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Electrochemical cycling performance of microsize bulk and thin film Sn electrodes up to 50 cycles in Mg half‐cell configuration, as well as Mg diffusivity and interfacial reaction behavior in a phenylmagnesium chloride (PhMgCl)/THF electrolyte are studied. The bulk Sn electrode delivers capacities of 321–289 mAh g−1 with capacity retention of 90 % and coulombic efficiencies higher than 99 % over 30 cycles, and thus demonstrates the potential of Sn anodes. The Sn film electrode shows good cycling ability. Surface analysis by XPS reveals that the surface of cycled electrodes is composed of a mixture of various inorganic salts of Sn and Mg formed by interfacial reactions between Sn and PhMgCl, and organic functionality produced by decomposition of THF, indicating surface film formation. The Mg2+ diffusivity of Sn is on the order of 10−11 cm2 s−1, which is four orders of magnitude lower than the Li+ diffusivity of Sn in Li‐ion batteries. Advanced material design for enhanced electronic conductivity and control of the interfacial chemistry for formation of a surface protective film are believed to be the keys to overcome such sluggish kinetics, increase the capacity, and improve the cycling performance.

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Capacity of layered lithium nickel-cobalt-manganese oxide (LiNi 1-x-y Co x Mn y O 2 ) cathode material can increase by raising the charge cut-off voltage above 4.3 V vs. Li/Li + , but it is limited due to anodic instability of conventional electrolyte. We have been screening and evaluating various sulfone-based compounds of dimethyl sulfone (DMS), diethyl sulfone (DES), ethyl methyl sulfone (EMS) as electrolyte additives for high-voltage applications. Here we report improved cycling performance of LiNi 0.5 Co 0.2 Mn 0.3 O 2 cathode by the use of dimethyl sulfone (DMS) additive under an aggressive charge condition of 4.6 V, compared to that in conventional electrolyte, and cathode-electrolyte interfacial reaction behavior. The cathode with