnO2-based
potential window. It clearly depicts the faradic behavior
nanocomposites using various methods for supercapaci-
of working electrode that consists of the ­SnO2@RH-SiO2
tor applications is summarized in Table 1. It clearly dem-
nanostructure. It is important to note that that CV curves
onstrates that electrolyte, phase composition, nanoscale
observed at different scan rate are quasi rectangular and
characteristics of the materials, and current density
symmetrical in nature indicating the excellent capacitive

Fig. 4  EDX spectrum of synthesized samples a Rice husk ash (RH-SiO2) and b ­SnO2@RH-SiO2 sample

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Fig. 5  TEM images of prepared

samples at different magnifica-
tions and corresponding SAED
pattern a, b, and e rice husk
ash (RH-SiO2), and c, d, and f
­SnO2@RH-SiO2

play a crucial role on maximum specific capacitance of
­SnO2-based nanocomposites.
Electrochemical impedance of prepared electrodes was
analyzed in between 0.01 Hz and 100 kHz, and it shows
capacitive behavior and ion diffusion nature of ­S nO 2@
RH-SiO2 electrode. The electrochemical impedance spec-
trum (EIS) of ­SnO2@RH-SiO2 electrode (Fig. 6d) shows
a semicircle in high-frequency region and linear slope at
low-frequency region. The equivalent circuit is shown as
inset in Fig. 6d. In practical applications, supercapacitors
should have the good cyclic stability property. Figure 6e
shows the long-time cycling stability of the as-prepared
­SnO2@RH-SiO 2 electrode performed by 7000 cycles of
GCD analysis at 10 ­Ag−1. The ­SnO2@RH-SiO2 electrode
revealed excellent stability after 7000 cycles with the
capacitance retention of 97%. The obtained results from
the above studies clearly indicate that the prepared mate-
rial ­(SnO2@RH-SiO2) has a promising application in elec-
trochemical supercapacitors.

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Journal of Materials Science: Materials in Electronics (2020) 31:5738–5745 5743

Fig. 6  a Cyclic voltammetry (CV) profile, b Galvanostatic charge and discharge behavior, c Correlation between current density and specific
capacitance, d Electrochemical impedance spectrum, and e Cyclic retention of ­SnO2@RH-SiO2 nanostructure

4 Conclusion amorphous silica ­(SnO2@RH-SiO2) nanostructures using

rice husk template as a silica source. The prepared sample
In this work, we have developed a facile and rapid micro- was characterized by XRD, FT-IR, TEM, and EDX tech-
wave combustion method to prepare tin oxide-decorated niques to know the phase purity and nanoscale features.

13
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Table 1  Recent progress in the synthesis of ­SnO2-based nanocomposites using various methods for supercapacitor applications
S. No Authors and year Materials Electrolyte Maximum Refs.
Specific capaci-
tance (F/g)

1 Hu et. al. (2009) Polyaniline/SnO2 nanocomposite 1 M ­H2SO4 305.3 [11]

2 Yan et. al. (2010) Manganese oxide coated tin oxide nanowires 1MN ­ a2SO4 800 [16]
3 Li et. al. (2012) Single walled carbon nanotube with 1 M ­Na2SO4 320 [35]
SnO2
4 Ren et. al. (2014) Tin oxide/carbon 1 M KOH 25.8 [36]
nanocomposite
5 Chen et. al. (2015) SnO2-decorated graphene/polyaniline nanocomposite 1M ­H2SO4 429 [34]
6 Velmurugan et. al. (2016) SnO2/graphene nanocomposite 6 M KOH 818 [12]
7 Ramesh et. al. (2019) SnO2@NiCo2O4/nitrogen-doped multiwalled 6 M KOH 728 [37]
carbon nanotube hybrids
8 Present work Tin oxide-decorated silica nanostructure 0.5 M N
­ a2SO4 448 –

The acquired results from various characterizations con-
firm the formation of tin oxide-decorated amorphous silica
nanostructures. The specific capacitance of ­SnO2@RH-
SiO2 nanostructures was analyzed through electrochemi-
cal measurements and the results showed that the specific
capacitances are about 448, 330, 275, 240, 225, and 200
F/g at the current density of 1, 2, 4, 6, 8, and 10 A/g. The
presence ­SnO2 nanoparticles on rice husk-derived silica
nanosphere can provide reactive surfaces for the adsorp-
tion/desorption of charges and it can facilitate the charge
storage at a surface of the sample. Hence, prepared S­ nO2@
RH-SiO2 nanostructure could be used for making electro-
chemical supercapacitors. Moreover, this study could be
useful for recycling the rice husk biomass to prepare the
valuable product.
Acknowledgements G. Suresh Kumar would like to express his sin-
cere thanks to University Grant Commission, India, for financial sup-
port through minor research project scheme (File No: 4–4/2015-16
(MRP/UGC SERO)). Gopalu Karunakaran would like to express his
sincere thanks to the Ministry of Science and ICT through the National
Research Foundation of Korea for financial support through the Korean
Research Fellowship (KRF Grant No. 2018H1D3A1A01037054).
The Authors also acknowledge the supports under the Basic Science
Research Program through the National Research Foundation of Korea
funded by the Ministry of Education (NRF-2019R1I1A1A01062458).
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