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https://doi.org/10.1007/s11581-020-03713-3
ORIGINAL PAPER
Received: 18 June 2020 / Revised: 9 July 2020 / Accepted: 21 July 2020 / Published online: 6 August 2020
# Springer-Verlag GmbH Germany, part of Springer Nature 2020
Abstract
New nanocomposite electrode material of rGO/MnCo2O4 was freely loaded on flexible substrate on nickel foam and prepared by
a simple, cost-effective, and eco-friendly pathway. The results show that the spinel manganese cobaltite (MnCo2O4) with reduced
graphene oxide (rGO) nanocomposite forms a uniform deposit and densely covers on the nickel foam (NF). The electrochemical
measurements were investigated in three methods, such as cyclic voltammetry (CV), galvanostatic charge/discharge (GCD), and
electrochemical impedance spectroscopy (EIS). The synergistic effects from rGO and MnCo2O4 deliver outstanding an excellent
electrochemical performance that was not realized by any of these components alone. The electroactive material exhibits a high
specific capacitance of Csp = 808 F/g at 2 mV/s in 1 M KOH solution. Furthermore, this device delivers an excellent power
density of P = 7658 W/kg and a high energy density of E = 15.2 Wh/kg. More importantly, cycling retention is 135% after 1000
charge/discharge cycles. This study proposes that the as-prepared (rGO/MnCo2O4)/nickel foam has a potential application and a
promising candidate for energy storage devices.
Keywords Reduced graphene oxide . Manganese cobaltite . Nickel foam . Electrochemical performance . Supercapacitor
Besides, the electrochemical impedance spectroscopy (EIS) percentage of oxygen (O) increased 22 times from 3.55 to
measurements were performed by a frequency ranging from 67.75% and the percentage of nickel (Ni) decreased from
100 kHz to 10 mHz. The applied potential of EIS is equal to 96.45 to 8.75% and this to give rise for another elements
10 mV. which are the element of manganese (Mn) as 2.59%, carbon
The value of specific capacitance (Csp) of the electrode can (C) 8.55%, and the element cobalt (Co) 12.03%. This result
be calculated via this equation [46, 47]. well confirms that rGO/MnCo2O4 was formed and in correla-
tion with FTIR-ATR analysis.
C sp ¼ ðI Δt Þ=ðm ΔV Þ ð1Þ
EDX measurements
O 3.55 67.75
Mn – 2.59
C – 8.55
Ni 96.45 8.75
Co – 12.03
This continuous network grown on Ni foam formed a uni- studies and with a good correlation with EDX measurements
form structure, which is suitable for the fast transportation of above.
electrons on different conduction paths on materials and im- Later, we investigate the electrochemical behavior of neat
prove their capacitive performances [48]. Such morphology nickel foam, rGO on nickel foam, and rGO/MnCo2O4 on
images suggest a high specific surface area and a good har- Nickel foam using CV, GCD, and EIS in 1 M KOH aqueous
mony between both materials in which not only stimulated electrolyte.
faradaic reactions, expanding the contact area between
electrode/electrolytes; nevertheless, it provides valuable struc-
ture stability for long-life cycling retention. Following, we Electrochemical performances
investigate the structural behavior of neat nickel foam,
(rGO) on nickel foam, and rGO/MnCo2O4 on nickel foam To evaluate the electrochemical performance of NF, rGO on
using FTIR characterization. NF, and rGO/MnCo2O4 on NF, three electrodes (working:
Nickel foam, counter: Pt wire, and Ag/AgCl as reference)
were applied in 1 M KOH at room temperature. The working
FTIR characterization electrode serves to measure the current through the entire cell
and the reference is useful to measure the potential of the
The evolution of functional groups in rGO/MnCo2O4 precur- working electrode, which is nickel foam in our case.
sor on nickel foam with calcination temperature is followed by However, the counter electrode allows the free passage of
FTIR to verify the presence of new groups. Figure 6 shows the the current and has not any influence for the electrochemical
appearance of peaks at 2924 cm−1 and 2851 cm−1 which be- measurement but ensures circuit closure without any interven-
longs to C–H. The peak at 1644 cm−1 is attributed to the tion [53].
stretching vibration of the carboxylate group with Co (II). To identify the best electrode between neat nickel foam,
1515 cm−1 peak is due to the coordination of Co2+ (or rGO on nickel foam, and rGO/MnCo2O4 on nickel foam for
Mn 2+ ) ions with carboxyl groups [49]. The peak at supercapacitor electrode elaboration, cyclic voltammetry of
1287 cm−1 reflects the stretching vibration of C–H group. each sample was recorded in the range of 0 to 0.8 V.
The peaks at 972 and 922, 923 cm−1 are attributed to C–C Figure 7a and b display the CV curves of samples cited above
deformation vibration [50]. Moreover, it well shows the ap- at two scan rates of (a)1000 mV/s and (b) 2 mV/s. The CV
pearance of two new peaks at around 641 and 544 cm−1 in curve of neat Nickel foam at a scan rate of 2 and 1000 mV/s
which are attributed to Co–O and Mn–O vibration modes and illustrated in Fig. 7a and b . Oxido-redox peaks are well de-
this demonstrates the formation of the spinel MnCo2O4 phase fined and the specific capacitance was measured and show a
[51, 52]. These results are in good agreement with previous negligible current response and then a lower value of specific
capacitance, power and energy densities compared with the 500, 750, and 1000 mV/s. We notice that the quasi-rectangle
other samples. shape is maintained at different scan rates ranging from the
The current response adequately increased with the incor- highest to the lowest one. Offering fast charge storage and an
poration of rGO and become more important with the addition easily accessible rGO/MnCo2O4 electrode to the as-prepared
of manganese cobaltite. For example, a maximum capacitance electrolyte was sustained by the spinel manganese cobaltite
of rGO was found at about Csp = 108 F/g at a low scan rate of inter-located and grown on the crisscrossed reduced graphene
2 mV/s and which was distorted in terms of shape to be 75 F/g oxide nanosheet loaded on 3D nickel foam framework. From
at 1000 mV/s at high scan rates. Power and energy densities these curves and via the equation cited above, the rGO/
were also calculated and according to the equation above and MnCo2O4 electrode exhibited the highest specific capacitance
we found P = 3138 W/kg and E = 7.08 Wh/kg, respectively. value compared with other electrodes. At 2 mV/s, we mea-
This can be explained that in a low scan rate, the ionic fluxes sured the specific capacitance of Csp = 808 F/g and an energy
were in equilibrium for this reason it gives a symmetrical plot density of E = 15.2 Wh/kg. However, the highest power den-
[54]. Nonetheless, at high scan rate, there is a modification in sity was recorded at 1000 mV/s and was found at around P =
CV curves because of the fast ion transport in solution and 7658 W/kg. The incorporation of MnCo2O4 plays a critical
also the absence of direct contact of the cell surface (active role to give rise to a large specific surface area and then an
electrode) and the electrolyte [55, 56]. increasing current response due to the creation of more
The largest surface area of rGO/MnCo2O4 electrode from electroactive cites which promotes the faradaic redox process-
CV plot is observed in Fig. 8. Thus, we plot the electrochem- es and then to better electrochemical performances. Our elec-
ical behavior at different scan rates: 2, 5, 10, 25, 50, 100, 250, trochemical results are in a good position compared with
previous studies done recently (Table 2) using nickel foam loses 32% of its initial capacitance, and retained only 68%
such as substrate-adopting electrode materials based on after 1000 cycles because of the structural damage during
graphene and manganese. charge/discharge process. The phenomenon of the increase
of the capacitance retention can be considered such as an
Galvanostatic charge/discharge activation process of the rGO/MnCo2O4 of this active elec-
trode and this can be explained with the improved wettability
Galvanostatic charge/discharge (GCD) behaviors were ap- and the activation process. The rGO/MnCo2O4 presents more
plied in 1 M KOH within a three-electrode system at different active sites as a faradaic reaction and good contact between
constant currents of 0.2, 0.5, 1, 2, 5 and 10 mA. Figure 9 electrode/electrolyte suggesting excellent cycling stability and
shows a quasi-symmetric charge/discharge curves indicating the presence of Mn can improve the lifetime of the as-prepared
a small internal resistance (IR) [70–72]. rGO/MnCo2O4 trans- active electrode. This favorable result was reported in other
lates a longer discharge time, indicating a good electrochem- previous studies [76, 77]. These outstanding results were due
ical behavior, which is in coincidence with cyclic voltamme- to the combined synergistic advantages of rGO and MnCo2O4
try measurements. Indeed, in terms of energy storage process materials.
as long as the internal resistance (iR) is low as long as the
heating is low during the charge and the discharge of the
Electrochemical impedance spectroscopy (EIS)
device and next less energy waste [7, 73–75].
All data extracted from complex impedance spectroscopy can
Cycling retention be modeled via those four complex formalisms [78, 79]; each
one is composed of two components: real and imaginary parts
The lifetime and long-term cycling retention are a vital and called:
fundamental factor to evaluate the intrinsic characteristic of
the electrode-based material and this was confirmed via cyclic Complex modulus : M ðwÞ ¼ M 0 þ JM″ ð4Þ
voltammetry. As depicted in Fig. 10, the specific capacitance Complex permittivity : ɛ ðwÞ ¼ ɛ 0 −jɛ″ ð5Þ
of rGO/MnCo2O4 increased as number cycle and further to
remain at 135% after 1000 cycles while rGO on nickel foam
Fig. 8 CV curves of rGO/MnCo2O4 on NF (from 2 to 1000 mV/s) Fig. 9 GCD of rGO/MnCo2O4 on nickel foam at different constant
currents ranging from 0.2 to 10 mA
Table 2 Comparison of the electrochemical performance for rGO-based hybrids on Nickel foam substrate
Electrode (on nickel foam) Methods C/g−1 E/Wh/kg P/Wkg−1 Cycling retention/% Ref
Cole-cole representation (Nyquist plot) In summary, rGO/MnCo2O4 and its porous network on 3D
nickel foam flexible substrate have been successfully synthe-
Impedance spectroscopy is a tool that focuses on measuring sized with a simple, cost-effective, and eco-friendly strategy.
the impedance Z (w) versus the impedance signal frequency The as-prepared active electrode provides a good electro-
between the frequency ranges to understand more the funda- chemical performance of Csp = 808 F/g and energy density
mental behavior at the electrode/electrolyte interface. The data E = 15.2 Wh/kg, P = 7658 W/kg, and cycling retention of
obtained could be visualized as a Nyquist plot also known as 135% after 1000 charge/discharge and this due to the good
the cole-cole plot expressed by the imaginary part Z″ versus electrical conductivity and the synergic effect between mate-
the actual real part Z′. The electrochemical impedance spec- rials. The results demonstrate that rGO/MnCo2O4 nanocom-
troscopy (EIS) was carried out at room temperature ranging posite displays good electrochemical performance than neat
from 100 kHz to 10 mHz. rGO and which shows that this electrode could be considered
The Nyquist plots can be fitted using an equivalent circuit as a promotional candidate for a favorable supercapacitor elec-
model (inset of Fig 11) consisting of those parameters: Rs trode material for next-generation energy storage devices.
Funding information The authors received financial support from the 16. Yun SI, Kim SH, Kim DW, Kim YA, Kim BH (2019) Facile prep-
Ministry of Higher Education and Scientific Research of Tunisia. aration and capacitive properties of low-cost carbon nanofibers with
Achref Chebil has studied in Ates polymer research group between 23 ZnO derived from lignin and pitch as supercapacitor electrodes.
May 2019 and 7 August 2019 in Tekirdag Namik Kemal University, Carbon 149:637–645
Turkey. 17. Fu H, Zhang XD, Fu JZ, Shen GZ, Ding YL, Chen ZJ, Du H (2020)
Single-layers of MoS2/graphene nanosheets embedded in activated
carbon nanofibers for high-performance supercapacitor. J Alloys
Compd 829:154557
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