Synthesis of lithium ion conducting tantalates has been carried out by conventional solid-state reaction (SSR) techniques and by precipitation from solutions (PS). It is shown that the latter chemical route leads to the formation of a pure perovskite phase, made up of nanosized particles, and uses milder conditions when compared with the solid-state reaction technique. Thermal analyses, X-ray powder diffraction (XRD) and infrared (IR) spectroscopy are used to investigate the phase transformations that occur during the preparation of these tantalates from powder precursors. After sintering, the nanosized particles of the powder obtained by the (PS) route are preserved and pellets with good compactness