Amorphous titanium oxide nanoparticles were prepared from titanium isopropoxide. In situ measurements reveal an extraordinary high capacity of 810 mAh/g on the first discharge. Upon cycling at a charge/discharge rate of 33.5 mA/g, this capacity gradually decreases to 200 mAh/g after 50 cycles. The origin of this fading was investigated using X-ray absorption spectroscopy and solid-state nuclear magnetic resonance. These measurements reveal that a large fraction of the total amount of the consumed Li atoms is due to the reaction of H 2 O/OH species adsorbed at the surface to Li 2 O, explaining the irreversible capacity loss. The reversible capacity of the bulk, leading to the Li 0.5 TiO 2 composition, does not explain the relatively large reversible capacity, implying that part of Li 2 O at the TiO 2 surface may be reversible. The high reversible capacity, also at large ͑dis͒charge rates up to 3.35 A/g ͑10C͒, makes this amorphous titanium oxide material suitable as a low cost electrode material in a high power battery. © 2010 The Electrochemical Society. ͓DOI: 10.1149/1.3332806͔ All rights reserved. Electrochemical storage devices based upon lithium-ion technology have replaced earlier battery types in numerous applications, e.g., portable devices, mainly due to their high energy density, long cycle life, and their relatively low impact on the environment. If materials that support higher current densities during discharging and satisfy the safety issues concerned, Li-ion batteries would become available for heavy duty applications such as ͑hybrid͒ electrical cars.A high power density requires both good ionic and electronic transport properties of the electrode materials. In many cases, the solid-state diffusion of Li ions through the electrode materials is several orders of magnitude smaller than in the electrolyte. Therefore, if the power density is to be improved, the electrode performance is to be investigated. In commercially available Li-ion batteries, the electrode material is dispersed in the electrolyte as microsized crystallites, which are capable of hosting the lithium ions inside their crystalline voids. By simply decreasing the size of these crystallites, the electrode-electrolyte interface is increased, whereas the diffusion length inside the electrode crystallite decreases. However, recent studies reveal a more complex behavior of nanosized Li insertion compounds in, e.g., TiO 2 anatase, 1-3 TiO 2 rutile, 4,5 or Li x FePO 4 , 6 showing distinct changes in electronic structure and ionic mobility upon downsizing to the nanodomain. 7 Usually, these differences in electronic structure and ionic mobility between bulk and nanosized crystallites are ascribed to the relatively increased impact of surface phenomena. [8][9][10] Between the crystalline structures anatase and rutile TiO 2 , similarities were observed in the physical behavior of the nanoscale compounds. Both reveal an increased Liion capacity compared to their microscale counterparts, which appears to be facilitated by an anomalous phase behavi...