Nanosized and highly crystalline spinel lithium titanium oxide (Li4Ti5O12, LTO) particles are synthesized in supercritical water. The effects of various synthesis conditions - feed concentration, reaction time, and calcination - on the particle properties, including particle size, surface area, particle morphology, phase purity, and crystallinity, are carefully analyzed. Phase-pure LTO particles are obtained with a long reaction time of 6h in supercritical water at 400 degrees C and 300 bar without subsequent calcination, while the anatase TiO2 impurity phase is detected at shorter reaction times of 5 min to 2 h. Particles synthesize in supercritical water with subsequent calcination at a relatively low temperature of 700 degrees C exhibit the highly crystalline LTO phase. Based on the analytical results using scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), and X-ray diffraction (XRD), an LTO formation mechanism in supercritical water is proposed. LTO particles prepare in supercritical water with subsequent calcination exhibit excellent long-term cyclability and high-rate performance. The discharge capacity after 400 cycles at 1C is 117.2 mAh g(-1), which is approximately 80% of the initial discharge capacity (147.1 mAh g(-1)), and the discharge capacity at 10C is 100.5 mAh g(-1). These electrochemical performances are significantly better than those of uncalcinated LTO synthesize in supercritical water and solid-state synthesize LTO. Crown Copyright (C) 2012 Published by Elsevier Ltd. All rights reserved.
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