Suppressed the High-Voltage Phase Transition of P2-Type Oxide

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Suppressed the High Voltage Phase Transition of P2-Type Oxide Cathode for High-Performance Sodium-Ion Batteries Kezhu Jiang, Xueping Zhang, Haoyu Li, Xiaoyu Zhang, Ping He, Shaohua Guo, and Haoshen Zhou ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.9b03326 • Publication Date (Web): 02 Apr 2019 Downloaded from http://pubs.acs.org on April 3, 2019

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ACS Applied Materials & Interfaces

Suppressed the High Voltage Phase Transition of P2-Type Oxide Cathode for High-Performance Sodium-Ion Batteries Kezhu Jiang,† Xueping Zhang, † Haoyu Li, † Xiaoyu Zhang, † Ping He, † Shaohua Guo,†* and Haoshen Zhou†§* †Center

of Energy Storage Materials & Technology, College of Engineering and Applied

Sciences, National Laboratory of Solid State Microstructures, Collaborative Innovation Center of Advanced Microstructures, Jiangsu Key Laboratory of Artificial Functional Materials, Nanjing University, Nanjing 210093, China §Energy

Technology Research Institute, National Institute of Advanced Industrial Science and

Technology (AIST), Umezono 1-1-1, Tsukuba, 305-8568, Japan. Corresponding Author *[email protected] (S. Guo); *[email protected] (H. Zhou)

Keywords: sodium-ion batteries, P2-type, Mn-based layered oxide, high voltage phase transition, Ru substitution

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ABSTRACT

Sodium-ion batteries (SIBs), using the resourceful Mn-based materials as cathodes, have been considered as the promising candidates for large-scale energy storage applications. However, the representative P2-type Mn-based layered oxide cathode usually suffers from limited specific capacity and poor cycle life in Na-ion intercalation and deintercalation processes, due to the unavoidable phase transition at high voltage. Herein, we developed a Ru substituted P2-Na0.6MnO2 (NaMR) as a promising sodium host with high reversible capacity and cycle life. The multiplecharacterization investigations reveal the Ru substitution could improve the electronic and ionic conduction, and particularly suppress phase transition of P2-OP4 resulting the extension of singlephase reaction region. Ru substitution not only enhances the capacity specific capacity (209.3 mAh g-1), but also improves the rate capability (~100 mAh g-1 at 50 C) and cycling stability. This work may open a new avenue to designing and fabricating SIBs by using Mn-based cathodes with high capacity and stability.


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1. Introduction With the advantages of abundant resources and low cost, sodium-ion batteries (SIBs) have been considered as one of the greatest potential energy storage devices for smart power grids and large-scale energy storage system.[1-4] However, the shortage of suitable cathode materials is an important factor to hinder SIBs practical application.[5-6] Therefore, the development of novel cathode materials are crucial for commercialization of SIBs.[7-8] Up to now, several types of materials such as sodium transition-metal layered oxides, polyanionic frameworks, hexacyanoferrates have been demonstrated as cathodes for SIBs.[9-10] Compared with other cathode candidates, the sodium transition-metal layered oxides are regarded as the promising cathode in SIBs because of their facile synthesis, environmental friendly and high reversible capacity.[11-12] Sodium transition-metal layered oxides NaXMO2 (M = transition metal, e.g., Ti, Cr, Mn, Fe, Co, Ni, Cu) can be generally fell into two families: P2-type and O3-type structures, which are on the basis of the oxygen layer packing and the occupied Na sites in the layered structure.[13-17] In contrast to O3-type materials, P2-type sodium transition-metal layered oxides exhibits more open framework structure and direct prismatic paths for sodium-ion migration, which makes the P2type material as one of the most appealing cathodes for SIBs with a large specific capacity, low polarization and superior rate performance.[18-20] Particularly, the P2-type Mn-based materials attracts a lot of attention due to the resourceful, low cost and eco-friendly nature of Mn element .[21-24] In 1985 Delmas and his coworkers first reported P2-type Mn rich material (P2-type Na0.70MnO2.25) as a promising cathode for SIBs.[25] However, the structural and electrochemical stability of P2-type NaXMnO2 will deteriorate rapidly during the electrochemical process.[26-27] Especially, the P2-O2/OP4 phase transition also often occurs by a transition metal layers shift when charging to high voltage, inescapably attended with the large volume change leading to the


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poor cycle life.[28-30] For example, Aranda and his coworkers reported that the P2-type Na0.6MnO2 could deliver a high specific capacity of ~150 mAh g-1 at the first cycle, but the capacity rapidly decayed after following several cycles, because of the frequent phase transitions with continuous strains and distortions resulting the host structure to gradually collapse during the Na-ion insertion and extraction process.[31] Recently, an interesting strategy to address this difficult issues is a small substitution of Mn element with other metal elements (such as: Mg, Fe, Co, Ni, Cu, Al etc.), which could effectively enhance the structural and electrochemical stability of this P2-type material.[32-39] For instance, a small substitution of Mn with Mg in P2-type Na0.67MnO2 could smooth potential profiles, reduce polarization and enhance cycling stability (96% capacity retention after 25 cycles). Further investigation indicated that Mg dopant could reduce the Jahn-Teller lattice distortion and relieve the P2-OP4 phase transition during P2-Na0.67MnO2.[40-41] Several substituted Mn rich materials show

improvements

of

electrochemical

performance,

however,

the

comprehensive

electrochemical performance of the reported materials is still limited when applied to full cells coupled with other anode materials, because there is still no effective strategy to avoid the complex phase transitions occurred at high voltage.[21] Therefore, the development of Mn-based cathodes with large capacity and long cycle life is still a severe challenge. Herein we report a Ru substituting P2-Na0.6MnO2 material (NaMR) with uniform lamellar morphology and typical P2-typed structure by a simple solid-state method. We found that the NaMR material exhibited the improved specific capacity, rate capability and cycle life relative to the unsubstituting P2-Na0.6MnO2 (NaM) because the introduction of Ru not only could improve the electronic and ionic conduction, but also could suppresses phase transition at high voltage and smooth electrochemical curves. Therefore, the NaMR material could show a high specific capacity


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(209.3 mAh g-1), high rate capability and superior cycling stability (75.4% capacity retention over 200 cycles), during the charge and discharge. The present work opens a new way for enhancing the specific capacity, rate capability and cycling performance of layer oxides materials through the reasonable element substituting effect. 2. Results and discussion The NaMR and NaM power samples were synthesized via a simple solid-state method. The phase structure of the initial NaM and NaMR compounds are initially characterized by power Xray diffraction (XRD). The XRD patterns of NaM and NaMR compounds reveal that all the diffraction peaks could be ascribable to a hexagonal pattern associated with P63/mmc space group without any impurities, suggesting the pure P2 phase structures for both substituting and unsubstituting materials and a uniform incorporation of Ru-ion into the crystal lattice of P2-type NaM (Figure 1a and Figure S1). All the diffraction peaks show a sharp feature, indicating their high crystallinity. The XRD Rietveld refinements for lattice parameters of NaMR and those of NaM are shown in Table S1&S2. The Figure 1b shows the representative crystal model of the P2type NaMR. The size and morphology of the initial NaMR material is characterized by scanning electron microscopy (SEM) and transmission electron microscope (TEM). The representative SEM images reveal that the uniform particles with lamellar stacking structure are the dominant products. The particle size of NaMR is about 0.2-1 μm (Figure 1c&1d and Figure S2). The detailed crystal structure of NaMR is further visualized by high-resolution transmission electron microscopy (HRTEM). The interplanar distance is measured as 0.553 nm, assigned to the (002) plane of the P2-NaMR (Figure 1e). The high-angle annular dark-field scanning transmission electron microscopy energy dispersive spectroscopy (HAADF-STEM-EDS) elementary mapping images are shown in Figure 1f. It is clear that the uniform distribution of Na, Mn, Ru and O


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elements are observed in the whole selected-area of particle, which further demonstates that Ru element is successfully incorporating into P2-type NaMn compound matrix. The NaMR sample was mixed with binder and conductor agent for further electrochemical properties of Na half-cells recorded in a propylene carbonate solution containing 1 M NaClO4 and 5 vol% fluoroethylene carbonate between 1.5 and 4.5 V. 1C corresponds to 100 mA g-1 for all the cell tests. The NaM sample was also examined as the reference. The Figure 2a and b show the representative charging and discharging curves for NaMR and NaM samples in half cells. The initial discharge capacities obtained from NaMR and NaM samples are 209.3and 151.8 mAh g-1, respectively, suggesting that the substitution of Ru element could trigger more active sites in P2host. Figure 2c and 2d compare the rate performances of the prepared NaMR and NaM materials, respectively. The discharge capacities of NaMR are 206.3, 183.3, 163.2, 136.2, 121.1, 108.7 and 97.3 mA h g-1 as testing at 0.5, 1, 2, 5, 10, 20 and 50 C, respectively, all of which are higher than those of NaM material. This result suggests that Ru element substituting could significantly improve the rate capability of Mn-based matierial, which could be attribute to higher electronic/ionic conductivity of P2-type NaMR.[42] Moreover, electrochemical stability of two samples are also compared at 2 C in Figure 2e and 2f, also indicating the better electrochemical stability of NaMR electrode. After 50 cycles at 2 C, the delivered capacities retentions are 87.4% for NaMR material. In contrast, the NaM sample shows rapid deterioration of cycle stability to 59.9% after 50 cycles. In addition, the cycle stability of NaMR material was further tested for 200 cycles of Na-ion extraction and insertion process (Figure S3), indicating the inherent structural stability of NaMR with addtion of Ru element during Na-ion extraction and insertion process. To further investigate the influence of the Ru substituting on P2-type material, the NaMR and NaM electrodes were analyzed by cyclic voltammogram (CV) measurement and electrochemical


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impedance spectroscopy (EIS) technique in Na half-cells. The CV measurements of two samples in Na half-cells were examined sweeping bewteen 1.5 and 4.5 V at 0.3 mV s-1. In Figure 3a, the NaM electrode shows many anodic peaks located at 2.64, 2.76, 2.93, 3.12, 3.55 and 3.65 V, respectively. Compare with the NaM electrode, the collected CV profile for NaMR electrode manifests only two large and broad oxidation peaks, suggesting that the substitution of Ru element into the crystal lattice could smooth the electrochemical curve in the Na deintercalation process. In order to evaluating the effect of Ru dopant on the resistances in half cells, the EIS of the NaM and NaMR samples were collected. Figrue. 3b shows the equivalent circuit on account of the Randles model and fitting patterns. A lower charge transfer resistance at the interface is obtained for P2-type NaMR, indicating the faster electronic and ionic conduction of NaMR electrode, which is benefited for lower polarization phenomenon and higher rate capability.[43] The sodium ion diffusion coefficient of these two samples were evaluated by galvanostatic intermittent titration technique . The Figure 3c, 3d and Figure S4 show the galvanostatic intermittent titration technique (GITT) curves and the sodium ion diffusion coefficients of the NaMR and NaM samples. Thediffusion coefficients of Na+ in NaMR is mainly in the region of 10-11  10-12 cm2 s-1 on the basis of the GITT curves, which is competitive with many other reported layered metal oxides,[4445]

and also higher than those of NaM sample, futher indicating the NaMR possesses the faster

sodium ion diffusion behavior during the sodium-ion (de)intercalation processes, which is responsible for high rate performance of NaMR. The charge compensation mechanism of NaMR was measured by the X-ray photoelectron spectroscopy (XPS). The Mn 2p peaks of initial material, charged 4.5V and discharged 1.5V electrodes are summarized in Figure S5. It is clear that the Mn element in initial material is consist of Mn3+ and Mn4+. After charged to 4.5 V, the peak area of Mn4+ remarkably increases and the peak area of Mn3+ only retains a small portion, suggesting that


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the majority of Mn3+ is turned into the Mn4+. Upto discharging insertion to 1.5 V, a large proportion of Mn4+ reduces to the Mn3+. Hence, the Mn3+/Mn4+ redox reaction are mainly responsible for the charge compensation mechanism during the Na-ion (de)intercalation processes. In order to further explore the structural evolution mechanism and more specifically on the effect of the Ru substituting into sodium manganate, the NaMR and NaM cathodes were analyzed by in-situ XRD at the first two cycles during Na-ion extraction/insertion process. As shown in Figure 4a, the typical P2-type (002) and (004) peaks was observed in initial NaM cathode. Upon Na-ion extraction, the (002) and (004) peaks showed no obvious shift and no new peak was formed until 3.5 V, revealing a single-phase reaction during this region. As the continuous Na-ion extraction, besides the P2-phase, a new phase was observed, which could be indexed based on OP4-phase according to previous literature, confirming phase transition from the P2-phase to OP4phase.[41] When further Na-ion deintercalation, a two-phase rection between the concurrence of P2-phase and OP4-phase for NaM could preserve until the end of charging at 4.5V. During the Na-ion intercalation process, the OP4-phase begins to diminish, translating reversibly to the single P2-pahse, and then the a solid-solution reaction proceeds with no new peak appearance until discharging at 2.4 V. Further discharge process, the (002) and (004) peaks split into two peaks, respectively, implying phase transition from the P2-phase to P`2-phase.[35] Finally, a two-phase rection reaction of P2-phase and P`2-phase is present throughout the end of discharge at 1.5V. Analogously, the structural evolution mechanism is reversible/similar to the initial Na-ion intercalation process at the second circle. However, the NaMR material shows a different phase transition mechanism, as shown in Figure 4b. It is clear that in the first charge process, the (002) and (004) peaks first tardily move to a lower angle. No obvious characteristic peak of the OP4 phase or other phase can be observed to the end of 4.5V, revealing an single-phase reaction


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throughout the whole first charge process. On the reverse discharging process, the NaMR cathode first shows an single-phase reaction with over a wide potential range at the potential of 2.0 V. Then a two-phase reaction with P2-phase and P`2-phase is found, and keeping until the end of the first discharge at 1.5V. From the above observation, Ru substitution could effectively suppress the frequent P2-OP4 phase transition by preventing the transition metal layers from gliding to form the OP4 phase. Therefore, the NaMR cathode shows the single-phase region with the P2-type structure over a wider voltage range, which is benefited to the cycling stability, resulting that the NaMR electrode could be cycled at 10 C over 200 cycles. To further research the practical performance of the cathode for SIBs, the prototype rechargeable sodium-ion full celll was assembled by using P2-type NaMR as a cathode and hard carbon as an anode. The reversible capacity of hard carbon is 329.8 mAhg-1 during the charge and discharge process (Figure S6). On the basis of the both anode and cathode mass, the typical electrochemical curves of the full cell show a reversible capacity of 101.0 mAh g-1 and an energy density of 252.5 W h kg-1 at a rate of 0.5 C, which are higher than other full cell systems (Figure 5). The reversible capacities are 101.0, 89.1, 80.6, 69.0, 60.1, mAh g-1 as testing at 0.5, 1, 2, 5, 10 C, respectively. The delivered capacities retention of full cell is 81.8% after 50 cycles at 2 C. Therefore, these achievements of this system are very promising for the deveolpment of Na-ion full battery for smart power grids and large-scale energy storage system. 3. Conclusions In summary, we have successfully prepared Ru substituted P2-Na0.6MnO2 with uniform lamellar morphology by a facile solid-state method. In contrast with NaM, the substituting Ru material could improve the electron conduction and sodium ion conduction, and effectively suppress phase transition at high voltage during sodium ion deintercalation and intercalation.


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Therefore, this NaMR material exhibits enhanced specific capacity, rate capability and cycling performance for Na-ion storage relative to unsubstituting NaM. We expect this basic work will provide new sights of layered oxide materials with further improved performance for Na-ion storage.


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Figure 1. (a) The X-ray diffraction patterns and Rietveld refinements of NaMR. (b) the representative structure model of P2-type NaMR. The (c) SEM, (d) TEM and (e) HRTEM images of NaMR sample. (f) The HAADF-STEM-EDS elemental mapping images of NaMR sample correspond to the selected areas of (d).


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Figure 2. Galvanostatic charge-discharge profiles of (a) NaMR and (b) NaM electrodes in half cells at 0.5 C rate. Rate capability of (c) NaMR and (d) NaM electrodes. The long-term cycling performance of (e) NaMR and (f) NaM electrodes.


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Figure 3. (a) CV profiles of NaMR and NaM electrodes at 0.3 mV s-1. (b) The Nyquist plots and the fitting equivalent circuit model of NaMR and NaM electrodes. (c) Galvanostatic intermittent modes and (d) Na+ diffusion coefficient of NaMR.


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Figure 4. The collected in-situ power XRD patterns of the (a) NaM and (b) NaMR at 0.2 C rate in the voltage window between 1.5 and 4.5 V.


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Figure 5. (a) Galvanostatic charge-discharge profiles of NaMR//hard carbon at a rate of 0.5 C. (b) Rate capability of NaMR//hard carbon. (c) The long-term cycling performance of NaMR//hard carbon at a rate of 2 C. (d) Summary of the specific capacity and energy density of the full cell between NaMR and hard carbon with others reported previously.[46-55]


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ASSOCIATED CONTENT Supporting Information. Material synthesis, SEM, XRD and XPS characterizations, electrochemical performance, supplementary figures S1-6, table S1-2. AUTHOR INFORMATION *E-mail: [email protected] (S. Guo); [email protected] (H. Zhou) Notes The authors declare no competing financial interest. ACKNOWLEDGMENT The financial support from the National Basic Research Program of China (2018YFB0104302), Natural Science Foundation of China (21633003, 51802149, 11704245, 11874199, and U1801251) and Natural Science Foundation of Jiangsu Province of China (BK20170630) are acknowledged. REFERENCES [1]. Armand, M.; Tarascon, J. M., Building Better Batteries. Nature 2008, 451 (7179), 652657. [2]. Vaalma, C.; Buchholz, D.; Weil, M.; Passerini, S., A Cost and Resource Analysis of Sodium-ion Batteries. Nat. Rev. Mater. 2018, 3, 18013. [3]. Hwang, J.-Y.; Myung, S.-T.; Sun, Y.-K., Sodium-ion Batteries: Present and Future. Chem. Soc. Rev. 2017, 3529-3614. [4]. Chen, C.; Wen, Y.; Hu, X.; Ji, X.; Yan, M.; Mai, L.; Hu, P.; Shan, B.; Huang, Y., Na+ Intercalation Pseudocapacitance in Graphene-Coupled Titanium Oxide Enabling Ultra-Fast Sodium Storage and Long-Term Cycling. Nat. Commun. 2015, 6, 6929. [5]. Fang, C.; Huang, Y. H.; Zhang, W. X.; Han, J. T.; Deng, Z.; Cao, Y. L.; Yang, H. X., Routes to High Energy Cathodes of Sodium-Ion Batteries. Adv. Energy Mater. 2016, 6, 1501727. [6]. Wang, P.-F.; You, Y.; Yin, Y.-X.; Guo, Y.-G., Layered Oxide Cathodes for Sodium-Ion Batteries: Phase Transition, Air Stability, and Performance. Adv. Energy Mater. 2018, 8, 1701912.


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Suppressed the High-Voltage Phase Transition of P2-Type Oxide

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