Multi‐layer‐Cake WS2/C Nanocomposite as A High‐Performance...

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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

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

This article is protected by copyright. All rights reserved.

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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).



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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).



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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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Entry for the Table of Contents (Please choose one layout) Layout 1:

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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”



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