Journal of Energy Storage 30 (2020) 101446

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Journal of Energy Storage

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MoS2 Confined MXene Heterostructures as Electrode Material for Energy T

Storage Application
Mijun Chandrana, Anitta Thomasa, Asha Raveendrana, Mari Vinobab,
Margandan Bhagiyalakshmia,⁎
a
Department of Chemistry, Central University of Kerala, Kerala, India
b
Kuwait Institute for Scientific Research, Kuwait

ARTICLE INFO ABSTRACT

Keywords: Two-dimensional (2D) titanium carbide Ti3C2 (MXene) is exemplified as the promising electrode material for
MXenes supercapacitors. MXene was derived by etching of Al-layer from MAX phase (Ti3AlC2), and MoS2 was confined
Metal chalcogenides on MXenes through incipient wet impregnation of MoS2 precursor. The prepared MXene and MoS2/MXene
Cyclic voltammogram materials were characterized by X-ray diffraction, scanning electron microscope and energy-dispersive X-ray
Supercapacitors
spectroscopy, BET analysis, and X-ray photoelectron spectroscopy. The electrochemical characteristics of MXene
MoS2/MXene
and MoS2/MXene heterostructures were evaluated by different techniques such as cyclic voltammogram, gal-
vanostatic charge-discharge, and electrochemical impedance spectroscopy. The electrochemical measurements
revealed that the maximum specific capacitance of the MoS2/Mxene electrodes reaches up to 342 F g−1 at a
discharge current density of 0.4 A g−1 in an enlarged voltage window of -1.5 V to 1.5 V. Also, Electrochemical
impedance studies show that the incorporation of MoS2 decreases the charge transfer resistance of MoS2/MXene.
Overall, the electrochemical performance of MoS2/MXene exhibited excellent reversibility, cycle stability, and
rate performance. The obtained results uncover MoS2/MXene as promising electrode materials for super-
capacitors.

1. Introduction [10]. The current research expansion in the area of advanced materials
invented 2D transition metal carbides, also called MXenes that possess
The current scenario of deriving energy from clean and renewable excellent metallic conductivity and highly defined morphologies that
energy sources has made energy storage systems as an essential com- makes it as suitable electrode material for supercapacitors [11].
ponent in the electronic, electrical, defence, and locomotives devices MXenes are 2D transition metal carbides, or nitrides (Mn+1Xn Tx)
[1, 2]. In this respect, supercapacitors are viewed as the most promising derived from ternary transition metal carbides or nitrides materials so-
energy storage system, as they perfectly fill the gap between dielectric called MAX phase, (Mn+1AXn), where M represents an early transition
capacitors and conventional batteries and can be used in high power metal (Sc, Ti, Zr, Hf, V, Nb, Ta, Cr, Mo, and so on), A stands for mostly
operators [3, 4]. However, there are challenges related to their lower IIIA group elements, n = 1–3, X is carbon and/or nitrogen, and Tx
energy density compared to batteries [5-7]. By concept, the super- stands for the surface terminations (OH, O or F)[11]. MXenes exhibits
capacitors are store and release energy through reversible adsorption of superior electrical conductivity due to its metallic nature with transi-
electrolyte ions onto the surface of electrode materials, either electro- tion metal (Ti) atomic layers alternately implanting between carbon
chemical double-layer capacitors (EDLCs) or pseudocapacitors through atomic layers [12-15]. Also, due to the existence of surface termina-
reversible faradic redox reactions and sometimes by both mechanism tions, the delaminated MXene are hydrophilic and electronegative with
that is mostly controlled by active electrode materials.[8] Even though a high negative zeta potential in the range of -39.5 to -63 mV and can be
conventional carbon-based materials like carbon nanotube (CNT), me- dispersed in most of the organic solvents [16, 17]. Other important
soporous carbon (CMK), graphene, which contain high surface area and characteristics of MXenes are their open channels that can be sponta-
conductivity, are reported as electrode material for supercapacitors [9]. neously intercalated by polar organic molecules and metal ions, which
However, the researchers are still involved in designing electrode ma- makes it as electroactive supercapacitor material [18-20].
terials for improving energy storage capacity with high energy density Currently, MoS2 few-layered metal dichalcogenide resembles

⁎
Corresponding author.
E-mail address: [email protected] (M. Bhagiyalakshmi).

https://doi.org/10.1016/j.est.2020.101446
Received 31 January 2020; Received in revised form 20 March 2020; Accepted 8 April 2020
2352-152X/ © 2020 Elsevier Ltd. All rights reserved.
M. Chandran, et al. Journal of Energy Storage 30 (2020) 101446

graphite-like material and has been reported as active electrode mate- vacuum for 4 h in the degassing port of the adsorption analyzer. The
rial in EDLCs due to its high intrinsic, fast ionic conductivity, faradaic specific surface area (SBET) was determined from the linear plot of the
capacitance and overall charge storage capacity [21, 22]. Un- BET equation, and the pore volume was calculated using (BJH) method.
ambiguously, the benefits of MoS2 has been selected to prepare MoS2 The surface morphology was acquired from scanning electron micro-
intercalated MXenes heterostructures by in-situ controlled thermal scopy (SEM) by ZEISS Gemini SEM 300. The metal distribution ob-
process for enhancing the electrochemical performance in terms of tained from energy-dispersive X-ray spectroscopy (EDX) by Gemini
energy storage. Even though MoS2/MXene was reported as anode ma- 300/EDS Octane Plus model. The electrochemical performance of
terials for batteries [23], no report on the in-situ MoS2 confinement into MXene and MoS2/MXene was carried out on Bio-Logic electrochemical
the layers of MXene is available that solely produced layered MoS2. workstation with symmetric two-electrode system (SP 240).
Upon combining the advantages of MoS2 and MXene, MoS2/MXene
electrode displays a redox profile in an enlarged voltage window up to 2.5. Electrochemical measurement
∼3.0V with aqueous electrolytes. Generally, such an extended oper-
ating voltage window are achieved with organic electrolytes [24, 25], The working electrodes were fabricated by mixing MXene and/or
while aqueous electrolyte exhibit limited cell voltage [26, 27]. How- MoS2/MXene- composite with acetylene black, and poly (tetra fluoro
ever, improvement in operating voltage window could also be influence ethylene) in a weight ratio of 8:1:1 and N-methyl-2- pyrrolidone (NMP)
by electrode materials, here combining MoS2 and MXene improves the was added then ultrasonicated to form a slurry. Freshly prepared slurry
total capacitance as well as the cell voltage that could fit this MoS2/ was coated on Grafoil paper across a 1 cm x 1 cm area, dried, and used
MXene as a promising electrode material to develop advanced super- as a working electrode. The active electrode material was used at about
capacitors with high energy density. 1.5 mg. The electrochemical measurements, such as cyclic voltammetry
(CV), galvanostatic charge-discharge (GCD), and electrochemical im-
2. Experimental methods pedance spectroscopy (EIS) were recorded on an electrochemical
workstation (Biologic SP-240) with symmetric two-electrode system
2.1. Materials used 1M H2SO4 as an electrolyte.

Ti3AlC2 (MAX Phase) (98 wt%) was procured from Hangzhou 3. Results and Discussion
Dayangchem Co. Ltd. P. R. China. Carbon black, Nafion, polytetra-
fluoroethylene (PTFE), N-methyl-2-pyrrolidinone (NMP), ammonium 3.1. Characterization of MAX phase, MXene, and MoS2 /MXene
heptamolybdate (NH4)6Mo7O24.4H2O) was purchased from Sigma-
Aldrich and used without purification. Dimethyl sulfoxide (DMSO), Figure 1 shows the XRD patterns of the MAX phase, MXene, MoS2,
40% hydrofluoric acid, ammonium hydroxide were purchased from SRL and MoS2/MXene. The well-defined diffraction peaks of MAX phase at
chemicals. 2θ= 9.2, 19.2, 34.0, 36.7, 39.0, 41.8, 48.5, 52.4, 56.6, 60.2,65.6, 70.5,
and 74.1° that corresponds to (002), (004), (100), (103), (104), (105),
2.2. Synthesis of MXene from MAX phase (107), (108), (109), (110), (1011), (118) and (1013) planes, respec-
tively were observed. The peak of (002) and (004) planes, at 2θ ∼ 9.2°
About 5 g of MAX phase Ti3AlC2 was mixed with 50 ml of 40 % HF and 19.2° of MAX phases are shifted to lower 2θ values after HF
at slow rates, and stirring continued for 4 days for selective etching of treatment that indicates the larger d spacing in MXene after etching of
Al-layer from Ti3AlC2. After that, the product was centrifuged and Al layer. Further, from the XRD patterns of MAX phase and MXenes
washed until the pH becomes neutral. The obtained residue MXene was were reveals that the most intense non-basal plane peaks at ≈ 39° of
dried at 80°C for 24 hours. The delamination of MXene was carried out MAX phase disappear in MXene. Also, the peaks corresponding to (001)
by dispersion of prepared MXene into 50 ml DMSO solution and fol- (002), (004), and (0010), planes appear broadened with low intensity
lowed by continuous stirring for 24 hours at room temperature. The and shifted to lower angles compared to their location before treatment,
above solution was centrifuged at 3500 rpm for 5 minutes and washed which indicates the removal of Al and formation of MXene. In the XRD
with deionized water twice. The deionized water was decanted and pattern of MXene, some less intense peaks at 25, 37, and 47o correspond
sonicated with fresh deionized water. The delaminated layers of MXene to the partially oxidized TiO2. XRD pattern of MoS2 shows characteristic
in the supernatant liquid was separated [18]. peaks at 2θ = 14.38, 33.12, 39.69, 49.94, and 58.83° due to (002),
(100), (103), (105), and (110) planes, respectively, which was con-
2.3. Synthesis of MoS2/MXene firmed with ICCD 03-065-0160. Low intense peaks confirmed the con-
finement of MoS2 between the MXene layers at 2θ angles of 33.8, 39.4,
MoS2/MXenes heterostructures were prepared as follows, the ap- and 57.1° that corresponds to (100), (103), (110) planes of MoS2.
propriate amount of ammonium heptamolybdate was dissolved in a However, MoS2 peaks such as (002) at 14.38°, and (100) at 33.12° were
mixture of ammonium hydroxide (60 ml) and water (5 ml), and H2S gas cloaked in MoS2/MXene pattern due to nanostructured MoS2 formation
was purged at 25°C for 60 min, then slowly temperature was increased associated with MXene. On comparing the XRD patterns of MXene and
up to 60°C, the mixture turns dark red color [28]. The as-prepared MoS2/MXene, the (002) peak was found shifted to lower values that
MXene was then dispersed in the dark red color mixture for incipient indicate the increased interplanar spacing of MXene due to the confined
wetness impregnation, and the slurry was calcined at 300°C under ni- of MoS2 in between the layers of MXene [23].
trogen to obtain MoS2/MXene. Figures 2 and S1 show the N2 adsorption/desorption isotherms and
pore size distribution of MoS2/MXene and MXene, respectively. The
2.4. Characterization isotherm of MXene possesses both meso and microporous structures.
The specific surface areas of MXene and MoS2/MXene are calculated to
The synthesized MXene and MoS2/MXene were characterized by X- be 15.50 and 67.30 m²/g, respectively. The increased specific surface
Ray diffraction (XRD) using a Rigaku Miniflex 600 diffractometer with area of MoS2/MXene compared to MXene could be ascribed to the
Cu Kα radiation (λ= 1.54 Å). The diffraction data were recorded in the confinement of MoS2 between the MXene layers. The pore volume of
2θ range of 5–90° at 0.02° step size and 1s step time. The nitrogen MXene and MoS2/MXene are found to be 0.025 and 0.077 cm3/g. The
adsorption-desorption isotherms were measured at −196°C on a pore volume of MoS2/MXene increases due to the introduction of MoS2
Micromeritics ASAP 2010 volumetric adsorption analyzer. Before each into MXene layers (Figure S1). The large surface area and porous vo-
adsorption measurement, the samples were evacuated at 105°C under lume increase the contact area of the electrode and electrolyte, which

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M. Chandran, et al. Journal of Energy Storage 30 (2020) 101446

capacitive performance as there are many sites for ion intercalation and
shortening the paths for ion-diffusion. SEM images of MoS2/MXene
exemplifies the deposition of MoS2 layers onto the MXene layers so that
accordion-like structures of MXene are significantly concealed. The
elemental analysis of MoS2/MXene obtained by EDX analysis depicts
the presence of mainly Ti, Mo, S, which confirms the formation and
existence of MoS2 on the surface of MXene.
Figure 4 shows the XPS spectra of MoS2/MXene. The survey spectra
display the peaks corresponding to the presence of Ti 2p, C 1s, O 1s, Mo
3d, and S 2p of the MoS2/MXene (Figure 4a). The surface available
element electronic states are confirmed by high-resolution XPS spectra
data of each element. Figure 4b displays Ti 2p spectrum which consists
of four fitting peaks located at 454.5,458.5, 460.1, 464 eV binding
energies correspond to Ti-C (Ti 2p1/2), Ti-C (Ti 2p3/2), Ti−O (Ti 2p1/2),
Ti-O (Ti 2p3/2) peak that could contribute to the formation of TiC, TiCO,
and TiO2 bonds. The C 1s region in the XPS spectra of MoS2/MXene was
fitted with four peaks at 284.2, 285.80, 289.35, and 285.06 eV were
assigned to C-Ti, C=C, C−C, C-O and/or the C-S, respectively (Figure
4c). Peaks fitted the O 1s profile of the MoS2/MXene at 530.8, 531.8,
532.5 eV that corresponds to Ti-Ox and/or the Mo-Ox, Ti-(OH) x, and C-
O, respectively (Figure 4d), which reveals the formation of MoS2/
MXene. Further, in situ MoS2 formation was verified by high solution
XPS spectra of Mo3d (Figure 4e). The Mo 3d exhibits two most intense
peaks at 229.5 and 232.6 eV, which correspond to the Mo4+ 3d5/2 and
Mo4+ 3d3/2 of MoS2, respectively. In addition, a peak located at 226.7
eV is the S 2s of MoS2, and a peak situated at higher energy region at
235.8 eV is belongs to Mo6+, which corresponds to slight oxidation of
Mo edges in MoS2 from the Mo4+ state to the Mo6+ state [23]. Also,
figure 4f represents S 2p spectra that are fitted for two peaks at 162.31
and 161.5 eV, which ascribed to S 2p1/2 and S 2p3/2, respectively, which
further confirms the formation of MoS2 on the MXene layers.

3.2. Electrochemical performance of MXene and MoS2/MXene

heterostructures
Figure 1. XRD patterns of MAX phase (Ti3AlC2), MXene, MoS2, and MoS2
The electrochemical performance of MXene and MoS2/MXene was
/MXene.
investigated by cyclic voltammetry with the symmetric two-electrode
system using 1M H2SO4 as an electrolyte. Figure 5a and S2 shows the
cyclic voltammogram of MoS2/MXene and MXene at different scan
rates of 20, 50, 100 mVs−1 in the potential window of -1.5 to 1.5 V
respectively. It can be seen that the CV response of both MXene and
MoS2/MXene is in quasi-rectangular shape, indicating the materials
have good capacitive behavior. In general, cell voltage for aqueous
electrolyte solutions is about 1 V, and for organic electrolytes is around
3 – 3.5 V, the MoS2/MXene in aqueous H2SO4 electrolyte exhibits
oxidation/reduction in the potential window of -1.5 to 1.5 V and the
cell voltage is around 3 V. The enlarged potential window is due to the
synergetic effect of MXene and MoS2, which makes these MoS2/MXene
electrodes suitable for high power applications.
On increasing the scan rate, no significant oxidation or reduction
peaks in the CV response of MXene and MoS2/MXene was observed,
which exemplifies that these electrodes are charged and discharged at a
pseudo-constant rate over the complete cycle. However, the area of CV
curve for MXene and MoS2/MXene increases with increasing scan rate
without disrupting the overall rectangular shape, which suggests that
MXene and MoS2/MXene are electrochemically stable at high potenti-
ality. At higher scan rates, the effective interaction between the ions
and the electrode is greatly reduced because of the resistance offered by
Figure 2. N2 adsorption-desorption isotherms of MXene and MoS2 /MXene. MoS2 and hence stable at high potential. Figure 5b shows that the area
of CV curve for MoS2/MXene is significantly more than MXene elec-
are conducive to improve the electrochemical performances of MoS2/ trodes, which indicate higher specific capacitance due to the synergetic
MXene. effect of MXene and MoS2. During confinement of MoS2 into MXene,
Figure 3 ascribed to the surface morphology of MXene and MoS2/ the stacks of MXene are filled with MoS2, and the synergistic effect of
MXene. SEM images of MXene display accordion-like structures that are MoS2/MXene contributes more active sites for reversible actions and
similar to those reported elsewhere [16]. The layered MXene contains leads to a reduction in the internal resistance and enhances ion transfer
2D heterostructures that are more favorable for promoting super and pseudocapacitance behavior.

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M. Chandran, et al. Journal of Energy Storage 30 (2020) 101446

Figure 3. EDX analysis and SEM images of MXene (a,b) and MoS2/MXene (c,d).

Figure 4. XPS for the a) Survey b) Ti 2p, c) C 1s, d) O 1s, e) Mo 3d and f) S 2p region for MoS2 /MXene

The specific capacitance of MXene and MoS2/MXene were in- GCD curve of MoS2/MXene at a high current density 10, 12.5, 20 Ag−1
vestigated with GCD measurements. Figures 6 show the GCD curves also reveals the same trend (Figure S4). The charging and discharging
under different current densities of 0.4, 1.0, 1.6, 2.0, and 4.0 A g−1 for steps reveal a small internal resistance (IR) drop along with symmetric
MoS2/MXene and MXene (Figure S3). GCD curves of MoS2/MXene and charge curve and discharge curves of binary composites indicating the
MXene depict nearly symmetrical triangle on charging and discharging; pseudocapacitance behavior along with the double-layer capacitance.
linear voltage/time profiles, thereby demonstrates outstanding capaci- The specific capacitance (Csp) of the electrode is obtained from the
tive performance, rapid and reversible faradaic reactions of the device. following equation (1):

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M. Chandran, et al. Journal of Energy Storage 30 (2020) 101446

Figure 5. (a) Cyclic voltammogram of MoS2 /MXene modified electrodes in 1M H2SO4 at different scan rates 20, 50, and 100 mV s−1. (b) Cyclic voltammogram of
MXene and MoS2 /MXene composite in 1M H2SO4 at 100 mV s−1.

Figure 6. (a) Galavostatic charge-discharge curve of MoS2 /MXene at current density 0.4, 1, 1.6, 2, and 4 A g−1. (b) Galavostatic charge-discharge curve of MXene
and MoS2 /MXene at 0.4 A g−1.

Csp =
2It pseudo-capacitance. The total gravimetric capacitance of the electrode
vm (1) material CT is extracted from equation (2) and the surface contribution
Where I, t, Δv, and m are the constant current (A), discharge time to the capacitance by the electrode material CEDL was obtained from
(s), the total potential difference (V), and the weight of active materials equation (3). By considering the total capacitance (CT) as the sum of the
(g), respectively. With the above equation, the specific capacitance of surface (CEDL) and CPSUEDO, the capacitance contribution by the elec-
MXene is calculated to be 194, 140, 142, 137, and 99 F g−1, and MoS2/ trode material CPSUEDOwas calculated by equation (4). Figure 7 (a)
MXene is 342, 275, 261, 253, 212 F g−1, at 0.4, 1.0, 1.6, 2.0, and 4.0 A shows the plots of reciprocal of gravimetric capacitance (C−1) against
g−1, respectively. the square root of scan rate (v1/2), Figure 7(b) shows plots of gravi-
Figure 6b shows of GCD curves of MXene and MoS2/MXene at 0.4 A metric capacitance (C) against reciprocal of the square root of scan rate
g−1, which clearly demonstrates that the discharge time of MoS2/ (v−1/2). By Trasatti method, it is found that MoS2/MXene exhibits 45.9
MXene was higher than MXene due to enhanced ions transfer of MoS2 % EDL capacitance and 54.1 % pseudocapacitance (Figure 7 (c)).
confined into the layers of MXene and hence resulted in improved ca- C 1 = constant *v 0.5 + CT 1 (2)
pacitance. The large specific surface area of the MoS2/MXene compo-
sites significantly reduces the diffusion path, increasing the interfacial
C = constant *v 0.5 + CEDL (3)
contact facilitating the fast transportation of electrons during the
charge/discharge process. This unique architecture enables the MXene/ CT = CEDL + CPSUEDO (4)
MoS2 composites electrode to have the best electrochemical capaci-
0.5 0.5
tance. Figure 8 (a) shows the plot of (V)/ν vs.ν for MoS2/MXene at
The capacitance from the CV curves of MoS2/MXene at the scan rate 0.25, 0.5, and 0.75V and used to derive the contributions by diffusion-
from 1 to 50 mV/s was analyzed with the help of the Trasatti method controlled current and capacitive current using Dunn's method with the
[29, 30] to differentiate the contribution from EDL capacitance and following equation (5) and (6)

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M. Chandran, et al. Journal of Energy Storage 30 (2020) 101446

Figure 7. (a) Plots of reciprocal of gravimetric capacitance (C−1) against the square root of scan rate (v0.5). (b) Plots of gravimetric capacitance (C) against reciprocal
of the square root of scan rate (v−0.5). (c) EDL capacitance (%) and pseudocapacitance (%) for MoS2/MXene by Trasatti method.

I (V ) = k1 v + k2 v 0.5 = ICapacitive + IDiffusive (5) frequencies, there is the presence of partial semicircle due to MoS2 charge
0.5 transfer resistance. The Rs value of MXene and MoS2 /MXene are at 1.92
Equation (5) when divided by v
and 1.88 Ω cm−2. The Rs value reveals that MoS2 /MXene has less
I (V ) equivalent series resistance than MXene, which might be due to the pre-
= k1 v 0.5 + k2
v 0.5 (6) sence of MoS2 and implants good conductivity on MXene.
The stability of MXene and MoS2 /MXene was assessed by GCD (Figure
Figure 8 (b) illustrates the % contribution by diffusion control
S5) and Nyquist plot (Figure S6). GCD plot of MoS2/MXene at a current
current and capacitive current at 0.25V for MoS2/MXene at scan rates
density of 20 A g−1 before and after 10000 cycles show more than 99 % of
1,2,5,10,20,30,40 and 50 mV/s. It can be seen that contribution by
discharge time was retained even after 10000th cycle. Another compelling
diffusion control current increases with increase scan rate, which is in
evidence from the cycle stability by Nyquist plot reveals that resistance
agreement in the available report [31].
value decreases after 10000 cycles, which indicates that the conductivity
The electrochemical performance of MoS2/MXene was verified with
of MoS2 /MXene increases, and hence the highly stable MoS2/MXene can
electrochemical impedance measurement. Figure 9 shows the Nyquist
be used as electrode material in long-term storage devices. Thus, the
plots of MXene and MoS2/MXene composite. The impedance spectroscopy
confinement of MoS2 between the MXene layers validates excellent rate
results exposed semicircle in the high-frequency region and linear plot in
performance that illustrates stable structures of MoS2/MXene even after
the low-frequency region. The impedance was measured within a fre-
10000 cycles under a high current density (20 A g−1).
quency range from 100 kHz to 10 m Hz with AC amplitude of 10 mV, and
Figure 10 shows the Ragone plot of MXene and MoS2 /MXene at the
data reveals nearly ideal capacitive behavior at low frequencies due to the
charging rate 0.4, 1.0, 1.6, 2.0, and 4.0 A g−1. The energy density E (W
limiting mass transport of MoS2 (Warburg resistance). Whereas, at high

Figure 8. (a) Plot of (V)/ν0.5vs.ν0.5 for MoS2/MXene at 0.25, 0.5, and 0.75V. (b) Diffusion controlled current (%) and capacitive current (%) for MoS2/MXene with
0.25V at scan rates 1,2,5,10,20,30,40 and 50 mV/s.

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M. Chandran, et al. Journal of Energy Storage 30 (2020) 101446

3600
P=E×
t (8)

V(ΔV) is the discharge potential window, and the Δt (s) is the dis-
charge time. It is observed that a maximum power density of 758 W
kg−1 was observed at the energy density range of 202 W h kg−1 for
MXene, and a power density 755 W kg−1 was observed at the energy
density range of 355 W h kg−1 for MoS2 /MXene at charging rate 0.4 A
g−1. A high energy density of 355 W h kg−1 for MoS2 /MXene makes it
an excellent electrode material with high energy density and power
output.
Also, Table 1 shows the comparative study of MoS2/MXene with the
other reported MoS2 materials that display high specific capacitance
and more than 99 % activity after 10000 cycles for MoS2/MXene. The
specific capacitances, energy densities, and cycling lives results ob-
tained for MoS2 /MXene are almost comparable with the few MOF
composites constructed as 2D layered architectures [32-34] Im-
portantly, the enlarged voltage window with an aqueous electrolyte and
high specific capacitances adds credit to MoS2/MXene. Thus, from the
above results, MoS2/MXene was recognized as a remarkable electrode
material for high power supercapacitors.
Figure 9. Nyquist plots of MXene and MoS2 /MXene.

4. Conclusions

MXene was successfully derived from MAX phase, and MoS2/MXene

heterostructures were formulated by the incipient wetness impregna-
tion method. The removal of Al from MAX phase and formation of
layered MXene was confirmed by XRD analysis. SEM-EDX and XPS data
revealed the formation of layered MXene and incorporation of MoS2
into the MXene layers. Further, BET analysis reflected the corre-
sponding changes in the surface area and pore volume of MoS2/MXene
due to the incorporation of MoS2 into MXene. A well defined quasi
rectangular shape CV response was obtained for MXene and MoS2/
MXene that shows pseudo-capacitor behavior. A maximum specific
capacitance of 342 F g−1 at 0.4 A g−1 in enlarged voltage window from
-1.5 V to 1.5 V was calculated for MoS2/MXene by GCD analysis. GCD
and impedance spectroscopy analysis depicts excellent cycle stability
and electrical resistance of MoS2/MXene. The incorporation of MoS2
decreases equivalent series resistance in MoS2/MXene. GCD data re-
vealed that the more than 99 % discharge time of MoS2/MXene was
retained even after 10000 cycles, and impedance data shows that in-
Figure 10. Ragone plot of MXene and MoS2 /MXene composite. ternal resistance decreases after 10000 cycles, which demonstrates that
MoS2 MXene can be used as electrode materials for long-term storage
devices. Thus, the MoS2/MXene heterostructure can be recognized as
h kg−1) and power density P (W kg−1) can be derived from the Gal-
an excellent electrode material for application in supercapacitors.
vanostatic charge-discharge data according to Equation (6) and (7):

E = 0.5 × C × v 21000 Declaration of competing interest

3600 (7)

The authors declare that we have no conflict of interest.

Table 1
Comparative study of MoS2 based electrode materials for specific capacitance study.
Electrode material Electrolyte Specific Capacitance (F g−1) Current density (A g−1) Retention (%) Ref.

MoS2-carbonite 1M Na2SO4 201.4 0.5 94.1 after 1000 cycles [35]

MoS2-Graphene hybrid films 1M Na2SO4 255.0 20 µA 93.0 after 1000 cycles [36]
MoS2-G 1M Na2SO4 270.0 0.1 89.6 after 1000 cycles [37]
nanocomposite
MoS2-MWCNT composite 1M Na2SO4 452.7 1 95.8 after 1000 cycles [38]
MoS2-graphene composite 1M Na2SO4 243.0 1 92.3 after 1000 cycles [39]
MoS2-RCF composite 1M Na2SO4 225.0 0.5 78.6 after 2000 cycles [40]
MoS2-graphene aerogel composite 1M Na2SO4 268.0 0.5 93.0 after 1000 cycles [41]
MoS2-RGO composite 1M H2SO4 442.0 1 90.3 after 1000 cycles [42]
MoS2-Ti3C2 1M H2SO4 342 0.4 > 99% after 10000 cycles This Work

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Acknowledgments outstanding volumetric capacitance, Adv. Funct. Mater 27 (2017) 1701264.

[20] Y.P. Gao, K.J. Huang, X. Wu, Z.Q. Hou, Y.Y. Liu, MoS2 nanosheets assembling three-
dimensional nanospheres for enhanced-performance supercapacitor, J. Alloys
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