In this paper, we reported the preparation of nanocrystalline Ta3N5 particles by nitridation of Ta2O5 nanoparticles using NH3 as reactant gas. It was found that nanocrystalline Ta2O5 was converted into Ta3N5 completely at 700°C within 5.0 h, which was much lower than the temperature 850°C for the complete nitridation of micron-sized Ta2O5 powder. The resulting nitride was characterized by X-ray diffraction analysis (XRD) and field emission scanning electron microscopy (FE-SEM). The nitrogen contents in the prepared Ta3N5 powders were quantitatively determined with CHN elemental analyzer and thermogravimetry and differential scanning calorimetry (TG-DSC). The color of nanocrystalline Ta3N5 is in fresh red while the one of micrometer-sized Ta3N5 is in dark red.