Neodymium Vanadate (NdVO4) nanostructures were successfully synthesized via a modified solid state method in the presence of ligand. These nanoparticles were further used as a photocatalyst. Primarily the best structural formations and smallest crystallite sizes of the systems were identified and optimized by changing the calcination time, calcination temperature and molar ratio of the ligand. The cationic (Methyl Violet (MV)), and anionic (Eosin Y (EY) and Eriochrome Black T (EBT)) dyes were used as a model to evaluate the photoactivity under UV-Vis irradiation. Several operational factors were examined to improve the photocatalytic efficiency include type of dye, type of light source, pH and dye concentration. As a result, the best efficiency in 5 ppm Eriochorome Black T at pH = 11 was achieved in the presence of 0.05 g NdVO4 nanocatalysts.