NdOHCO3 dodecahedral microcrystals with an orthorhombic structure have been successfully synthesized by the hydrothermal method used urea as the precipitator. Experimental parameters, such as the reaction temperature, the reaction time, and the molar ratio of the starting reagents were examined. The as-synthesized products were characterized by powder X-ray diffraction, transmission electron microscopy, field-emission scanning electron microscopy, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, and photoluminescence. The possible growth process of NdOHCO3 dodecahedral microcrystals was discussed. (C) 2009 Elsevier Ltd. All rights reserved.