LnPO(4) (Ln = Y, Lu) orthophosphates have been prepared by a new sol-gel route. Eu3+ doped materials have also been synthesized and studied. X-ray diffraction performed on all samples showed that pure xenotime phase is obtained in all cases even for doped samples. The morphology of the powders has been determined and small grains with narrow size distribution are evidenced. Finally the optical properties of the doped materials have been studied, the substitution of Eu3+ for Ln(3+) is confirmed and the radiative lifetimes are compatible with potential applications of these phosphors. (C) 2003 Elsevier Science B.V. All rights reserved.