Monoclinic and hexagonal CePO 4 nanoparticles and nanorods were successfully synthesized from Ce(NO 3) 3·6H 2O and Na 3PO 4·12H 2O solutions at pH 1-5 by a 180 W microwave radiation for 60 min. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, and scanning electron microscopy (SEM). XRD patterns revealed that the products are hexagonal CePO 4 structures at pH 2-5, and monoclinic CePO 4 structures at pH 1. SEM characterization shows that these products were nanoparticles, short nanorods, and long nanorods, controlled by the pH of the precursor solutions. Optical properties of the nanorods were also investigated by ultraviolet-visible (UV-vis) and photoluminescence (PL) spectroscopy. © The Nonferrous Metals Society of China and Springer-Verlag Berlin Heidelberg 2011.