Pure hexagonal Nd 2 O 3 nanostructures have been synthesized via a simple precipitation way. For the first time, nanostructured Nd 2 O 3 was produced with utilizing triethylenetetramine as a new precipitant and neodymium nitrate as a neodymium source. The analyses of XRD, FESEM, FT-IR, TEM, EDX, BET and DR-UV-vis were applied to characterize the as-prepared nanostructured Nd 2 O 3. To evaluate the influence of various capping agents on the morphology, grain size and photocatalytic performance of Nd 2 O 3 , several experiments were performed. The results demonstrated that the kind of capping agent has substantial impact on the shape, grain size and photocatalytic performance of Nd 2 O 3. In addition, application of the synthesized Nd 2 O 3 samples as photocatalyst by photodegradation of methylene blue contaminant under ultraviolet illumination was investigated.