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 21 for the cubes versus 12 pm V 21 for spheres).