Chemical Prelithiation of Negative Electrodes in Ambient-Air for

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Chemical Prelithiation of Negative Electrodes in Ambient-Air for Advanced Lithium-ion Batteries Gongwei Wang, Feifei Li, Dan Liu, Dong Zheng, Yang Luo, Deyu Qu, Tianyao Ding, and Deyang Qu ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.8b19416 • Publication Date (Web): 19 Feb 2019 Downloaded from http://pubs.acs.org on February 19, 2019

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ACS Applied Materials & Interfaces

Chemical Prelithiation of Negative Electrodes in Ambient-Air for Advanced Lithium-ion Batteries Gongwei Wanga, Feifei Lia, Dan Liub, Dong Zhenga, Yang Luoa, Deyu Qub, Tianyao Dinga, and Deyang Qua*

a

Department of Mechanical Engineering, University of Wisconsin Milwaukee, Milwaukee, WI 53211, United States. b

Department of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, 122 Luoshi Road, Wuhan 430070, P. R. China *Corresponding author. E-mail: [email protected]

Abstract This study reports an ambient-air tolerant approach for negative electrode prelithiation by using 1 M lithium-biphenyl (Li-Bp) / tetrahydrofuran (THF) solution as the prelithiation reagent. Key to this strategy are the relatively stable nature of 1 M Li-Bp/THF in ambient air and the unique electrochemical behavior of Bp in ether and carbonate solvents. With its low redox potential of 0.41 V vs. Li/Li+, Li-Bp can prelithiate various active materials with high efficacy. The successful prelithiation of a phosphrous / carbon composite electrode and the notable improvement in its initial coulombic efficiency (CE) demonstrates the practicality of this strategy.

KEYWORDS: lithium-ion batteries, negative electrode, prelithiation, ambient air, biphenyl

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Address: Department of Chemistry, Wuhan University, Wuhan, China 430072 ACS Paragon Plus Environment

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Lithium-ion batteries (LIBs) with high energy densities and good cycling performance are highly desired for the widespread usage of portable electronic devices and the emerging market of electric vehicles.1-2 The conventional LIBs are primarily based on graphite negative electrodes (NE) and lithium metal oxide (LMO) positive electrodes (PE). Their energy densities are typically 150 ~ 200 Wh kg-1, which struggles to fulfil the increasing demand.3 Considerable efforts have been devoted to developing high-capacity NE and PE materials for next-generation LIBs with improved energy densities.4-5 Various lithium-free materials (e.g. P, Sn, Si, metal oxides) have been considered as promising alternative NEs, which could deliver high capacities after hundreds and even thousands of charge-discharge cycles using a lithium-excess half-cell configuration.6 However, most of them suffer from low initial coulombic efficiencies (CE, 50% ~ 85%) because of the solid-electrolyte interphase (SEI) formation and irreversible parasitic reactions (such as Li2O formation for some metal oxides),7-8 especially when nanostructured designs are utilized for improving the power capability and cycling performance.9 A large amount of active lithium ions from PE is consumed and permanently trapped in NE at the first charge, causing an appreciable capacity loss of full cell.10 Moreover, the optional lithium-rich PEs are usually limited to LMO with low specific capacities (< 200 mAh g-1), which hinders further improvement in energy densities of full cells. Accordingly, the prelithiation of NE is regarded as an appealing approach to overcome these shortcomings.11-12 It could not only compensate for the initial active lithium loss, but also enable the pairing with high-capacity lithium-free PEs (e.g. sulfur, oxygen, V2O5) and thus configure novel LIBs with high energy densities.13-14 Two strategies have been attempted to prepare the prelithiated NEs. A direct approach is to in-situ introduce a precise amount of lithium metal (e.g. ultra-thin lithium metal foil15, stabilized

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lithium metal powder16-17) into NE during battery assembly,18 which remains a technically challenging operation.12 An alternative approach is to ex-situ prepare the prelithiated NEs prior to battery assembly by using electrochemical or chemical prelithiation techniques. Electrochemical prelithiation, which is based on either galvanostatic reduction of NE with a lithium-excess half-cell configuration19-21 or shorting with lithium metal in the presence of electrolyte22-24, is the most utilized method in academic studies. It allows for prelithiation of all kinds of NE materials, but the whole process is complex and time-consuming, making it unsuitable for large-scale applications. Chemical prelithiation, on the other hand, depends on a direct reaction of NE active materials with reductive prelithiation reagents (e.g. molten lithium metal13,

25-27,

lithium-organic complex solutions28-29), which is simple and facile with less

procedures. However, the challenge is that both prelithiation reagents and prelithiated NE materials can hardly survive in ambient air due to their low potenitals and high chemical reactivity towards air (oxygen, nitrogen) or moisture. Inert atmosphere is therefore needed for the previously reported chemical prelithiations. Here we report an ambient-air tolerant method for NE prelithiation by using 1 M lithiumbiphenyl (Li-Bp) / tetrahydrofuran (THF) solution as the prelithiation reagent. Biphenyl (Bp) was chosen because of its unique chemical / electrochemical behavior in different solvents. In ether solvents (e.g. dimethoxyethane (DME), THF), it can react with lithium metal and form a strong reducing reagent of Li-Bp. Moreover, the resulting Li-Bp solution is relatively stable towards air and moisture, which is critical to the prelithiation in ambient air. Bp can be readily dissolved into both ether-based electrolytes (e.g. 1 M lithium hexafluorophosphate (LiPF6) in DME) and carbonate-based electrolytes (e.g. 1 M LiPF6 in ethylene carbonate (EC)/diethyl carbonate (DEC) (1:1 v/v)) (Figure 1 inset, a and b). However,

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only the former turned to dark blue after further adding a piece of lithium metal (Figure 1 inset, a′ and b′). Cyclic voltammetry (CV) was carried out in the two solutions. A pair of quasi-reversible redox peaks were observed for Bp / Li-Bp conversion in the ether-based electrolyte, whereas no such peaks were found in the carbonate-based electrolyte electrolyte in the potential range of 0 ~ 4.5 V vs. Li/Li+ (Figure 1). These results clearly demonstrate that Bp is redox-active in ether solvent but redox-inert in carbonate solvent. In addition, the redox potential for Bp / Li-Bp conversion is as low as 0.41 V vs. Li/Li+, which is applicable to prelithiate most of the reported active materials for LIBs, such as Sn, P, metal oxides and other materials listed in the shaded area of Figure 1 (upper).

Figure 1. The capacities and potentials of various active materials for LIBs (upper). These active materials listed in the shaded area are all applicable to be prelithiated by Li-Bp. Cyclic voltammograms in ether-based (a’) and carbonate-based (b’) electrolytes at a scan rate of 20 mV/s (lower): (a) 0.1 M Bp and 1 M LiPF6 in DME, (b) 0.1 M Bp and 1 M LiPF6 in EC/DEC (1:1 v/v). (a’) and (b’) are the resulting solutions after adding a piece of lithium metal.

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To verify the effectiveness of this prelithiation reagent, red P and Sn powder samples were chosen as starting materials and separately added into 1 M Li-Bp/THF. After overnight reaction, the dark-red P turned into an orange powder (denoted as Li-P), and the light-gray Sn turned into a dim-gray powder (denoted as Li-Sn, Figure 2a). ICP analysis (Figure S1) shows that the Li/P and Li/Sn atomic ratios are 3.5/1 and 3.9/1, respectively (Figure 2b), which are approximately the stoichiometric ratios of their fully lithiated products (Li3P and Li22Sn5). X-ray diffraction (XRD) patterns of Li-P and Li-Sn are also in good accordance with the standard Li3P (PDF # 040525) and Li22Sn5 (PDF # 18-0753) (Figure 2c), further confirming a fully prelithiation efficacy. Scanning electron microscopy (SEM) was utilized to examine the morphology of each sample (Figure 2d). As expected, the mophology changed significantly after the prelithiation. Red P and Li-P exhibit a clearly different aggregation state. The originally smooth surface for Sn particles obviously becomes rough after prelithiation. Some Li-Sn particles even crack and crumble due to a large volume expansion.

Figure 2. Characterization of red P and Sn powder samples before and after prelithiation. (a) Digital images. (b) Chemical compositions. (c) XRD patterns. (d) SEM images.

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Prelithiation in ambient air is desirable but very challenging owing to the high reactivity of prelithiated NE products and prelithiation reagents. When exposed to ambient air, Li-P powder rapidly changes from orange to white and Li-Sn powder rapidly changes from dim-gray to lightgray. XRD confirms the complete deterioration of Li-P and Li-Sn after 0.5 h of exposure (Figure S2). Similarly, a low concentration of 10 mM Li-Bp/THF solution also quickly turns from darkblue to colorless and transparent after amibient-air exposure. However, an exciting finding was that the concentrated (1 M) Li-Bp/THF solution can be stored in ambient air for more than two weeks and can even withstand repeated stirring (Figure 3a and b). With a close look at the 1 M Li-Bp/THF solution in ambient air, a visible protective film can be observed on the liquid surface (Figure S3), which may contribute to prevent further reaction of Li-Bp with air and moisture. Besides, the reaction of 1 M Li-Bp/THF with water is more milder than that of lithium metal (Figure 3b), suggesting that Li-Bp/THF is more stable and safe. Such characteristics make the concentrated (1 M) Li-Bp/THF a practicable prelithiation reagent that can be used in ambient air. An ambient-air tolerant procedure for NE prelithiation is thus proposed and schematically illustrated in Figure 3c. The NE active material is firstly coated on a current collector and then dipped into the 1 M Li-Bp/THF solution. After prelithation, the residual Li-Bp/THF on NE acts as a robust protecting layer, avoiding the exposure of high-reactive prelithiated NE active material to ambient air. During battery assembly, the residual Li-Bp on NE can be consumed by carbonate-based electrolyte and converted to soluble Bp. Given that Bp is redox-inert in carbonate-based electrolyte (Figure 1), the soluble Bp will not affect battery performance in the following charge / discharge cycles.

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Figure 3. (a) Digital images of the 1 M Li-Bp/THF exposed to ambient air for different durations. (b) Snapshots of the 1 M Li-Bp/THF under stirring in ambient air or after adding water. (c) Schematic illustration of the prelithiation procedure in ambient air. To demonstrate the applicability of this procedure, red P was prelithiated as a typical example. The electrochemical performance was evaluated using a half-cell configuration with a lithium foil as counter electrode and a carbonate-based electrolyte (1 M LiPF6 in EC/DEC (1:1 v/v) with 10 wt % FEC and 2 wt % VC). Red P was first preloaded into a homemade mesoporous carbon material (P/C) via a vaporization / adsorption strategy (Figure S4a),30 and then coated on a carbon-coated copper foil to form pristine P/C electrode (Figure S4b). As shown in Figure 4a, the pristine P/C electrode exhibits an initial open-circuit voltage (OCV) of ~ 2.9 V, an initial lithiation capacity of 1773 mAh g-1(P/C), and subsequent reversible capacities of around 1200 mAh g-1(P/C). The initial CE (1st delithiation / 1st lithiation capacities) is only 74% due to the formation of SEI layer (Figure 4f). A control prelithiated P/C electrode was prepared in an argon-filled glovebox by dipping the pristine P/C electrode into 1 M Li-Bp/THF for 10 min treatment, washing with THF and then vaccum-drying (Figure S4c). It exhibits an initial OCV of ~ 0.8 V. As the prelithiated P/C electrode is in Li-rich state, it begins Li-extraction with an initial Current


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delithiation capacity of 840 mAh g-1(P/C) and similarly subsequent reversible capacities of around 1200 mAh g-1(P/C) (Figure 4b). The degree of prelithiation (DOPL), which is defined as the ratio of the 1st to 2nd delithiation capacities, is ~ 80%. The rest of ~ 20% unprelithiated reversible capacity can be attributed to the contribution of carbon materials (mesoporous carbon and Super C65) in the electrode (Figure S5). Since the electrochemcial lithiation potential of carbon is lower than the redox potential of Bp/Li-Bp conversion (Figure 1), these carbon materials cannot be prelithiated by Li-Bp/THF but can undergo repeated lithiation / delithiation under cycling conditions. Notably, the control prelithiated P/C electrode exhibits a much higher initial CE of ~ 94% (2nd delithiation / 1st lithiation capacities) relative to that of the pristine P/C electrode (Figure 4f), indicating the prelithiation is sufficient to compensate the initial irreversible capacity. A series of P/C electrodes were also treated and assembled according to the proposed procedure as shown in Figure 3c, by using 1 M Li-Bp/THF with different exposure durations (Figure 3a) as the prelithiation reagents. Figure 4c and 4d show the first two cycle voltage profiles of these prelithiated P/C electrodes, which exhibit a same plateaus as that of the control prelithiated P/C electrode. All these prelithiated P/C electrodes, no matter prepared in ambient air or inside glovebox, exhibit similar initial delithiation capacity, subsequent reversible capacity, initial CE as well as DOPL (Figure 4e). These results illustrate that the proposed prelithiation procedure can be performed in ambient air with no ill effects. Moreover, the cycling performances of the pristine and prelithiated P/C are almost accordant with each other except for the initial few cycles (Figure 4f), suggesting that this chemical prelithiation would not damage the electrode structure and affect the cycling stability.

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Figure 4. Voltage profiles of the pristine P/C electrode (a) and the control prelithiated P/C electrode (b). The red curves represent the initial segments. The first (c) and second (d) cycle voltage profiles of the prelithiated P/C electrodes prepared by using the 1 M Li-Bp/THF with different exposure duration as shown in Figure 3a. The capacities, initial CE and DOPL of the pristine P/C (dark-gray box), control prelithiated P/C (light-gray box) and prelithiated P/C prepared in ambient air (white box) (e). Cycling performance of the pristine and prelithiated P/C electrodes at 1 A g-1 (f). The pristine P/C began with lithiation and the prilithiated P/C began with delithiation.

In conclusion, this work demonstrates an ambient-air tolerant method for NE prelithiation for the first time by using 1 M Li-Bp/THF as the prelithiation reagent. The main advantages for this prelithiaiton reagent are its strong reducing ability (0.41 V vs. Li/Li+), ambient-air stable nature and unique redox property. By utilizing these characteristics, a P/C electrode is succusfully prelithiated in ambient air with no ill effect. The initial CE of P/C is significantly increased from 74% to 94% after the prelithiation treatment. We expect this ambient-air tolerant

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chemical prelithiation approach could be further implemented into a commercial manufactural process using a scalable roll-to-roll design (Figure S6).

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