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Accepted Manuscript
Three-dimensional S-MoS2@α-Fe2O3 nanoparticles composites as lithium-ion
battery anodes for enhanced electrochemical performance
Cheng-Yu Wu, Wei-En Chang, Yu-Guang Sun, Jyh-Ming Wu, Jenq-Gong Duh
MAC 20902
To appear in:
Materials Chemistry and Physics
Received Date:
09 May 2018
Accepted Date:
20 August 2018
Please cite this article as: Cheng-Yu Wu, Wei-En Chang, Yu-Guang Sun, Jyh-Ming Wu, Jenq-Gong
Duh, Three-dimensional S-MoS2@α-Fe2O3 nanoparticles composites as lithium-ion battery anodes
for enhanced electrochemical performance, Materials Chemistry and Physics (2018), doi: 10.1016/j.
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Three-dimensional SMoS2@α-Fe2O3 nanoparticles
composites as lithium-ion
battery anodes for enhanced
electrochemical performance
Cheng-Yu Wu, Wei-En Chang, Yu-Guang Sun, Jyh-Ming Wu*, JenqGong Duh*
Department of Material Science and Engineering, National Tsing-Hua
University, Hsinchu, Taiwan
Corresponding author:
Tel.: +886-3-571-2686.
E-mail address: (J.G. Duh),
(J.M. Wu)
Two-dimensional (2D) structures have received substantial attention in the energy
applications. However, a common problem with 2D layered structures is restacking
during the charge–discharge process. In this work, a graphene-like structure,
molybdenum disulfide (S-MoS2), was synthesized using the hydrothermal method.
Moreover, zero-dimensional (0D) α-Fe2O3 nanoparticles were constructed to act as a
spacer in the slurry. Subsequently, the three-dimensional (3D) S-MoS2@Fe2O3
nanoparticles were fabricated by the ultrasonic vibration process to improve their
electrochemical properties.
On the basis of the 3D architecture, the α-Fe2O3
nanoparticles not only prevent the restacking of MoS2 sheets, but also increase
accessibility for electrolyte penetration to provide more active sites and lower the
diffusion energy barrier for Li+ ions during the charge–discharge process. In the
potential window of 3 V to 0.01 V, high-rate charge–discharge and long cycle tests
were performed to investigate the electrochemical performance of all electrodes. The
electrochemical performance was enhanced through spatial distribution of MoS2. In
summary, these S-MoS2@Fe2O3 nanoparticles possess high potential for application as
anode materials in next-generation lithium-ion batteries.
Keywords: 3D structure, MoS2, anode, lithium-ion battery
1. Introduction
Lithium-ion batteries (LiBs) are widely used in consumer electronics products,
such as portable electronics and electric vehicles, and are a promising candidate for
next-generation energy storage[1]. The primary anode material in batteries is natural
graphite, but it still has a limitation for high energy storage above ~ 372 mAhg-1,
although it is quite stable with chemically inert. To meet the requirements of
transportation electrification and renewable energy integration, scientists have focused
on developing high-working-voltage and high-capacity LiBs. Alloy-type materials,
such as Si[2, 3] and Sn[4], have high capacity owing to their reaction with Li ions to
form a lithiated compound. Nevertheless, a common problem of alloy-type materials is
volume expansion during the charge/discharge process, which could aggravate the
failure of the battery and trigger human hazards.
Two-dimensional (2D) structures have received substantial attention in the field
of energy[5-9] and catalysis related field[10-13]. The structures are superior to alloy-
type structures and have a high theoretical capacity, resulting in the 2D materials, which
may exhibit a great potential for use as substitutes to alloy-type materials. Recently,
molybdenum disulfide (MoS2) has become a common anode material for LiBs[14-20].
It comprises transition metal and sulfide layers that are stacked on each other by a weak
van der Waals interaction. However, a drawback of the 2D materials is restacking of
neighboring materials during the charge–discharge process, which could result in the
electrolyte infiltration to prevent ionic transportation in battery.
To solve this problem and to improve the cycling performance of the LiBs , several
studies have modified 2D materials using various methods, such as coating[21-23],
composites[24-37], doping[38, 39] and structural design[22, 40-47]. Jiang et al. used
MoS2–carbon composites to create an interoverlapped superstructure that can
efficiently improve Li-ion storage and achieve cycling stability[30]. Similarly, Chen et
al. demonstrated the development of high-energy-density, high-capacity LiB
anodes[28]. In mitigating the restacking effect and enhancing the electrical conductivity
by designing the conductive networks and buffer space to provide an accessible
approach for prolonging the cycling lifetime of MoS2 anodes.
In this work, the MoS2 was used to combine with α-Fe2O3 nanoparticles to
fabricate the LiB anodes. The feature of α-Fe2O3 acted as a spacer in this system. The
aim was to realize the chemical performance of MoS2 anodes by designing a fluent
pathway for Li ions. These results indicate that 2D structures improved by 3D structure
have high potential in high-performance applications in the future.
2. Experimental
2.1. Synthesis of MoS2
The MoS2 was synthesized using the hydrothermal method [11-13]. First,
Na2MoO4.2H2O (98% purity) and CS(NH2)2 (99% purity) were added to a deionized
(DI) water solution. Subsequently, 1 mL of HCl was slowly added while stirring. After
the stirring, a conductive substrate was placed into a Teflon-lined stainless-steel
autoclave and maintained at 220 °C for 24 h. Finally, a black bulk MoS2 powder was
obtained by washing the substrate.
2.2 Synthesis of graphene-like MoS2 sheets
The lithiated MoS2 was prepared using the hydrothermal process and exfoliated
by ultra-sonication process[34]. First, an appropriate amount of LiOH was dissolved in
ethylene glycol (EG) under constant stirring to obtain a uniform solution. The bulk
MoS2 powder was added to the LiOH solution and vigorously stirred for 1 h.
Subsequently, the mixture was transferred into the autoclave and heated at 220 °C for
24 h. Lithiated MoS2 powder was obtained through centrifugation. The product was
washed with acetone to eliminate EG and LiOH and added to DI water under
ultrasonication for 30 min. Finally, sheet-like MoS2 (S-MoS2) was obtained.
2.3 Synthesis of α-Fe2O3 nanoparticles
Calcination process was employed to prepare α-Fe2O3[48]. First, FeCl3·6H2O
(reagent grade, ≥98%) was added to DI water under ultrasonic vibration. Next, a red
flocculent precipitate appeared immediately when methyl orange (0.05 M) was added
to the solution. After that, the product was collected and washed with distilled water
several times and then dried under vacuum. Finally, α-Fe2O3 nanoparticles were
fabricated through pyrolysis of the product at 800 °C in a furnace for 5 h in atmosphere.
2.4 Fabrication of S-MoS2@Fe2O3 composite
A self-assembly process was employed to synthesize the S-MoS2@Fe2O3
composite through ultrasonication. In brief, α-Fe2O3 nanoparticles were added to 100
mL of DI water and then mixed uniformly in an ultrasonic bath for 1 h. Subsequently,
the S-MoS2 was added to the solution under stirring for another hour. The ratios of S-
MoS2 and α-Fe2O3 were controlled at 10 and 1 wt%, respectively. The mixture was then
filtered and rinsed with DI water. Finally, the samples were collected and dried in a
vacuum oven at 60 °C for 24 h to obtain the S-MoS2@Fe2O3 composite.
2.5 Characterization
The surface morphology was observed using field-emission scanning electron
microscopy (JEOL 7600F, Japan). The phases were identified through high-resolution
transmission electron microscopy (HR-TEM, JEOL Cs Corrected Field Emission TEM,
Japan) and X-ray diffractometry (XRD, Rigaku TTRAX III, Japan). The
electrochemical properties were characterized by using the coin cell method (type 2032)
with various electrodes as working electrodes. The Li foil was used as the counter
electrode and reference electrode. The electrolyte used was 1 M LiPF6 in an ethylene
carbonate and ethyl-methyl carbonate mixed solution (volume ratio 1:1). All cells were
assembled in an Ar-filled glove box (H2O < 0.1 ppm, O2 < 0.1 ppm) to avoid water
contamination. The cells were analyzed using the charge–discharge process (ArbinBT2000) in the potential window of 0.01 –3 V, and the cycling test was performed at
0.2 C in the same potential window for 70 cycles.
3. Results and Discussion
The synthesized MoS2 powders, namely bulk-like MoS2 (B-MoS2), sheet-like
MoS2 (S-MoS2) and S-MoS2@Fe2O3, are shown in Fig. 1. The B-MoS2 was shown in
Figure 1(a), revealing that the B-MoS2 powder did not exhibit a high surface to volume
ratio. In contrast, as illustrated in Figures. 1(b) and 1(c), the lithium ions are intercalated
into the laminae of MoS2 to form lithiated MoS2. The product was washed under
ultrasonication for 30 min with DI water. Finally, S-MoS2 was obtained. The products
comprise well-dispersed nanosheets with abundant active surfaces. The reaction
formula is shown as follows:
LiMoS2 + H2O → S-MoS2 + LiOH + 1/2H2
The α-Fe2O3 nanoparticles have an average size of approximately 20 to 100 nm,
as shown in Fig. 1(d). The XRD pattern in Fig. 1(e) shows a single phase of MoS2,
including the polycrystalline Fe2O3 structure.
As shown in Fig. 2(a), the HR-TEM image illustrates that the α-Fe2O3 was mixed
into the MoS2 to form a heterojunction structures. In Fig. 2(b), the spacing between
atoms were 0.32 nm and 0.27 nm which is identified to be the (0 0 2) crystal plane of
MoS2 sheets and the (1 0 -1 4) crystal plane of Fe2O3, respectively. In addition, the
different fast Fourier transform (FFT) images in the inset of Fig. 2(b) can effectively
check the lattice constant as 0.32 nm and 0.27nm, respectively. In Fig. 2(c), The STEM
model can be used to identify each element of the sphere structure that is attributed to
Fe and O. Furthermore, Mo and S were uniformly distributed around the sphere
structure, implying that S-MoS2 and α-Fe2O3 were uniformly mixed without
The electrochemical performance for various types of MoS2 was investigated. As
shown in Fig. 3(a), the bulk-like MoS2 anode showed poor cycling stability that dropped
markedly within 20 cycles. By contrast, a flower-like S-MoS2 sample exhibited good
stability in capacity. After 20 cycles, the remaining capacity was approximately 900
mAhg-1, which can be attributed to the high surface area of the flower-like MoS2. The
petal structures mitigate restacking of the material during the charge and discharge
processes to prevent capacity fading. Nevertheless, capacity fading became more severe
after 20 cycles. Among all the samples, S-MoS2@α-Fe2O3 exhibited the greatest
stability in capacity. Adding α-Fe2O3 nanoparticles enhances stability because of the
crucial role played by MoS2 anodes in capacity retention. The capacity was 600 mAhg-1
after 70 cycles, which is higher than that of B-MoS2 and S-MoS2, and the fading rate
was lower. Moreover, the coulombic efficiency of S-MoS2@α-Fe2O3 was much higher
than that of the other samples. A schematic of the potential mechanism underlying
stability improvement is shown in Fig. 3(b). In fact, Bulk-like MoS2 exhibited a lower
surface area than the other samples. In fact, its surface area was not sufficiently high
for the MoS2 to react with Li+ ions to achieve high capacity. After exfoliation, S-MoS2
exhibited a much higher capacity than bulk-like MoS2 because of their high surface to
volume ratio. This resulted in a short migration path of Li+ into the host and provided
more electrolyte to infiltrate the electrode. However, this type of 2D structure suffers
from the restacking effect. Therefore, α-Fe2O3 was used to create a 3D architecture,
including 0D spacer which not only prevented restacking of the MoS2 sheets but also
increased accessibility for electrolyte infiltration to provide more active sites and lower
the diffusion energy barrier of Li+ ions during the charge–discharge process. As a result,
the 3D structure of S-MoS2@Fe2O3 exhibits high stability.
Fig. 4(a) shows the cyclic voltammetry curves to clarify the electrochemical
behavior of S-MoS2@Fe2O3. In the first cycle, the negative scan began at 1.5 V, which
can be attributed to Li-ion insertion into α-Fe2O3 to form LixFe2O3. The peaks at 1.1 V
and 0.6 V correspond to MoS2 transfer to LixMoS2 (1.1 V vs Li/Li+) and solid
electrolyte interface formation (0.6 V), respectively. The last peak around 0.3 V
indicates LixMoS2 transfer to Mo, which was shifted to a lower voltage after the first
cycle. By contrast, the positive scan exhibited two peaks at 1.6 V and 2.3 V,
corresponding to the conversion of Mo to MoS2 and Li2S to S, respectively.
Subsequently, a new peak at 1.9 V indicates S transfer to Li2S. Fig. 4(b) depicts the
voltage profile of S-MoS2@α-Fe2O3, which is in good agreement with the result of
cyclic voltammetry test. In order to confirm the capacity of Fe2O3, the Fe2O3 was
assembled as the coin cell to test the electrochemical performance. The data is shown
in Fig. 4(c). In first cycle, the long plateau that appeared near 0.8 V is attributed to the
conversion from Fe(II) to Fe (0) and the decomposition of electrolyte. A small plateau
from 1.5 to 2.2 V shown in the charge curve is corresponding to the reverse reaction.
To compare the reaction plateau between MoS2 and Fe2O3, the reaction plateau of Fe2O3
is observed below 2.2V. Thus, In Fig. 4b, the contributed capacity of Fe2O3 in the
system only provide a little. The main capacity comes from MoS2 itself. This result
proves that the capacity of MoS2 slowly decreased by cooperation with α-Fe2O3.
To determine the stability of MoS2, the discharge capacities of all samples cycled
at various current rates (0.2 C to 5 C) as shown in Fig. 5(a). S-MoS2@Fe2O3 exhibits
more stability in capacity than the other samples because of the smooth aisle of Li+ ions
during the charge–discharge process. The capacity of S-MoS2@ Fe2O3 was
approximately 500 mAhg-1, which is higher than that of bulk-like MoS2 at a high current
rate. The results indicate that an appropriate amount of α-Fe2O3 added to MoS2 can
improve the capacity at various current rates because of the reduction of both the Li+
diffusion pathway and electrochemical resistance. The electrochemical impedance
spectroscopy was further employed to investigate this result. All the cells were analyzed,
and the Nyquist plots are shown in Fig. 5(b). The Nyquist plots can be analyzed by
fitting the spectra using the equivalent circuit inset in Fig. 5(b). In the figure, Rs denotes
the resistance of the electrolyte, Rct is the charge transfer resistance of the electrode or
electrolyte, CPE is the interface capacitance of the electrode or electrolyte, and Wo1 the
Warburg impedance. As the semicircular portion of the Nyquist plot shows, the charge
transfer resistance of the S-MoS2@Fe2O3 electrode was slightly lower than that of bulklike MoS2. This indicates that the nanoparticle improves MoS2 stability during cycling
and thus verifies the improved electrochemical performance of MoS2. This result also
confirms that the special design is more beneficial to transportation of charge. As a
consequence, this 3D architecture design not only prevents the restacking effect of
MoS2 sheets, but also enhances approachability of electrolyte to penetrate, providing
lower diffusion energy barrier for Li+ ions during the charge–discharge process.
4. Conclusions
In this study, MoS2 was enhanced through a simple method. The exfoliation
processes can effectively enhance the capacity of MoS2. Nevertheless, the restacking
phenomenon inevitably affects 2D material, which can aggravate the fading of capacity
after a few cycles. Therefore, α-Fe2O3 was used as a spacer to prevent the restacking of
2D material during the cycling process. S-MoS2@Fe2O3 exhibited an initial reversible
capacity of approximately 1000 mAhg-1 and a high capacity of approximately 600
mAhg-1 after 70 charge–discharge cycles with a low decay. In addition, it also exhibited
excellent capacity in a rate test. The improved anode performance can be attributed to
the accessible active sites of 2D structures obtained via the special design and the
reduction of the ionic transportation pathway. These results indicate that 2D structures
have high potential in high-performance applications in the future.
Fig1. SEM images of various condition (a) B-MoS2, (b) S-MoS2, (c) S-MoS2@Fe2O3
(d) Fe2O3 nano-particles and (e) XRD analysis
Fig2. (a,b) HR-TEM images with FFT imges (c)EDS images with SEM model.
Fig3. (a) Reversible capacity and Coulombic efficiency for the 70 cycles are plotted
with various electrodes at rate 0.2 C. (b) . The schematic diagram of experimental
process and mechanism.
Fig4. (a) The first three cycles of cyclic voltammogram for S-MoS2@Fe2O3 from 3V
to 0.01 V versus Li/Li+ at 0.2 mV s-1 scan rate. (b) The voltage profile of SMoS2@Fe2O3 with different cycles and (c)The voltage profile of Fe2O3 with different
Fig 5. (a) Capacities of samples MoS2, S-MoS2 and S-MoS2@Fe2O3 subject to charge–
discharge under different charging rates. (b) The EIS impedance of MoS2, S-MoS2 and
S-MoS2@Fe2O3 after first three cycles. The frequency is ranged from 0.1 MHz to 0.1
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