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Batteries 2018, 4, 8 8 of 10 3.4. Cell Assembly and Electrochemical Tests Three-electrode Swagelok cells were assembled inside an argon-filled glove-box (mBraun) with water and oxygen content below 0.1 ppm. The cell configuration for all tests was: Na metal (99.8%, ACROS ORGANICS, Geel, Belgium) as reference and counter electrode (RE, CE), 1M NaPF6 (sodium hexafluorophosphate, 99+%, FluoroChem, Glossop, UK) in PC (propylene carbonate, battery grade, BASF, Ludwigshafen, Germany) as electrolyte with glass fiber disks (GF/D, Whatman, Maidstone, UK) as separator and NMO as working electrode (WE). NaPF6 and PC were used without further purification. Electrodes (all possessing similar mass loading) were tested through cyclic voltammetry (CV) with a scan rate of 0.1 mV s−1 in the potential range of 2.0 V–3.8 V vs. Na/Na+ (VMP3 multichannel potentiostat, BioLogic, Seyssinet-Pariset, France). The galvanostatic cycling was performed between 2.0 V and 3.8 V at various current densities ranging from C/10 to 5 C (1 C = 121 mA g−1) (Maccor battery tester 4300, Maccor Inc., OK, USA). All electrochemical tests were carried out at 20 ± 1 ◦C. 4. Conclusions For the first time, Na0.44MnO2 nanometric slabs were synthesized using an urea-based solution combustion synthesis and a subsequent annealing process. This simple synthetic approach, which makes use of the eco-friendly urea, enabled the preparation of Na0.44MnO2 cathode material in less time (2 h) and at a lower annealing temperature (700 ◦C) compared to state-of-the-art synthesis routes such as solid-state and sol-gel methods. SEM revealed smaller particle dimensions as a result of the aforementioned synthesis conditions. Moreover, the final cathode material has shown superior electrochemical performances, in terms of delivered capacities at high C rates of up to 5 C (i.e., 105mAhg−1 at1Cand80mAhg−1 at5C). The improved capacities at high rates can be ascribed to the different morphology, i.e., smaller slabs characterized by a lower degree of anisotropy. Hence, the results suggest that reducing the particle sizes may be a suitable strategy for improving the high rate performances of Na0.44MnO2 cathode materials. Supplementary Materials: The following are available online at www.mdpi.com/2313-0105/4/1/8/s1, Figure S1: XRDP of the NMO sample after a thermal treatment at 800 ◦C under N2 flux, Figure S2: Thermogravimetric analysis of the SS- and SC-NMO powders. Acknowledgments: L.G.C., S.P and D.B acknowledge the financial support of the Helmholtz Association. C.T. is grateful for the financial support of Fondazione Cariplo and Regione Lombardia through grant 2015-0753. Conflicts of Interest: The authors declare no conflict of interest. References 1. Kundu, D.; Talaie, E.; Duffort, V.; Nazar, L.F. The Emerging Chemistry of Sodium Ion Batteries for Electrochemical Energy Storage. Angew. Chem. Int. Ed. 2015, 54, 3432–3448. [CrossRef] [PubMed] 2. Hwang, J.-Y.; Myung, S.-T.; Sun, Y.-K. Sodium-ion batteries: Present and future. Chem. Soc. Rev. 2017, 46, 3529–3614. [PubMed] 3. Kubota, K.; Komaba, S. Review—Practical Issues and Future Perspective for Na-Ion Batteries. J. Electrochem. Soc. 2015, 162, A2538–A2550. [CrossRef] 4. Yabuuchi, N.; Kubota, K.; Dahbi, M.; Komaba, S. Research Development on Sodium-Ion Batteries. Chem. Rev. 2014, 114, 11636–11682. [CrossRef] [PubMed] 5. Kim, H.; Kim, H.; Ding, Z.; Lee, M.H.; Lim, K.; Yoon, G.; Kang, K. Recent Progress in Electrode Materials for Sodium-Ion Batteries. Adv. Energy Mater. 2016, 6, 1600943. 6. Xiang, X.; Zhang, K.; Chen, J. Recent Advances and Prospects of Cathode Materials for Sodium-Ion Batteries. Adv. Mater. 2015, 27, 5343–5364. [CrossRef] [PubMed]PDF Image | Sodium-Ion Batteries Obtained through Urea Based
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