Nanodiscs and nanorods of LaF3: Nd3+, Sm3+ (LFNS) have been obtained by new rapid microwave assisted synthesis using deionized water and methanol as solvents. Structural analysis shows a hexagonal crystal structure with particle size lying between Band 20 Rm. FTIR, FT-Raman and thermal studies show the presence and removal of surface groups which make LFNS water soluble. Annealed samples indicate adsorption of atmospheric CO2. Narrow size distribution of particles and presence of wide transparency window desirable in optoelectronic applications have been detected in UV-visible spectra. The SHG efficiency is seen to be enhanced in methanol. Photoluminescence studies show emission of red (654 nm) fluorescence. Dielectric studies inchoate a dc conduction mechanism with involvement of the real part of dielectric constant in the process of polarization. (C) 2013 Elsevier B.V. All rights reserved.