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High Rate Lithium Ion Battery with Niobium Tungsten Oxide Anode

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High Rate Lithium Ion Battery with Niobium Tungsten Oxide Anode Journal of the Electrochemical Society OPEN ACCESS High Rate Lithium Ion Battery with Niobium Tungsten Oxide Anode To cite this article: Yumi Kim et al 2021 J. Electrochem. Soc. 168 010525 View the article online for updates and enhancements. This content was downloaded from IP address 131.111.184.102 on 25/01/2021 at 10:01 Journal of The Electrochemical Society, 2021 168 010525 High Rate Lithium Ion Battery with Niobium Tungsten Oxide Anode Yumi Kim,1 Quentin Jacquet,1 Kent J. Griffith,2,* Jeongjae Lee,1 Sunita Dey,1 Bernardine L. D. Rinkel,1 and Clare P. Grey1,**,z 1Department of Chemistry, University of Cambridge, Cambridge, CB2 1EW, United Kingdom 2Departments of Chemistry and Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208, United States of America Highly stable lithium-ion battery cycling of niobium tungsten oxide (Nb16W5O55, NWO) is demonstrated in full cells with cathode materials LiNi0.6Mn0.2Co0.2O2 (NMC-622) and LiFePO4 (LFP). The cells show high rate performance and long-term stability under 5 C and 10 C cycling rates with a conventional carbonate electrolyte without any additives. The degradation of the cell performance is mainly attributed to the increased charge transfer resistance at the NMC side, consistent with the ex situ XRD and XPS analysis demonstrating the structural stability of NWO during cycling together with minimal electrolyte decomposition. Finally, we demonstrate the temperature-dependent performance of this full cell at 10, 25 and 60 °C and confirm, using operando XRD, that the structural change of the NWO material during lithiation/de-lithiation at 60 °C is very similar to its behaviour at 25 °C, reversible and with a low volume change. With the merits of high rate performance and long cycle life, the combination of NWO and a commercial cathode represents a promising, safe battery for fast charge/discharge applications. © 2021 The Author(s). Published on behalf of The Electrochemical Society by IOP Publishing Limited. This is an open access article distributed under the terms of the Creative Commons Attribution Non-Commercial No Derivatives 4.0 License (CC BY- NC-ND, http://creativecommons.org/licenses/by-nc-nd/4.0/), which permits non-commercial reuse, distribution, and reproduction in any medium, provided the original work is not changed in any way and is properly cited. For permission for commercial reuse, please email: [email protected]. [DOI: 10.1149/1945-7111/abd919] Manuscript submitted October 17, 2020; revised manuscript received December 14, 2020. Published January 15, 2021. This was paper 381 presented at the Atlanta, Georgia, Meeting of the Society, October 13–17, 2019. Supplementary material for this article is available online The growing global energy demand, together with the quest for present the full cell performance of more practical electrodes of NWO clean and renewable sources of energy, drives research into Li-ion in combination with two commercial cathode materials for high rate Li- batteries with high energy density and high rate performance.1–3 In ion batteries: LFP and NMC. many portable electronics and electric vehicles, fast charging and high power density are two of the key requirements.4–6 In this Experimental regard, LiFePO (LFP) has been extensively used as a stable cathode 4 Electrode preparation.—NWO powder was synthesized as pre- material allowing for high currents in a full cell; it however exhibits viously reported in the literature.17 NMC-622 (Targray) and a a lower working voltage (vs Li) and practical capacity than Ni-rich – commercial source of carbon-coated LFP with 0.5 um particle size cathodes such as LiNi Mn Co O (NMC-622).7 10 On the anode 0.6 0.2 0.2 2 were used as cathodes (Fig. S1 available online at stacks.iop.org/ side, graphite is used commercially due to its low cost, wide JES/168/010525/mmedia). The XRD analysis of all active materials availability and low delithiation voltage (vs Li); however, it has confirm that they are phase pure as shown in Fig. S2. High loadings electrolyte stability issues at low voltages resulting in the formation electrodes were prepared mixing Super P carbon (TIMCAL) and of a passivating layer.11,12 This surface–electrolyte interphase (SEI) polyvinylidene fluoride (PVdF; Kynar) dispersed in N-methyl-2- layer is known to be an essential component for graphite anodes; + pyrrolidone. All slurries were composed of 90% active material, 5% however, it consumes Li during formation, lowering the initial super P and 5% PVdF binder, and the mixing was conducted with a coulombic efficiency of the cell. Moreover, graphite has the serious Thinky Mixer 250. The NMC and LFP electrodes were dried in an issue of Li plating at high rates and/or low temperatures leading to oven at 80 °C for 2 h in a dry room, and the NWO electrodes were the formation of dendrites negatively impacting the cycle life, rate dried in an oven at 60 °C overnight under ambient atmosphere. All capability and safety of the cell. Li Ti O (LTO), having a higher 4 5 12 electrodes were calendared at room temperature and the resulting working voltage (1.55 V vs Li) hence reduced SEI formation and electrode porosities were in the range of 35%–45%. The electrodes dendrite growth, is commonly suggested as a promising candidate − − loadings were 8.0–8.3 mg cm 2 (NMC), 8.4–8.7 mg cm 2 (LFP) and for high power applications. However, it needs to be nanosized to − 8.8–9.4 mg cm 2 (NWO) with 1 cm2 electrode size. Low loading access high rates, leading to a low volumetric energy density of electrodes were prepared in a similar fashion but with a different LTO-based cells, and problematic evolution of H2 and CO2 gases – composition namely having 10% Li250 carbon (Denka), 10% PVdF upon cycling.13 16 Clearly, novel anode materials with high rate (Kynar) dispersed in N-methyl-2-pyrrolidone, and 80% of active performance are needed for safe Li-ion cells with high energy and − material. The resulting active material loading were 4.0 mg cm 2 power densities. − − for NMC, 3.8 mg cm 2 for LFP and 4.4 mg cm 2 for NWO. Recently, our group has reported that Nb16W5O55 (NWO) which crystallizes in a ReO block-type structure, featuring 2D tunnels 3 Electrochemical characterization.—All electrochemical mea- suitable for Li conduction shows promising performance for high- surements were evaluated with 2032-type stainless steel coin cells. rate lithium-ion energy storage even with micro-sized particles.17 Many Prepared cathode and anode electrodes were dried at 100 °C for 3 h other studies of compounds having different stoichiometries but similar under vacuum, then transferred into an argon-filled glove box structural motifs have also shown excellent high rate performance in (MBraun) without exposure to air. Full cells were assembled in half-cell configurations and for electrodes having a high conductive − – the glove box with LP30 electrolyte (Sigma-Aldrich, battery grade), carbon content (>10%) and low loading (<2mgcm 2).18 21 Here we which is composed of 1.0 M lithium hexafluorophosphate (LiPF6)in ethylene carbonate (EC): dimethyl carbonate (DMC) (1:1 v/v). A polyethylene separator (Toray) was used after drying at 40 °C for 2 h *Electrochemical Society Member. fi fi **Electrochemical Society Fellow. under vacuum. For electrolyte analyses, glass ber lter paper zE-mail: [email protected] (Whatman, GE) was used as the separator. The filter was also dried Journal of The Electrochemical Society, 2021 168 010525 Figure 1. (a) Cell voltage profiles of the high loading NWO/LFP full cell at 0.2 C, 1 C, 2 C, 5 C, 10 C and 20 C, (b) Rate performance of the high loading and low loading NWO/LFP full cells and (c) Discharge capacity and coulombic efficiency (C.E.) plots from long-term cycling of the high loading NWO/LFP cell operated at 25 °C at 5 C and 10 C (d) XRD patterns of ex situ NWO electrodes cycled in a LFP/NWO full cell at 5 C for 200 and 500 cycles and stopped after charge (lithiated NWO) and discharge (delithiated NWO). at 150 °C under vacuum in a drying oven (Buchi). For half cells, Li of pristine and cycled electrodes were obtained in Bragg–Brentano metal chip (250 μm, PI-KEM), LP30 electrolyte and glass fiber filter geometry (Empyrean, Panalytical) at ambient temperature with a were used as the counter electrode, electrolyte and separator, respec- Cu-Kα source. The operando XRD measurement at high tempera- tively. Galvanostatic electrochemical tests were conducted at various ture was performed in the same instrument using a home-made cell current densities by using a galvanostat/potentiostat (BioLogic) in a with a Be window and heating bars. The scan time was 10 min. temperature-controlled oven at 10, 25 and 60 °C. All cells had a Lattice parameters, phase and purity of the material were determined negative-to-positive capacity ratio of 1.1–1.2, which is calculated by Rietveld refinement (or Lebail on the NWO material due to its based on the practical capacities of the active materials, i.e. 171.3 mAh large unit cell) using the FullProf software.22 X-ray photoelectron g−1 for NWO, 175 mAh g−1 for NMC and 165 mAh g−1 for LFP. Full spectroscopy (XPS) was carried out with a Thermo Fisher Scientific cell capacities in this study are calculated by active material mass of instrument with a monochromated Al-Kα X-ray source (hν of the cathode. In full cell tests, charge was performed under constant 1468.7 eV).
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