Microwave-assisted hydrothermal synthesis of low-temperature LiCoO2

A microwave-assisted hydrothermal synthesis route was developed for LT-LiCoO2 and compared with the conventional hydrothermal synthesis. Our X-ray diffraction, magnetisation, and electron microscopy and electrochemical studies in both cases indicate phase-pure and practically stoichiometric material...

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Main Authors: Jähne, Carsten (Author) , Klingeler, Rüdiger (Author)
Format: Article (Journal)
Language:English
Published: July 1, 2012
In: Solid state sciences
Year: 2012, Volume: 14, Issue: 7, Pages: 941-947
ISSN:1293-2558
DOI:10.1016/j.solidstatesciences.2012.04.033
Online Access:Verlag, Volltext: http://www.sciencedirect.com/science/article/pii/S1293255812001501
Verlag, Volltext: http://dx.doi.org/10.1016/j.solidstatesciences.2012.04.033
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Author Notes:C. Jähne, R. Klingeler

MARC

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520 |a A microwave-assisted hydrothermal synthesis route was developed for LT-LiCoO2 and compared with the conventional hydrothermal synthesis. Our X-ray diffraction, magnetisation, and electron microscopy and electrochemical studies in both cases indicate phase-pure and practically stoichiometric materials with Li-content ≥0.99. The microwave-assisted procedure allows reducing the synthesis temperature down to 170 °C which yields plate-like nano-sized LT-LiCoO2 compared to the conventionally synthesized micro-scaled material. These differences clearly show-up in the cyclic voltammetry and the galvanostatic intermittent titration technique data which are used for further characterisation of the materials. In both cases, a tiny non-stoichiometry is suggested by the presence of low-temperature small high-spin Co4+-ions. Our results show that the microwave-assisted process allows lower synthesis temperatures for practically stoichiometric LT-LiCoO2 which is associated to size-reduction of the resulting crystallites down to the nanometre-scale and a higher fraction of the competing spinel phase. 
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