Synchrotron powder X-ray diffraction (PXRD) has been used to study in-situ the hydrothermal intercalation of lithium ions in titania powder following the reaction TiO 2 + 2 LiOH Ǟ Li 2 TiO 3 + H 2 O. Syntheses were performed in a sapphire capillary at temperatures between 133 and 230°C. By sequential Rietveld refinement of the PXRD data, the particle growth of the metastable cubic α-Li 2 TiO 3 compound was determined as a function of the reaction time, as well as the transforma-