Nanocrystalline LiFePO 4 and doped LiTi 0.01 Fe 0.99 PO 4 powders were synthesized via a sol-gel preparation route. High-resolution tunneling electron microscopy observation and energy dispersive spectroscopy, mapping show the homogeneous distribution of dopant Ti cations in the crystals. Fe and O K-edge X-ray absorption near-edge structure ͑XANES͒ measurements show that Ti 4+ doping induces an increased unoccupied d-state in LiFePO 4 , resulting in an enhanced p-type semiconductivity. In situ Fe K-edge XANES measurements of Ti-doped and undoped LiFePO 4 electrodes have been performed to determine the change of Fe valence during the lithium intercalation and de-intercalation processes. Both LiFePO 4 and doped LiTi 0.01 Fe 0.99 PO 4 cathodes demonstrate good electrochemical performance.
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