Methods have been developed for the shape-selective synthesis of ferroelectric LiNbO 3 nanoparticles. Decomposition of the single-source precursor, LiNb(O-Et) 6, in the absence of surfactants, can reproducibly lead to either cube- or sphere-like nanoparticles. X-Ray diffraction shows that the LiNbO 3 nanoparticles are rhombohedral (R3c). Sample properties were examined by piezoresponse force microscopy (PFM) and Raman where both sets of nanoparticles exhibit ferroelectricity. The longitudinal piezoelectric coefficients, d 33, varied with shape where the largest value was exhibited in the nanocubes (17 pm V -1 for the cubes versus 12 pm V -1 for spheres).