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Bull. Mater. Sci. _#####################_

https://doi.org/10.1007/s12034-023-03099-8 Sadhana(0123456789().,-volV)FT3](012345
6789().,-volV)
Ó Indian Academy of Sciences

Structural, electrochemical and corrosion resistance properties

of ZnO/rGO nanocomposite for supercapacitor electrode material

SAGOLSEM NONGANBI CHANU, SHUBHAM JHA, PUKHRAMBAM SUSHMA DEVI

and BIBHU PRASAD SWAIN*
Department of Physics, National Institute of Technology Manipur, Imphal 795004, India
*Author for correspondence (bibhuprasad.swain@gmail.com; bpswain@nitmanipur.ac.in)

MS received 2 March 2023; accepted 31 August 2023

Abstract. In this work, zinc oxide/reduced graphene oxide (ZnO/rGO) nanocomposites have been synthesized by a
chemical reduction approach with different concentrations of ZnO. The morphology, structural, optical and electro-
chemical, and corrosion properties characterizations of the synthesized ZnO/rGO nanocomposite were analysed. From
XRD, the crystalline size of rGO was found to be 0.28 nm and the average crystallite size for the ZnO/rGO composite was
found to be 36.62–30.56 nm from 5 and 7 wt%. The maximum specific capacitance of 7 wt% of ZnO/rGO was found to be
848 F g–1 at a scan rate of 10 mV s–1 with the potential window range of –0.3 to 0.3 in 1 M KCl as the electrolyte, when
compared for GO. The cyclic stability of the specific capacitance was tested for 1000 cycles at 5 A g–1 current density, the
result shows good cyclic stability, with a retention rate of 60.7%. The minimum values of corrosion potential (Ecorr) and
corrosion current (Icorr) are 0.012 V and 2.17 A. The ZnO/rGO nanocomposite demonstrated high specific capacitance and
strong supercapacitor capabilities.

Keywords. ZnO/rGO; nanocomposite; reduced graphene oxide; supercapacitor.

1. Introduction material. rGO can enhance the properties of ZnO nanofibres

The zinc oxide (ZnO) and reduced graphene oxide (rGO)
nanocomposites have widely received a lot of attention
because of their environment friendly, low cost, improved
corrosion resistance and better electrochemical properties,
which are considerably different from those of individual
materials. Zinc oxide is a direct bandgap semiconductor
having a bandgap of 3.4 eV and it has a wurtzite structure [1].
ZnO has remarkable properties as a semiconductor material,
such as high optical, electrical and piezoelectric performance.
It also has high electron mobility, and excellent chemical
stability. These features make ZnO suitable for various
applications in optoelectronics, sensors and energy conver-
sion systems. However, ZnO nanofibres face some chal-
lenges, such as poor dispersion and aggregation. Graphene
oxide (GO) is a promising material for supercapacitor elec-
trodes due to its unique characteristics, such as its morphol-
ogy, high electrical conductivity, large surface area,
exceptional mechanical strength and chemical stability. In
addition, the combination of electric double-layer capaci-
tance (EDLC) and pseudocapacitance in the reduced GO and
metal oxide materials results in improved electrochemical
performance. Reduced graphene oxide (rGO) is obtained
from graphene oxide by a reduction process that restores the
sp2 carbon network and gives electrical conductivity to the
by improving their electrical conductivity, mechanical
strength and surface area, leading to better device perfor-
mance. Moreover, the nanofibres composed of ZnO, rGO and
PCL have a wide range of potential applications in flexible
electronics, energy storage devices, photocatalysis and sen-
sors. The unique properties of each component add to the
overall performance of the nanofibres, making them highly
adaptable and versatile for different applications [2]. Rod-
wihok et al [3] synthesized ZnO/rGO nanocomposite using a
simple one-pot solvothermal process, which improved pho-
tocatalytic and photosensitivity activity [3]. According to
Jayachandiran et al [4], ZnO/rGO nanocomposite can reach a
maximum specific capacitance of 312 F g–1 at 5 mV s–1 with a
window potential of 0 to 1 V and exhibit capacitance stability
of 95% over 1000 cycles [4]. The authors Rajeswari et al [5]
employed a hydrothermal synthesis method to fabricate a
graphene–ZnO composite, resulting in a measured capaci-
tance value of 719.2 F g–1 when tested with 3 M KOH as the
electrolyte and a scan rate of 5 mV s–1. [5].
In this study, a straightforward chemical reduction
approach was used to create the ZnO/rGO nanocomposite.
This paper focuses on ZnO/rGO nanocomposite structural,
morphological, optical, electrochemical and anticorrosion
studies. Three electrode setup (Model No. CHI608E)
electrochemical tests were carried out in the potential
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Scheme 1. Schematic illustration for the preparation of ZnO/rGO nanocomposite.
window range of –0.3 to 0.3 V using 1 M KCl as the
electrolyte. The frequency range of the electrochemical
impedance spectroscopy measurements for rGO and ZnO/
rGO nanocomposite is from 1 Hz to 105 Hz.
2. Experimental
2.1 Preparation of graphene oxide
Graphene oxide was synthesized using the Hummer’s
method. Initially, a mixture of 3 g of graphite powder and
66 ml of sulphuric acid (H2SO4) was prepared, and the
magnetic stirring was employed to ensure complete dis-
persion of the graphite powder. Following that, 1.5 g of
sodium nitrite was introduced into the mixture, and mag-
netic stirring was continued for 30 min. To lower the
temperature below 20°C, the solution was then cooled using
an ice bath. While maintaining the temperature below 20°C,
15 g of potassium permanganate (KMnO4) was gradually
added, resulting in the solution turning dark brown. The ice
bath was removed, and the temperature was raised to 35°C
while stirring the solution using a magnetic stirrer for 2 h.
Afterward, 300 ml of deionized water was added to the
solution, and the temperature was further increased to 98°C.
The solution was stirred for an additional 30 min, causing it
to turn dark orange. To terminate the reaction, 20 ml of
hydrogen peroxide was added. The resulting precipitate was
washed multiple times with a 10% HCl solution. Further
washing with distilled water was performed, followed by
drying and crushing of the precipitate to obtain graphene
oxide powder [6, 7].
Bull. Mater. Sci. _#####################_
2.2 Preparation of zinc oxide/rGO nanocomposite
Graphene oxide (GO) was synthesized from graphite using
a modified Hammer’s method. To prepare zinc oxide
(ZnO), zinc nitrate hexahydrate (Zn(NO3)26H2O) was
mixed with 150 ml of distilled water. Sodium hydroxide
pellets (2 g) were dissolved in 25 ml of distilled water, and
the resulting solution was added to the zinc nitrate hex-
ahydrate solution. After stirring the mixture for a few
minutes, it was filtered. The filtrate was then rinsed several
times with distilled water before being stored in a 60°C
oven. Subsequently, the zinc oxide powder was obtained by
crushing and drying the filtrate.
In the next step, 0.2 g of GO was dissolved in DI water,
and zinc oxide was added to the solution. The mixture was
stirred for 2 h before adding 3 ml of hydrazine hydrate. The
resulting solution was repeatedly rinsed with DI water and
left to dry for 3 h. This process was repeated using different
ZnO contents, specifically 5, 7 and 10 wt% of ZnO/rGO
nanocomposites, as illustrated in scheme 1
3. Result and discussions
3.1 Surface morphology and energy dispersive X-ray
analysis
Figure 1 illustrates the high-magnification scanning electron
microscope (SEM) image of a ZnO/rGO composite with
varying ZnO concentrations (5, 7 and 10%). The SEM
image, obtained using Model no. JEOL, IT-100, clearly
reveals the distribution of ZnO nanoparticles in a spherical
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Bull. Mater. Sci. _#####################_
Figure 1. SEM image of ZnO/rGO nanocomposite of 5–10 wt% with energy dispersive X-ray
analysis.
shape on the rGO sheet. The average size of these ZnO
nanoparticles ranges from approximately 5 to 10 lm, with
an average value of 0.35 to 0.45 lm. The surface roughness,
measured by root mean square roughness (Rq) and mean
roughness (Ra), increases with the increase in ZnO con-
centration, ranging from 235.6 to 263.7 nm for Rq and 200
to 281.5 nm for Ra. This increase in surface roughness is
also supported by the results of the cyclic voltammetry
(CV) analysis, which indicates an increase in specific
capacitance. Furthermore, the presence of carbon, oxygen
and zinc in the ZnO/rGO composite is confirmed through
Page 3 of 9 _####_
energy-dispersive X-ray (EDX) analysis. The weight per-
centages of carbon, oxygen and zinc are found to be in the
ranges of 67.78–63.47–48.49%, 16.83–18.79–18.20% and
15.39–17.75–33.3%, respectively. The atomic percentages
of carbon, oxygen and zinc are 81.42–78.53–71.02%,
15.18–17.44–20.02% and 3.404.03–8.96%, respectively,
with an increase in ZnO concentration. This observation
suggests that as the concentration of ZnO increases, the
atomic percentage of carbon decreases, while that of oxygen
increases, indicating the presence of excess oxygen in the
ZnO/rGO nanocomposites. Moreover, this increase in ZnO
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Figure 2. XRD pattern for GO, rGO, ZnO/rGO nanocomposites
of 5 and 7 wt%.
concentration also results in a homogenous distribution of
carbon, oxygen and zinc elements in the nanocomposites
[8].
3.2 X-ray diffraction
Figure 2 shows the XRD characterization done to charac-
terize GO, rGO and 5–7 wt% of ZnO/rGO nanocomposites
(Bruker D8). Graphene oxide shows a broad peak at
2h = 10.04° corresponding to the plane (001). After the
reduction of graphene oxide to reduced graphene oxide by
hydrazine treatment, rGO shows a peak at 2h = 23.5 for the
plane (002). XRD peak of ZnO nanoparticle was found at,
2h = 32.67°, 35.11°, 36.84°, 45°, 55.78°, 64.49° and 72.55°
corresponding to (100), (002), (101), (102), (110), (103) and
(112) diffraction planes (JCPDS-36-1451). The diffraction
peaks shown by zinc oxide correspond to the wurtzite
structure. The crystallite size was calculated by using
Scherer’s equation (1) [9].
Kk
Dhkl ¼ ð1Þ
bhkl cosh
where Dhkl is crystal size, K denotes Scherer’s constant, bhkl
denotes the full-width half-maximum (FWHM) and h
denotes Bragg’s angle. The average size of the rGO crystals
in the (002) plane was 0.28 nm. The ZnO/rGO (zinc oxide/
reduced graphene oxide) composite had smaller crystals,
ranging from 30.56 to 36.62 nm for 5–7 wt% of ZnO. This
is because more ZnO nanoparticles create more sites for
crystals to grow. Smaller crystals have more surface energy
than larger ones. More ZnO nanoparticles mean more high-
energy surfaces. The system prefers to reduce the surface
area by forming smaller crystals. The distance between the
[10] planes of ZnO nanoparticles was 0.3–0.56 nm for 5 and
7 wt% of ZnO/rGO composite. This shows that adding ZnO
Bull. Mater. Sci. _#####################_
nanoparticles changes the lattice structure of the composite.
ZnO has a smaller lattice parameter than rGO, and the
lattice of the composite becomes more like ZnO as its
concentration increases. Also, more ZnO nanoparticles
make them interact more with rGO sheets. This makes the
bonding and packing between ZnO nanoparticles and rGO
sheets stronger and tighter. This leads to a smaller d-spacing
in the composite.
3.3 UV–visible spectroscopy
Figure 3a shows the UV–visible spectra of GO and ZnO/
rGO nanocomposites of different weight percentages of zinc
oxide and reduced graphene oxide. Graphene oxide shows a
maximum absorption peak at 224 nm due to the p–p*
transition of atomic C=C bonds. After reduction by hydra-
zine, rGO shows an absorption peak at 266 nm and zinc
oxide shows its characteristic absorption peaks at 365.7 and
418.2 nm due to intrinsic bandgap electron–hole recombi-
nation and the other one is due to surface oxygen defects or
vacancies [10–12]. Figure 3b shows the bandgap calculated
for different ZnO/rGO nanocomposites using Tauc’s plot
varies from 1.8, 1.82 and 1.86 eV for 5–10 wt% [13]. This
increase is due to the increase in surface charges between
ZnO and rGO and which results in the optical bandgap
shifting to a higher wavelength.
3.4 Photoluminescence spectroscopy
Figure 4 shows the wavelength vs. intensity plots for pho-
toluminescence (PL) spectra for rGO and ZnO/rGO (3.6 eV
excitation energy) nanocomposites (Model no.VGESCA-
LABMK II). rGO shows a high peak at 396 (3.13 eV) nm
and this peak is also visible in all of the nanocomposites
contributed to the p–p* band transition. This peak is due to
the recombination of the hole and electron. The other two
peaks at 466 nm (2.6 eV) and 492 nm (2.52 eV) are due to
oxygen in the sample [13]. As the percentage of zinc oxide
is increased, the intensity increases. In PL electron–hole
pairs are formed due to excitation by the photons and these
electron–hole pairs recombine, this improves the efficiency
of separating photo-excited electron–hole pairs produced
from ZnO and enhances the overall transfer of charge car-
riers [14].
3.5 Electrochemical analysis
In figure 5a, CV curves were obtained for rGO and ZnO/
rGO nanocomposites with varying concentrations of ZnO
(5–10 wt%) in 1 M KCl electrolyte at scan rates ranging
from 10 to 50 mV s–1. The rectangular shape of the oxi-
dation–reduction peaks seen in the ZnO/rGO nanocom-
posites indicates their faradic redox performance of
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Figure 3. (a and b) UV–visible spectra and Touc plots of ZnO/rGO nanocomposites for different concentrations of ZnO
from 5 to 7 wt%.
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Figure 4. PL spectra for GO, rGO, ZnO/rGO nanocomposites for
5–10 wt% of ZnO content.
electrical double-layer capacitances [15]. Specific capaci-
tance values were calculated using equation (2) [8].
ZV2
I dV
CP ¼ ð2Þ
m  vð ðV2  V1 Þ
V1
where CP represents specific capacitance in F g–1 and the
mass of active material (m) [15]. The highest specific
capacitance values were achieved at a scan rate of 10 mV s–1,
reaching 753, 801 and 849 F g–1 for rGO and 5–7 wt% of
ZnO/rGO nanocomposites, respectively, with specific
capacitance values of 597, 563 and 641 F g–1 obtained at
20 mV s–1. At higher scan rates, the specific capacitance for
rGO and ZnO/rGO for 5 and 7 wt% samples decreased due
to a decrease in the charge transfer rate through the elec-
trical double-layer capacitance formed at the electrode–
electrolyte interface, as shown in table 1 [11, 12]. When the
scan rate is increased, the redox peak gets shifted due to
faster scan rates creating diffusion limitations for the redox
species involved in the electrochemical process. When the
scan rate is high, the redox species may not have enough
time to fully participate in the electrochemical reaction,
resulting in incomplete oxidation or reduction at lower
potentials. In addition, at higher scan rates, the ZnO/rGO
nanocomposite might undergo structural modifications or
encounter variations in the electrode/electrolyte interface.
These changes in the interface can influence the adsorption
or desorption of ions and potentially alter the electro-
chemical behaviour of the redox-active species, thereby
causing a shift in the redox peaks.
In figure 5b, the Bode plot is shown for a frequency range
of 100 to 10000 Hz. As the concentration of ZnO increases,
the Bode plots increase gradually and the peak shifts to a
higher frequency. The impedance value remains constant,
with the maximum impedance obtained at the lower fre-
quency region (1 to 100 Hz) and a phase degree (*U) of 0°
[16, 17]. The minimum impedance value, along with the
electrolyte resistance (Re) and maximum phase (Umax)
Bull. Mater. Sci. _#####################_
value, were 14.54 X and 49.6°, respectively. In figure 5c,
the polarization curves were obtained for ZnO/rGO
nanocomposites with varying concentrations of ZnO (5–7
wt%) in a 1 M KCl solution. The cathodic and anodic
polarization branches shift to lower current densities in the
case of rGO compared to ZnO/rGO nanocomposites, with
the shift increasing with increase in ZnO content in the
rGO. The Tafel slopes bc and ba increase with an increase in
ZnO content, with the slopes of ba found to be greater than
the respective cathodic Tafel slopes. These observations are
because the anodic exchange current density values are
greater than those of the cathodic counterparts. In anodic
slopes, ba redox peak was observed which were shifting
with increases in ZnO concentration. The anodic slope (ba)
in the Tafel plot represents the rate of the anodic reaction,
which is the oxidation process occurring at the electrode
surface. In this case, the shifting of the redox peak with an
increase in ZnO concentration suggests a change in the
electrochemical behaviour of the nanocomposite. The shift
in the redox peak can be attributed to several factors,
including changes in the surface area, electron transfer
kinetics and active sites available for the reaction. Fur-
thermore, the presence of ZnO nanoparticles in the
nanocomposite can influence the electron transfer kinetics
at the electrode surface. The interaction between ZnO and
rGO may affect the charge transfer properties, resulting in a
change in the redox peak position. As shown in table 2, the
corrosion potential and current were 0.027, 0.012 and 0.016
V, and 2.17, 2.22 and 2.63 A, respectively, for rGO and
nanocomposites of rGO with 5–7 wt% of ZnO. The
nanocomposite’s overall surface area can be increased by
adding ZnO nanoparticles. More sites that are prone to
corrosion are exposed when the surface area is larger.
Moreover, the surfaces of ZnO nanoparticles may have
flaws and irregularities that can serve as starting points for
corrosion. The corrosion current increases as the concen-
tration of ZnO increases in ZnO/rGO nanocomposites, and
the electrochemical reactions that occur at the nanocom-
posite’s surface can be affected by the presence of ZnO.
ZnO can undergo reduction and oxidation processes, which
may alter the corrosion behaviour of the nanocomposite. In
figure 5d, a constant current of 0.1 mA was applied during
the galvanostatic charge–discharge process. The specific
capacitance (Csp) was calculated using equation (3), which
takes into account the current density (I) applied on rGO
and rGO–ZnO nanocomposite with varying concentrations
of ZnO (5–7 wt%), discharge time (Dt), potential window
(DV), and total mass of active material (m).
I:Dt
CSP ¼ ð3Þ
DV:m
According to the data obtained from galvanostatic
charge–discharge analysis, the nanocomposites 5 A g–1,
rGO and ZnO/rGO exhibit specific capacitances of 316, 625
and 916 F g–1, respectively. Equations (4 and 5) can be used
to calculate the specific energy (E) and power density of the
Bull. Mater. Sci. _#####################_
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(d) (e)
0.4 -1 rGO 1000
5 Ag 5ZnO/rGO
rGO
0.3
Specific capacitance (F/g)

7ZnO/rGO 848
801
7ZnO/rGO
800 753 5ZnO/rGO
0.2
Voltage (V)

641
0.1 600 597
563 563

479
0.0 459
401 406 399
400 342 353 357
-0.1

-0.2 200

-0.3
0
-100 0 100 200 300 400 500 600 700 800 10 20 30 40 50
Time (s) Scan rate (mV/s)

(f) (g)
3500
96 5 ZnO/rGO
3000

2500 84
5ZnO/rGO
% retension

7ZnO/rGO
-Z"/ ohm

2000 rGO 72
1500
60 60.7%
1000

500 48

0 36
0 1000 2000 3000 4000 5000
0 200 400 600 800 1000
Z'/ ohm No. of cycles
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b Figure 5. Electrochemical capacitance of different wt% of ZnO
varying from 5 to 10 wt% of ZnO/rGO nanocomposites. (a) Cyclic
voltammetry, (b) Bode plot, (c) Tafel plot, (d) Galvanostatic
charge–discharge, (e) scan rate vs. specific capacitance, (f) Nyquist
plot and (g) cyclic stability of 5 wt% ZnO/rGO.
supercapacitor device from the galvanostatic charge–dis-
charge results.
10000  CSP  ðDV Þ2
E¼
2  3600
E stability of the specific capacitance was tested for 1000
P ¼  3600
Dt
Upon investigation, specific energy values of 15.8, 31.25
and 45.8 Wh kg–1 were obtained for rGO, 7ZnO/rGO and
5ZnO/rGO nanocomposites, respectively. Moreover, power
density values of 1496, 1500 and 1351 W kg–1 were
observed for the respective nanocomposites. The close
contact between rGO and ZnO nanoparticles resulted in a
reduction of ion path length and an increase in electrolytic
ion diffusion rates. This intimate contact led to the
remarkable energy and power density of the nanocompos-
ites. The specific capacitance from CV of rGO and ZnO–
rGO composite electrodes containing 5–7 wt% is plotted
against different scan rates in figure 5e. The specific
capacitance decreases with an increase in scan rate from 10
to 50 mV s–1. This is due to the diffusion limitations that
restrict the movement of electrolyte ions at high scan rates,
and only the outer active surface can be utilized for charge
storage. However, at lower scan rates, the entire active
surface area can be used for charge storage. Additionally,
the specific capacitance values of the 7ZnO–rGO composite
electrode were significantly higher than those of the 5ZnO–
rGO and rGO electrodes for all scan rates. Electrochemical
impedance spectroscopy is a fundamental method used to
investigate the behaviour of electrode materials for super-
capacitors. The electrochemical impedance spectra of rGO
and ZnO–rGO composite electrodes containing 5–7 wt%
are presented in figure 5f. These plots demonstrate a linear
relationship in the low-frequency range, which can be
attributed to the diffusive resistance of the electrolyte
penetrating the electrode’s interior and the transport of ions
to the electrode surface [5]. Conversely, there is a lack of
semicircle in the high-frequency region, which is associated
with the charge transfer-limiting process and the pseudo-
capacitance at the interface between the electrolyte solution
and the electrode [22, 23]. The equivalent series resistance
by determining the X-axis intercepts of the electrochemical
impedance spectra. This equivalent series resistance
includes the resistance of the 1 M KCl aqueous solution, the
intrinsic resistance of the electro-active material, and the
contact resistance between the electrode and the current
collector at their interface. The equivalent series resistance
value of the 7ZnO–rGO (4.2 X) electrode material is con-
ð4Þ siderably lower than that of the 5ZnO–rGO (23.3 X) and
rGO (8.5 X) electrode materials. In figure 5g, the cyclic
ð5Þ
cycles at 5 A g–1 current density, and the result shows good
cyclic stability, with a retention rate of 60.7%.
4. Conclusion
The ZnO/rGO nanocomposites were synthesized by incor-
porating varying weight percentages of ZnO, ranging from
5 to 10% (wt% of ZnO). Remarkably, the highest specific
capacitance was achieved at a scan rate of 10 mV s–1,
yielding values of 753, 801 and 848 F g–1 for rGO, 5% and
7% (wt%) of ZnO/rGO nanocomposites. To evaluate cyclic
stability, the specific capacitance was tested over 1000
cycles at a current density of 5 A g–1, demonstrating
favourable cyclic stability with a retention rate of 60.7%.
Moreover, the PL spectra exhibited enhanced intensity,
displaying peaks at 2.66 and 2.52 eV, which can be attrib-
uted to the transitions of oxygen and trapped water states in
p-bands tail. Notably, the nanocomposites exhibited altered
structural properties, characterized by a smaller crystallite
size compared to pure rGO.
Table 2. Tafel plots were utilized to obtain distinct parameters of
ZnO/rGO nanocomposites at varying concentrations of ZnO.
Sample Ecorr (mV) Icorr (A) ba (V) bc (V)
rGO 0.027 2.17 0.028 0.023
5 ZnO/rGO 0.012 2.22 0.033 0.024
7 ZnO/rGO 0.016 2.63 0.038 0.029

Table 1. An investigation into the electrochemical performance of ZnO/rGO nanocomposites under various electrolytic conditions.

Material Synthesis procedure Electrolyte Current density/scan rate Specific capacitance Ref.

ZnO/rGO Hydrothermal method 1MNaOH 5 mV s–1 293.37 F g–1 [18]

ZnO/rGO Chemical reaction 6MKOH 15 mV s–1 185.48 F g–1 [19]
ZnO/rGO A simple chemical vapour deposition 1.0MNa2SO4 5 mV s–1 275 F g–1 [20]
ZnO/rGO Reduction base process 0.5MH2SO4 5 mV s–1 345 F g–1 [21]
ZnO/rGO Chemical reduction method 1MKCl 10 mV s–1 848 F g–1 This study
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Bull. Mater. Sci. _#####################_
Acknowledgement
We acknowledge the Department of Chemistry, NIT
Manipur, for providing the FTIR, XRD and electrochemical
analysis facilities.
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