Neodymium fluoride nanoflakes were successfully prepared by a facile liquid phase preparation with Nd(NO 3 ) 3 and NaF as raw materials. In the process, oxalic acid acting as template agent was found to play important roles in the morphology of neodymium fluorides. The as-synthesized NdF 3 nanoflakes were characterized by various techniques of X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive X-ray spectrometer instrument (EDS). The fluorescent properties of neodymium fluoride nanoflakes were investigated, showing a strong luminescence emission peak at 402nm by the excitation wavelength of 250nm.