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Accepted Article
A Journal of
Title: Multi-layer-Cake WS2/C Nanocomposite as A
High-PerformanceAnode Material for Lithium-Ion Batteries: "regular"
and "alternate"
Authors: Jiaming Zou, Liu Cheng, Zhanxu Yang, Chengyuan
Qi,Xiaorong Wang, Qingdong Qiao, Xian Wu, and Tieqiang Ren
This manuscript has been accepted after peer review and appears
as anAccepted Article online prior to editing, proofing, and formal
publicationof the final Version of Record (VoR). This work is
currently citable byusing the Digital Object Identifier (DOI) given
below. The VoR will bepublished online in Early View as soon as
possible and may be differentto this Accepted Article as a result
of editing. Readers should obtainthe VoR from the journal website
shown below when it is publishedto ensure accuracy of information.
The authors are responsible for thecontent of this Accepted
Article.
To be cited as: ChemElectroChem 10.1002/celc.201700414
Link to VoR: http://dx.doi.org/10.1002/celc.201700414
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ARTICLE
Multi-layer-Cake WS2/C Nanocomposite as A High-Performance Anode
Material for Lithium-Ion Batteries: “regular” and “alternate”
Jiaming Zou, Cheng Liu, Zhanxu Yang*, Chengyuan Qi, Xiaorong Wang*,
Qingdong Qiao, Xian Wu and Tieqiang Ren
Abstract: A multi-layer-cake WS2/C nanocomposite was
successfully synthesized via an intercalation-transformation
method, in which few-layered WS2 and carbon were sandwiched in an
alternating sequence. As a benefit of the electronic conductivity
enhanced by the interlayer carbon and the unique “regular” and
“alternate” architecture, the WS2/C nanocomposite showed promising
performance as anode material for lithium-ion batteries. The
nanocomposite demonstrated a high capacity of 829.4 mAhg-1 at 0.3
Ag-1 after 140 cycles and it could still deliver a stable capacity
of about 326.8 mAhg-1 at a current density of 8.0 Ag-1.
Introduction
The rechargeable lithium-ion batteries (LIBs) that commonly use
graphite as commercial anode material have revolutionized the
portable electronic devices, hybrid electric vehicles and emerging
smart grids.[1-4] However, for the next-generation LIBs, graphite
as an anode material cannot meet the requirements due to its low
theoretical specific capacity (372 mAhg−1). To fundamentally
address this issue, it is necessary to design and improve advanced
electrode materials with high specific capacity and good cyclic
stability for future applications.[5-10]
WS2 as a member of the layered transition metal dichalcogenides
(LTMDs) has received tremendous attention owing to its high
specific capacity (ca. 433 mAhg-1 based on 4 mol of Li+
insertion)[11,12] and good lithium storage performance. It is
composed of S-W-S layers stacked together through weak Van der
Waals interactions during the process of facile insertion and
extraction of Li+. However, two-dimensional S-W-S layers inevitably
are re-stacked with volume expansion during the cycling process,
which causes a rapid capacity decrease and poor rate performance.
To overcome these drawbacks, one widely adopted strategy is to
disperse nano-WS2 into a 2D or 3D conductive matrix such as
carbons.[13-16] This can not only improve the electric conductivity
of the electrode greatly but also provide space to buffer the
volume changes of WS2 during the charge/discharge process, thereby
leading to enhanced cycling and rate performance. However, the
WS2/carbon 2D hybrid structures with high surface energy tend to
re-aggregate or restack, and the WS2/carbon 3D hybrid materials
need templates. The two types of dispersed structures with
disordered WS2 are not able to effectively and easily take full
advantage of the fast charge/release characteristics of WS2. So, if
we change the disordered arrangement of WS2 for WS2 layers-based
nanocomposites to orderly one, what would happen? Moreover, [*] J.
Zou, C. Liu, Prof. Z. Yang, C. Qi, Prof. X. Wang, Q. Qiao, X. Wu,
T. Ren
College of Chemistry, Chemical Engineering and Environment
Engineering
Liaoning Shihua University Fushun Liaoning 113001 P. R. China
E-mail: [email protected]; [email protected];
[email protected] Supporting information available:
Figure S1, S2, S3; See DOI:
it is still difficult to obtain pure WS2 in a green,
cost-effective and easy way.[12, 17] The impurities directly affect
the electrochemical performance for reversible lithium storage.
Therefore, it is challenging to synthesize “regular” pure-WS2
layers-based nanocomposites for LIBs. In this work, we report a
novel regular pure-WS2 layers/carbon nanocomposite called
“multi-layer-cake”. The alternating WS2 layers (5~8 layers) and
carbon layers constitute the skeleton together. The few-layered WS2
can minimize transport problems for both electrons and lithium
ions. The intercalated carbon layers help prevent the restacking of
WS2 sheets and increase the conductivity of the electrode when used
as LIBs. The whole 3D structure formed can limit the volume
expansion of WS2. This design by using the topological effect of
material structure, is totally different from other reports on
former 2D or 3D structures where WS2 is dispersed into the
conductive matrix. Such a “multi-layer-cake” structure can be
prepared in two easy steps. The first step is to synthesize the
“multi-layer-cake” structure of WO3-x / C. The second step is in
situ conversion from WO3-x to pure WS2. The whole preparation
process is simple, non-toxic and cost-effective. Meanwhile, the
as-prepared hybrid material exhibits excellent lithium storage
properties with high capacity, stable cycling performance, and
remarkable rate capability. To the best of our knowledge, the
unique “Multi-layer-Cake” 3D architecture of WS2/C for anode
material in this paper is reported for the first time thus
contributing to the design of next generation of LIBs.
Scheme 1. Schematic of the synthesis process of Multi-layer-Cake
WS2/C nanocomposite.
10.1002/celc.201700414ChemElectroChem
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ARTICLE
Results and Discussion
Figure 1A shows the XRD patterns of WS2/C nanocomposite and bare
WS2. As shown in Figure 1A, both samples can be assigned to
hexagonal WS2(JCPDS no. 08-0237).[11,15,18]
However, the diffraction peaks for the WS2/C nanocomposite
(Figure 1A(b)) are distinguished from that of bare WS2 (Figure
1A(a)), in that the (002) peak appears from 13.81º to 13.53º,
indicating an expansion of interlayer distance, which leads to a
larger space for Li ions intercalation.[19-21]
Figure 1. XRD patterns of bare WS2 (a) and WS2/C nanocomposite
(b) (A); XPS spectra of WS2/C nanocomposite: the survey scan (B), W
4f (C), S 2p (D) and C 1s peaks (E), respectively. X-ray
photoelectron spectroscopy (XPS) measurement was conducted to
analyze the element valence states of the WS2/C nanocomposite. As
shown in the overall XPS spectra (Figure 1B), W, S, C and O can be
detected on the surface. The presence of O element may be due to O2
adsorbed on the sample surface.[11,22] Figure 1C shows typical
deconvoluted XPS scan for W(4f) of WS2/C thin film, and W(4f) peak
was observed in the range 31eV-40 eV. It was further deconvoluted
into three component bands nearly 32.9 eV, 35.3 eV and 38.5 eV,
which were assigned to W 4f7/2, W 4f5/2 and W 5p3/2 peaks,
respectively. The positions of these XPS peaks suggested that the
valence of W is +4, the evidence for the complete conversion of the
WO3-x phase to WS2.[23,24] Figure 1D shows typical deconvoluted XPS
scan for sulfur (2p) of WS2/C thin film, a S (2p) peak was observed
in the range 159 eV-166 eV. It was deconvoluted into the two
component bands nearly 162.2 eV and 163.5 eV, which were assigned
to S 2p1/2 and S 2p3/2 peaks respectively. All of
these results are consistent with the reported values for WS2
crystal.[11] A sharp peak of C 1s was detected at 284.8 eV with a
small portion of graphitic carbon in the region of 286-288 eV
(Figure 1E). The asymmetric peak reveals that the carbon exists as
a mixture of sp2 and sp3 bonding.[25,26] Raman shift of WS2/C
nanocomposite is shown in Figure 2A. Two prominent peaks
corresponding to the in-plane E12g and out-of-plane A1g modes of
WS2 were observed, which also verified that the crystalline WS2
phase was successfully prepared.[27,28] The peaks at 1359cm-1 and
1587cm-1 were assigned to the disordered carbon peak (D band) and
the ordered graphitic carbon peak (G band), thus verifying the
presence of the carbon in the composite. As shown in Figure 2B, 2C
and Figure S1C (low magnification top view SEM image), the WS2/C
nanocomposite retained the Multi-layer-Cake structure of precursor
H2W2O7 and WO3-x/C nanocomposite (Figure S1A and S1B). The WS2
nanosheets are tightly stacked together due to the unique
Multi-layer-Cake structure, indicating that the WS2 nanosheets will
have maximum electrical contact with carbon. And, it could result
in hybrids with a high conductivity. In order to gain a much
clearer knowledge of the Multi-layer-Cake structure, HRTEM was
conducted to obtain a closer observation of the WS2/C
nanocomposite. As shown in Figure 2D, the WS2 with few layers (5-8
layers) and carbon were sandwiched in an alternating sequence and
the clear lattice fringes corresponded to the interlayer distance
between the (002) crystal planes along the c-axis of WS2, the value
of which was 0.65 nm consistent with the XRD measurements.
Furthermore, the carbon was intercalated between the WS2
interlayers and tightly immobilized with ~8.11 nm thick, which
could provide a buffer matrix for the volume change of WS2 during
lithiation as well as unique electrical conductivity.[29] The
crystalline structure of WS2 was characterized by the selected area
electron diffraction (SAED) pattern (Figure 2E). The computed
interlayer distances from the
Figure 2. Raman spectra of WS2/C nanocomposite under excitation
wavelength of 532 nm (A); The cross-section SEM images of WS2/C
nanocomposite (B,C); HRTEM image of WS2/C nanocomposite (D); SAED
pattern of WS2/C nanocomposite (E).
10.1002/celc.201700414ChemElectroChem
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ARTICLE
SAED pattern were 0.28 and 0.16 nm, which well matched with the
d spacing values for the (100) and (110) planes of hexagonal WS2,
respectively. Figure S2 shows the first three CV curves of the
WS2/C electrodes. In the 1st cycle, a reduction peak around 1.5 V
and oxidation peak at 2.38 V were attributed to the lithium
intercalation/deintercalation according to the conversion reaction:
WS2+xLi++xe-→LixWS2. The strong reduction peak at 0.49 V was
ascribed to the reduction of LixWS2, or the formation of Li2S
originated from the conversion reaction (WS2+4Li++4e-→W+2Li2S) and
accompanying the irreversible decomposition of nonaqueous
electrolyte.[30,31] From the 2nd cycle onwards the reduction peak
at 0.49 V disappeared while a new reduction peak appeared in the
potential range from 1.6-2.2 V. This change can be explained by the
formation of a gel-like polymer layer formed out of the dissolution
of the Li2S in the electrolyte.[30] The cyclic voltammograms were
nearly perfectly superimposable in subsequent cycles and yielded
the same peak current and the same integrated peak area from cycle
to cycle. The CV measurements were the evidence of the good
electrochemical reversibility and cycle stability of WS2/C
nanocomposite as Li+ storage hosts. The WS2/C nanocomposite was
then galvanostatically charged (lithiation) and discharged
(delithiation) in the 0.01 and 3.0 V voltage window at a current
density of 0.3 Ag-1. As shown in Figure 3A, the WS2/C nanocomposite
demonstrated high specific capacity and favorable cycling stability
compared with the bare WS2. These good cycling properties resulted
from the unique Multi-layer-Cake structure of WS2/C nanocomposite.
The carbon sandwiched between WS2 nanosheets ensures good contact
with WS2, so that it can act as an electron pathway during
electrochemical cycling.[29] The WS2/C nanocomposite exhibits
excellent cycling behavior with discharge capacity of 829.4 mAhg-1
at 0.3 Ag-1 after 140 cycles as it possesses suitable lamellar
space for Li ions intercalation and maintains a high electrical
conductivity of the overall electrode as confirmed by the
electrochemical impedance results (Figure 3D). Figure 3B
shows the third charge-discharge curves at a constant current
density of 0.3 A g -1, the WS2/C had a lower charge plateau and
higher discharge plateau, which indicated a low kinetic
polarization responsible for its higher reversible capacity. Figure
3C shows the superior rate capability of the WS2/C nanocomposite
compared with the bare WS2. A capacity of ~326.8 mAhg-1 can still
be retained even at a current density of 8.0 Ag-1, which is
significantly higher than that of bare WS2. Moreover, the capacity
can recover the original values when the current densities are
switched back to 0.15 Ag-1 from a high current density (8.0 Ag-1),
demonstrating good capacity retention after high current density
cycling. The corresponding charge and discharge profiles for
various current densities (0.15 Ag-1 to 8.0 Ag-1) are displayed in
Figure S3 as well. We consider that the stable cycle ability and
rate performance of the WS2/C nanocomposite are attributed to the
following aspects. Firstly, few-layered WS2 allows for very
efficient storage, not only by minimizing transport problems for
both electrons and lithium ions, but also by reversibly “combining”
interfacial storage, insertion and conversion.[32] Secondly, in the
thousand layer cake architecture, the carbon significantly expands
the inter-space between the WS2 nanosheets, which results in plenty
of channels for the electrolyte diffusion.[33] Thirdly, the
interbedded carbon can effectively reduce the restacking of WS2
sheets and utilize the surface of WS2 as much as possible.
Fourthly, carbon itself is a very good electronic conductor. Thus,
the interlayer carbon can increase the conductivity of the
electrode and provide rapid charge transfer during the
electrochemical reaction. The electrodes of bare WS2 and the WS2/C
nanocomposite were also analyzed by electrochemical impedance
spectroscopy (Figure 3D). The Nyquist plots for the two types of
electrodes display both a depressed semicircle in the high
frequency region and an inclined straight line in the low frequency
region. The size of the semicircle, which measures the resistance
of an electrode to the charge transfer reaction, was smaller for
the WS2/C electrode. The WS2/C nanocomposite showed low
Figure 3. Cycling performances of bare WS2 and WS2/C
nanocomposite (A); The third charge/discharge curves (B) of bare
WS2, WS2/C; Cycling performance of the WS2/C and bare WS2
nanocomposite at different current densities(C); Nyquist plots of
bare WS2 and WS2/C over the frequency range from 100 kHz to 0.01 Hz
at open potential (the inset is the equivalent circuit for Nyquist
plots) (D).
10.1002/celc.201700414ChemElectroChem
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ARTICLE
charge transfer resistance compared to bare WS2 due to the fact
that the intercalated carbon not only decreased the charge
diffusion distance but also accelerated the charge transfer.
Conclusions
A multi-layer-cake WS2/C nanocomposite consisting of alternative
layer-by-layer inter-overlapped few-layered WS2 and carbon has been
synthesized by the intercalation-transformation method. It exhibits
remarkably enhanced electrochemical performance, including a large
specific capacity and excellent capacity retention. The reasons are
that in the unique “regular” and “alternate” structure, the
interlayer carbon can inhibit the restacking of WS2 layers, buffer
the volume expansion, enhance the electrical conductivity of the
electrode, and provide rapid charge transfer during the
electrochemical reaction. Furthermore, the multi-layer-cake WS2/C
nanocomposite exhibits high lithium storage capacity due to its
optimized conductivity and inter-planar distance. This novel
structure designed herein will provide a new and facile route to
prepare the advanced anodes for next-generation performance
LIBs.
Experimental Section
Synthesis. Scheme 1 presents the preparation of WO3-x/C and
WS2/C nanocomposite. The WO3-x/C nanocomposite was prepared as
follows: 7.5 g of Bi2O3 and 7.5 g of WO3 were combined and ground
to a fine powder with a mortar and pestle. The powder was then
annealed in air at 800 oC for 48 h. The resulting solid (Bi2W2O9 )
was again ground to a fine powder and 12 g was added in 300 mL of 6
M HCl at room temperature for seven days under stirring to get
H2W2O7. The solid was centrifuged at 5000 rpm for ten minutes and
the acidic supernatant was discarded. The samples were dried in an
oven at 60 oC for 12 h. And then, 2 g of H2W2O7, 7 g of C12H27N and
100 mL heptane were added to a 250 mL four neck flask stirring for
three days. The precipitates in the solution were filtered, washed
sequentially with heptane and ethanol, and then dried at 60 oC.
Finally, the above products were placed inside the tube furnace
calcining at 600 oC for 2 h in N2 atmosphere.
Under N2 atmosphere, reacting WO3-x/C nanocomposite (0.3 g) with
thiourea (4.8 g) at 700 oC for 2 h to produce Multi-layer-Cake
WS2/C nanocomposite after they were ground to a fine powder. This
black product obtained was cooled down naturally under N2 and used
directly for further analysis. Materials characterization. X-ray
powder diffraction (XRD) measurements were obtained on Bruker D8
Advance diffractometer operated at 40 kV and 40 mA in the range
2-70° with Cu-Kα radiation (λ=0.15406 nm). The morphologies of the
products were observed by means of a field emission scanning
electron microscope (FE-SEM) (Hitachi SU 8010) operated at an
acceleration voltage of 15 kV. High-resolution transmission
electron microscope (HRTEM) was performed on a JEM-2100 microscope
(JEOL). Raman spectra were recorded on the DXR Raman microscope
(Thermo Scientific) with a 532 nm excitation laser (setting 10 s
exposure time, 20 accumulations). X ray photoelectron spectroscopic
(XPS) measurement of the composites was obtained from an ESCALAB
250 spectroscopy (Thermo Fisher Scientific) with an Al Kα (1486.6
eV) X-ray source operated at 15 kV and 150 mW.
Electrochemical measurements. The working electrodes were made
by coating a paste of the as-synthesized materials, Super P, and
binder (polyvinylidene fluoride, PVDF) in a weight ratio of
80:10:10 on a copper-foil collector. After pressing and punching,
the electrodes of 12 mm diameter were acquired. The negative
electrodes were dried at 110 °C for 12 h in a vacuum oven and the
mass loading of the as-synthesized material was about 2.6 mgcm-2.
Li metal foil was used as the counter and reference electrodes.
Coin-type cells (CR 2032) were assembled in an argon filled glove
box with an electrolyte of 1 molL–1 LiPF6 in EC-EMC-DMC (1:1:1
volume ratio) solution and a separator of Celgard 2400. The cells
were assembled in an Ar-filled glove-box followed by an overnight
aging treatment before the test. The electrochemical data were
collected by a LAND CT2001A test system within the potential range
of 0.01-3.0 V (vs. Li/Li+). Cycling voltammetry (CV) was measured
at a scan rate of 0.3 mVs-1 using a CHI 660E electrochemical
workstation (Shanghai CHI Instruments). For electrochemical
impedance spectroscopy (EIS), a sine wave with amplitude of 5.0 mV
over the frequency range of 100 kHz to 0.01 Hz was applied.
Acknowledgements
This work was supported by the National Natural Science
Foundation of China (21671092), Program for Liaoning Excellent
Talents in University (LNET LR2015036), and the Opening Funds of
State Key Lab of Chemical Resource Engineering.
Keywords: Anode • Few Layer • Lithium-ion Batteries •
Multi-layer-Cake • WS2
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ARTICLE
A “regular” and “alternate” WS2/C nanocomposite called
“multi-layer-cake” was successfully synthesized, it demonstrated a
high capacity of 829.4 mAhg-1 at 0.3 Ag-1 after 140 cycles, and
could still deliver a stable capacity of about 326.8 mAhg-1 at a
current density of 8.0 Ag-1.
Jiaming Zou, Cheng Liu, Zhanxu Yang*, Chengyuan Qi, Xiaorong
Wang*, Qingdong Qiao, Xian Wu and Tieqiang Ren
Page No. – Page No.
Multi-layer-Cake WS2/C Nanocomposite as A High-Performance Anode
Material for Lithium-Ion Batteries: “regular” and “alternate”
10.1002/celc.201700414ChemElectroChem
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