A kind of lead-free nanocrystalline powder, (Li0.06Na0.47K0.47)NbO3 (LNKN), has been prepared by a newly developed sol-gel method using Nb2O5 as the Nb source. Phase analysis, microstructure and morphology of the powder were determined by X-ray diffraction (XRD), Fourier transform infrared (FTIR), Raman, transmission electron microscope (TEM) and high-resolution transmission electron microscopy (HRTEM). The experimental results showed that pure perovskite phase was formed at the temperature as low as 500 degrees C. Besides, the obtained powder belonged to tetragonal symmetry, and the mean particle size was as small as 20nm. It is believed that the high-quality gel precursor and low processing temperature play a key role in the formation of the LNKN nano-particles. The process developed in this work was convenient to realize the mass production of LNKN nano-powders at low cost. (C) 2008 Elsevier B.V. All rights reserved.