Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965

https://doi.org/10.1007/s10854-020-03204-1

Electrochemical analysis of conducting reduced graphene oxide/

polyaniline/polyvinyl alcohol nanofibers as supercapacitor electrodes
Zhuoming Chen1   · Yu Jiang1 · Binjie Xin1 · Shouxiang Jiang2 · Yan Liu1 · Lantian Lin1

Received: 2 December 2019 / Accepted: 3 March 2020 / Published online: 10 March 2020
© Springer Science+Business Media, LLC, part of Springer Nature 2020

Abstract
Supercapacitor is a promising electrochemical energy-storage device, which has the advantage of good cycle stability, short
charging time, and high power density, so it has broad application prospects. Electrode as a core component has an important
influence on the specific capacitance and performance of the supercapacitor. In this study, a series of reduced graphene oxide/
polyaniline/polyvinyl alcohol (RGO/PANI/PVA) nanofibers with different RGO concentrations were synthesized by electro-
spinning method and then studied as electrode materials for supercapacitors. The experimental result reveals that the PANI/
PVA nanofiber shows the pseudocapacitance properties, while the RGO/PANI/PVA nanofibers exhibit the electrochemical
properties of the double-layer capacitor. In addition, the RGO/PANI/PVA nanofibers have a uniform diameter distribution
of 119.8 nm without beads and droplets sticking when the concentration of RGO is 0.2%. This morphology contributes to
a large specific surface area of fibers and provides sufficient channels for the transport of ions. RGO/PANI/PVA nanofibers
exhibit better specific capacitance of 174 F/g when compared with the PANI/PVA (105 F/g). The research indicates that
RGO/PANI/PVA nanofibers with high specific capacitance can provide a promising application as supercapacitor electrodes.

1 Introduction has good redox reversibility and high energy-storage charac-

Supercapacitor is a kind of promising electrochemical
energy-storage device, which exhibits good cycle stability,
fast charge/discharge rate, long cycle life, and high power
density [1]. It has broad application prospects in wind power
generation, transportation facilities, wireless communica-
tion, electronic equipment, and other fields [2, 3]. As a core
component of supercapacitors, electrodes have an important
influence on the specific capacitance and performance of
supercapacitors.
Common supercapacitor electrodes are usually prepared
by transition metal oxides, conductive polymers [3–5], and
carbon-based materials. Polyaniline (PANI) as one of the
conducting polymers has a great potential in the application
of supercapacitors [2]. PANI is easy to be synthesized, and it
* Zhuoming Chen
chenzhuoming178041@163.com
* Binjie Xin
xinbj@sues.edu.cn
1
School of Textiles and Fashion, Shanghai University
of Engineering Science, Shanghai 201620, China
2
Institute of Textiles and Clothing, The Hong Kong
Polytechnic University, Hong Kong 999077, China
teristics. In addition, some recent studies confirmed that add-
ing carbon materials into polymer solutions can effectively
enhance the overall properties of the resultant composite
[6]. Therefore, combining PANI with carbon materials can
make up for the deficiency of a single material and improve
the performance of the composite [7]. Gui et al. [8] prepared
PANI/graphene oxide nanocomposites with three different
mass ratios (aniline to graphene oxide) of 1000:1, 100:1, and
10:1. The results show that the specific capacitance of the
composite is 355.2 F/g when the ratio is 1000:1. Jiang et al.
[9] prepared polyaniline/reduced graphene oxide (PANI/
RGO) membrane by in situ polymerization. The results show
that the conductivity of PANI/RGO composite membrane
is higher than PANI membrane. Shayeh et al. [10] discov-
ered the addition of RGO and gold can improve the specific
capacitance of PANI. The specific capacitance of PANI and
PANI/RGO/gold is 190 F/g and 303 F/g, respectively.
It is reported that the electrodes with high specific sur-
face area and appropriate porosity can significantly improve
the properties of supercapacitor. Electrospinning is a low-
cost and high-efficiency method to prepare nanofibers. The
fiber diameter can be adjusted from nanometer to micron
by applying different voltages to the polymer solution from
a micro-syringe pump [11–14]. Electrospun nanofibers are

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Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965 5959
the most promising candidates for engineering tissue scaf-
folds, filtration, sensors, release control, wound healing, and
energy-storage applications [15–17]. Rose et al. [18] pre-
pared GO/PANI/PVA nanofibers by using electrospinning.
The results show the GO/PANI/PVA nanofibers as super-
capacitor electrodes have higher specific capacitance than
PANI nanofibers. Sudeshna et al. [19] found the capacitance
retention of PANI-NFs web prepared by electrospinning is
higher than PANI; the result indicated the feasibility of elec-
trospun PANI-NFs web can be used as superior electrode
materials for supercapacitors.
In this study, a series of RGO/PANI/PVA composite
nanofibers with different RGO concentrations were pre-
pared by electrospinning method and then studied as elec-
trode materials for supercapacitors. The surface morphology,
chemical structure, and electrochemical properties of the
PANI/PVA and RGO/PANI/PVA nanofibers with different
RGO concentrations were studied. The results reveal that the
RGO/PANI/PVA composite nanofiber is a promising candi-
date for electrode material in supercapacitors.
2 Experimental
2.1 Materials
Hydrazine hydrate ­(N2H4·H2O, concentration: 80 wt%) and
polyvinyl alcohol (PVA, MW~1799 g/mol) were purchased
from Aladdin Reagent Co., Ltd. (China). Aniline (An,
≥ 99 wt%), dodecylbenzne sulfonic acid (DBSA, 90 wt%),
ammonium persulfate ((NH4)2S2O8, APS, 98 wt%), hydro-
chloric acid (HCl, mass fraction: 36 wt%), and polytetra-
fluoroethylene (PTFE, 40 wt%) were purchased from Sin-
opharm Chemical Reagent Co., Ltd. Graphite oxide (GO,
SE2430W, mass fraction: 42.78 wt%) was provided by The
Sixth Element (Changzhou) Materials Technology Co.,
Ltd. Transparent indium tin oxide (ITO) glass (resistance
6–8 Ω/sq, 2.0 cm × 2.0 cm in size) used as a substrate were
obtained from Foshan Meijingyuan Glass Technology Co.,
Ltd, (China). Deionized water was used throughout the
experiment. All chemicals are analytical reagents and used
as received unless otherwise specified.
2.2 Reduction of graphene oxide
100 mg GO was dispersed in 100 ml deionized water by
using ultrasonic wave until a uniform solution was obtained.
After the dispersion, 1 ml N­ 2H4·H2O was added to convert
the GO into RGO with ultrasonic treatment at 90 °C for 1 h.
During the reduction, the color of the solution changed from
yellow brown to black. RGO sheets can be obtained after
washing with deionized water for 5 times and subsequently
drying in an oven at 60 °C for 12 h.
2.3 Preparation of PANI/PVA and RGO/PANI/PVA
emulsions
Even though PANI is a conducting polymer, it’s difficult for
it to form a fiber mat by using electrospinning. Polyvinyl
alcohol (PVA) is a good film former, therefore combining
the PANI with PVA can effectively solve this problem, and
PANI can homogeneously disperse in PVA due to the for-
mation of hydrogen bond between them [20]. In this study,
PVA particles with a concentration of 4.3% were dispersed
in 30 ml deionized water and kept ultrasonic stirring at 90 °C
until a completely dissolved PVA aqueous solution was
obtained. Then, the solution was cooled to room tempera-
ture to obtain solution A. Solution B was prepared by adding
RGO with different concentrations (0.2%, 0.4%, 0.6%, 0.8%,
and 1.0%) into solution A and sheared at high speed for
30 min. Solution A and solution B were, respectively, mixed
with 2.38 g DBSA at 0 °C in an ice-water bath and stirred at
1500 rmp for 20 min. After that, aniline solution was added
into the mixed solutions. The solutions changed into milky
white floc as the stirring speed increased to 2000 rmp and
then kept stirring for 4 h. APS solution was prepared by dis-
solving the APS into 10 ml deionized water. Then, the APS
solution was added into the white emulsions at a rate of 6
drops/5 min. This blend was then further poured into PVA
aqueous solution and stirred for 6 h to prepare the spinning
solution with dark green color.
2.4 Preparation of PANI/PVA and RGO/PANI/PVA
nanofibers
The preparation of RGO/PANI/PVA emulsions and the rele-
vant nanofibers is shown in Fig. 1. The PANI/PVA nanofiber
was also prepared without the addition of RGO. As depicted
in the figure, the nanofibers were fabricated by electrospin-
ning method. 5 ml of the viscous solution was loaded into
a syringe and fed at a rate of 6 ml/min with an applied volt-
age of 23 kV. Distance from the spinneret to collector was
16 cm. The electrospinning was carried out with a constant
temperature at 27 °C and constant humidity of 60%.
2.5 Characterization
Scanning electron microscopy (SEM) tests were performed
on a scanning electron microscope (SEM; JEOL JSM-840,
Japan). Fourier transform infrared spectra (FTIR) were
obtained with a Fourier Transform Infrared Spectroscopy
(FTIR; Spectrum Two, USA). X-ray diffraction (XRD)
measurements were conducted using D2 PHASER X-ray dif-
fractometer (Bruker AXS, Germany). Electrochemical meas-
urements were recorded using a CHI660E electrochemical
13

5960
Fig. 1  Schematic of preparation process of RGO/PANI/ PVA nanofibers
work station (CHI, Shanghai, China) with three-electrode
cell. The nanofibers, a calomel electrode, and a platinum
wire were used as the work electrode, reference electrode,
and counter electrode, respectively, in 1.0 mol/l HCl electro-
lyte. The weight of RGO/PANI/PVA nanofiber used in cyclic
voltammetry (CV) measurements was 0.0015 mg. The sub-
strate is ITO glass, and the binder is polytetrafluoroethylene
solution (PTFE). The potential window of CV measurements
is between − 0.6 and + 1.0 V at scanning rate of 5, 10, 20, 50
,and 100 mV/s. The frequency range used for electrochemi-
cal impedance spectroscopy is from 10 MHz to 100 kHz.
3 Results and discussion
3.1 Surface morphology
SEM images of PANI/PVA and RGO/PANI/PVA nanofibers
with different RGO concentrations are shown in Fig. 2. It is
clear from Fig. 2a, PANI/PVA nanofibers exhibit smooth
surface and have a uniform diameter distribution of about
117 nm. For the RGO/PANI/PVA nanofibers as shown in
Fig. 2b–f, it can be observed that the fiber diameter is grad-
ually increased as the RGO concentration increased from
0.2 to 1.0%, and some beads with an increasing diameter
are also found in the nanofibers. Fahimeh et al. [21] also
reported the similar result that the diameter of the nanofiber
13
Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965
increased with the raising concentration of RGO. The forma-
tion of the beads is probably due to the capillary instability
of the liquid jet caused by surface tension on the spinning
solution [22]. As the concentration of RGO increases, the
viscosity of the spinning solution increases. At the same
voltage, the electric field force is not sufficient to provide
the surface tension to form the fiber. In addition, large slabs
of solution are thrown down on the fiber mat when the RGO
concentration is high at 0.8–1.0%. From the above results,
it can be concluded that 0.2%-RGO/PANI/PVA nanofibers
have the good fiber morphology and the fiber diameter is
about 119.8 nm.
The diameter variations of the nanofibers (shown in
Fig. 3) can be obtained based on the results in Fig. 2. The
average diameter of all the RGO/PANI/PVA nanofibers is
larger than that of PANI/PVA nanofibers. Obviously, the
average diameter of RGO/PANI/PVA nanofibers increased
with the increasing concentration of RGO.
3.2 Crystallization behavior
XRD patterns of PANI/PVA and RGO/PANI/PVA nanofib-
ers with different RGO concentrations are shown in Fig. 4. It
is obvious that the XRD patterns show three peaks at 19.6°,
29.3° and 41°, which correspond to (010), (110), and (100)
crystal faces, respectively. In the XRD patterns, the sharp
peak at 19.6° can be attributed to the diffraction of PVA and
Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965 5961
Fig. 2  SEM images of a PANI/PVA and RGO/PANI/PVA nanofibers with different RGO concentrations: b 0.2%, c 0.4%, d 0.6%, e 0.8%, and f
1.0%
PANI. This overlapped peak indicates the good compatibil-
ity between PVA and PANI. Obviously, the peak at 19.6°
became sharp after the addition of RGO and it is becoming
increasingly sharp as the raising concentration of RGO. The
result revealed that RGO can act as nucleation sites for the
growth of PANI resulting in a contribution to the improve-
ment of the crystallinity of the composite nanofibers.
3.3 Chemical structure
Figure 5 shows FTIR spectra of PANI/PVA and RGO/PANI/
PVA nanofibers with different RGO concentrations. As
shown in the figure, the spectra shape and peak positions of
RGO/PANI/PVA nanofibers are similar with that of PANI/
PVA. The result indicates that the addition of RGO would
not influence the functional groups of PANI/PVA. The peak
positions corresponding to the functional groups of PANI
and PVA are illustrated in Table 1. Based on the recorded
functional groups, the absorption peak at 1418 cm−1 and
the stretching peak at 1644 cm−1 are the main characteristic
peaks of PANI, which are corresponding to its conductivity
properties.
3.4 Cyclic voltammetric behavior
To confirm the influence of RGO on the ion transport of
PANI, CV studies were carried out. Figure 6 presents the
CV curves of PANI/PVA and RGO/PANI/PVA nanofibers
from − 0.6 to + 1.0 V, and performed in 1 mol/l HCl solution
at a scanning rate of 50 mV/s. The CV curves exhibit all the
nanofibers have the redox peaks at − 0.6 and + 1.0 V, which
can be attributed to proton insertion into and extraction out
from the host lattice, respectively [23]. As demonstrated in
the figure, an obvious anodic peak as marked in the CV
curve of PANI/PVA nanofiber indicates its pseudocapaci-
tance properties, which are relative to the basic electrochem-
ical performance of PANI. This is because reversible Fara-
day reaction occurred on the electrode surface resulting in
charge transfer and then to form the capacitance. However,
the marked peak was inhibited after the addition of RGO
and the RGO/PANI/PVA nanofibers exhibit the predominant
electrochemical properties of the double-layer capacitor. In
this process, the formation of capacitance can be attributed
to the charge accumulation at the electrode–electrolyte
interface.
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5962 Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965

40 40
(a) Dmean=117.4±3.33nm (b) Dmean=119.8±2.88nm
35 35

30 30

25 25
Frequency

Frequency
20 20

15 15

10 10

5 5

0 0
50 90 130 170 210 250 290 330 370 60 90 120 150 180 210 240 270 300
Diameter(nm) Diameter(nm)

35 35
(c) Dmean=120.9±3.44nm (d) Dmean=125.7±3.07nm
30 30

25 25
Frequency

Frequency

20 20

15 15

10 10

5 5

0 0
60 90 120 150 180 210 240 270 300
30 60 90 120 150 180 210 240 270
Diameter(nm) Diameter(nm)

35 30
(e) Dmean=147.5±5.75nm (f) Dmean=162.8±4.2nm
30 25

25
20
Frequency

Frequency

20
15
15
10
10

5
5

0 0
0 60 120 180 240 300 360 420 480 50 100 150 200 250 300 350 400 450

Diameter(nm) Diameter(nm)

Fig. 3  Diameter distribution of a PANI/PVA and RGO/PANI/PVA nanofibers with different RGO concentrations: b 0.2%, c 0.4%, d 0.6%, e
0.8%, and f 1.0%

13
Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965 5963

0.0%
CV curves of the 0.2%-RGO/PANI/PVA nanofibers at

(110)
0.2% different scanning rates were presented in Fig. 7 to fur-

(010)

(100)
0.4% ther analyze the capability of the nanofibers to be used as
0.6%
0.8% electrode materials for supercapacitor. The area enclosed
1.0% in the CV curves increases with the increasing scanning
rate from 5 to 100 mV/s. The peak current responses pro-
Intensity(a.u)

portionally with the increasing scanning rate indicating a

rapid charge propagation of the nanofibers [24]. In addi-
tion, there is no significant shift in the positions of the
anodic and cathodic peaks with the increasing scanning
rate. This is because of the fast electron transport between
the nanofibers and electrolyte, and the result implies a
good rate capability and stability of the nanofibers.

10 20 30 40 50
2θ(degree) 3.5 Specific capacitance

Fig. 4  XRD patterns of PANI/PVA and RGO/PANI/PVA nanofibers The developed RGO/PANI/PVA nanofibers can be the
with different RGO concentrations promising materials for the preparation of electrode, and
the specific capacitance is one of the important properties
of electrode for supercapacitor application. In this study,
105
the specific capacitance of the PANI/PVA and RGO/PANI/
2912
3306

1418
1324

100 PVA nanofibers was investigated and calculated from the

841

CV results by using Eq. (1).

95
[( )/ ]

∫
Transmittance(a.u.)

90 Csp = IdV (SΔVm) (1)

85
1644

In the equation, I is the current (mA), S is the scan rate

80
0.0 % (mV/s), ‘ΔV’ is the potential (V), and ‘m’ is the mass of
75 0.2 % the electrode material (mg). Figure 8 shows the calculated
0.4 % results of the nanofibers with different concentrations of
70 0.6 %
RGO. As shown in the figure, the capacitance of PANI/
0.8 %
65 PVA increases after the addition of RGO because of the
1090

1.0 %
60
high electrical conductivity of RGO. Obviously, the high-
4000 3500 3000 2500 2000 1500 1000 500 est capacitance occurs when the RGO concentration is
Wavenumber(cm-1) 0.2%. This is because the diameter distribution of 0.2%-
RGO/PANI/PVA nanofibers is relatively uniform and the
Fig. 5  FTIR spectra of PANI/PVA and RGO/PANI/PVA nanofibers surface of the nanofibers is in good shape which have no
with different RGO concentrations

Table 1  The peak positions Polymer Peak posi- Corresponding functional group

and functional groups of the tion ­(cm−1)
nanofibers
PANI 841 The bending vibration absorption near the C–H plane of 1, 4-substituted benzene
1090 In-plane ring deformation C–H bending of the quinoid ring, and C–H bending of
quinoid ring
1324 The absorption of benzene rings
1418 The absorption of quinoid ring
1644 C=N stretching of quinoid ring
2912 The aromatic C–H group
3306 Stretching vibration of N–H bond
PVA 2912 O–H group, and stretching vibration of the aliphatic C–H group

13

5964 Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965

2
×10-5
200

174 171
1
162
160 154
145

Specific capacitance(F/g)
0

-1
120
105
Current/A

-2

-3 0.0% 80
0.2%
-4
0.4%
0.6% 40
-5
0.8%
-6 1.0%
0
-0.8 -0.6 -0.4 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 0.0 0.2 0.4 0.6 0.8 1.0
Potential/V RGO concentration(%)

Fig. 6  CV curves of PANI/PVA and RGO/PANI/PVA nanofibers Fig. 8  Specific capacitance of PANI/PVA and RGO/PANI/PVA
with different RGO concentrations (the scanning rate is 50 mV/s) nanofibers with different RGO concentrations (the scanning rate is
50 mV/s)

×10-5
1

0.0 %
0 12
×10
4 0.2 %
0.4 %
-1 10 0.6 %
0.8 %
Current/A

-2
8 1.0 %
Z''(ohm)

-3 ×10
4
1.0
6
-4 5mV/s
10mV/s
4 Z''(ohm)

-5 20mV/s 0.5

50mV/s
100mV/s 2
-6
0.0 4
0.0 0.5 1.0 1.5×10
Z'(ohm)
-0.6 -0.4 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 0 4
×10
Potential/V 0 2 4 6 8 10 12 14 16 18 20
Z'(ohm)
Fig. 7  CV curves of 0.2%-RGO/PANI/PVA nanofibers at different
scanning rates Fig. 9  Electrochemical impedance spectroscopy of PANI/PVA and
RGO/PANI/PVA nanofibers with different RGO concentrations

beads and droplets and then leads to a relatively uniform

network structure as identified by the SEM results.
3.6 Electrochemical impedance behavior
Electrochemical impedance spectroscopy (EIS) is usually
used to investigate the internal resistance of the spinning
fibrous electrodes. As observed in Fig. 9, the curve slope
of 0.2%-RGO/PANI/PVA nanofiber is highest in the low-
frequency region, indicating a rapid diffusion of ions, a
low resistance, and an ideal capacitive behavior. That is
because the 0.2%-RGO/PANI/PVA nanofiber has a small
diameter as discussed in Figs.  2 and 3, which leads to
a large specific surface area, and then the charge trans-
fer channel is unobstructed and the nanofiber electrode
capacitor shows a better capacitance performance. As the
concentration of RGO increased, the slope of the curve
gradually decreased, indicating that a gradual deterioration
in impedance performance of the nanofibers. A semicircle
was observed at the curve of PANI/PVA nanofiber fol-
lowed by a straight sloped line, and the result reveals that
the interfacial charge transfer resistance of the nanofiber
is high and the capacitive performance is poor because of
the low electrical conductivity of PANI/PVA nanofiber.

13
Journal of Materials Science: Materials in Electronics (2020) 31:5958–5965 5965
4 Conclusion
In summary, a series of RGO/PANI/PVA nanofibers with
different RGO concentrations were prepared by using elec-
trospinning method. SEM images show that the diameter
of the PANI/PVA nanofiber increases after the addition of
RGO, and the average diameter of RGO/PANI/PVA nanofib-
ers increased with the increasing concentration of RGO.
The PANI/PVA nanofiber shows the pseudocapacitance
properties, while the RGO/PANI/PVA nanofibers exhibit
the electrochemical properties of the double-layer capaci-
tor. The specific capacitance of RGO/PANI/PVA nanofibers
reaches a maximum of 174 F/g, which is higher compared
to the capacitance of PANI/PVA nanofibers (105 F/g). The
addition of RGO has a positive influence on the specific
capacitance of PANI/PVA nanofiber, and the EIS of the
0.2%-RGO/PANI/PVA nanofibers shows a low resistance
and an ideal capacitive behavior. Therefore, the electrospun
RGO/PANI/PVA nanofiber can be the promising candidate
materials for supercapacitor application and it can be used as
the counter electrode to improve the electrocatalytic activity
of supercapacitors.
Acknowledgements  The authors gratefully acknowledge the finan-
cial support by Research Initiation Funds of Shanghai University of
Engineering Science (2016-27), Student Research Innovation Train-
ing Program-SUES (cs1809004), Young Scholar Training Scheme of
Shanghai Universities (ZZGCD16028), 2017 Talents Action Program
of Shanghai University of Engineering Science (2017RC432017), and
Shanghai Local Capacity-Building Project (No. 19030501200).
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