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High temperature X-ray diffraction study of the formation of Na_(2)Ti_(3)O_(7) from a mixture of sodium carbonate and titanium oxide

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Journal of Energy Chemistry 2022年第2期31卷 210-218页

作者： Caroline Piffet Bénédicte Vertruyen Frédéric Hatert Rudi Cloots Frédéric Boschini Abdelfattah Mahmoud GREENMAT CESAM Research UnitChemistry DepartmentUniversity of Liège4000 LiègeBelgium Laboratory of Mineralogy Geology Research UnitUniversity of Liège4000 LiègeBelgium

Na2Ti3O7 has attracted much attention in the field of anode materials for Na-ion batteries thanks to its non-toxicity and very low working potential of 0.3 V vs Na0/Na+.Building a clearer picture of its formation from cheap Na_(2)CO_(3) and TiO_(2) starting materials is therefore of obvious interest.Here,we report new insights from an in-situ high temperature X-ray diffraction study conducted from room temperature to 800°C,complemented by ex-situ characterizations.We were thereby able to position the previously reported Na_(4)Ti_(5)O_(12) and Na_(2)Ti_(6)O_(13) intermediate phases in a reaction scheme involving three successive steps and temperature ranges.Shifts and/or broadening of a subset of the Na_(2)Ti_(6)O_(13) reflections suggested a combination of intra-layer disorder with the well-established ordering of successive layers.This in-situ study was carried out on reproducible mixtures of Na_(2)CO_(3) and TiO_(2) in 1:3 molar ratio prepared by spraydrying of mixed aqueous suspensions.Single-phase Na_(2)Ti_(3)O_(7) was obtained after only 8 h at 800°C in air,instead of a minimum of 20 h for a conventional solid-state route using the same precursors.Microstructure analysis revealed~15 mm diameter granules made up from rectangular rods of a fewmm length presenting electrochemical properties in line with expectations.In the absence of grinding or formation of intimate composites with conductive carbon,the specific capacity of 137 m Ah/g at C/5 decreased at higher rates.

关键词： Formation mechanism High temperature XRD Na_(2)Ti_(3)O_(7) Spray-drying synthesis Na-ion batteries

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