In this work, a set of nanoparticles of Nb2O5 nanoparticles were grown by both the Pechini and the sol-gel methods. The amorphous materials were calcined at 650 #xB0;C or at 750 °C. X-ray diffraction, scanning electron microscopy, luminescence and Raman spectroscopy were used in order to characterize the materials. From the study, it is possible to state that the method of production of nanoparticles, beyond the temperature of synthesis, has a great influence on whether the phase produced is hexagonal or orthorhombic. Additionally, compared to de Sol-gel method, the Pechini method produced samples with smaller particle sizes. The photoluminescence spectra of niobium pentoxide nanostructure materials show that the emission peaks are positioned between 334 to 809 nm and there is a change of intensity which varies depending on the synthesis route used. High pressure Raman spectra at room temperature were obtained from two samples grown by the sol-gel method. Up to 6 GPa, where it is possible to observe the Raman bands, no modification other than the increase of disorder was observed, and this can be associated with a change of phase.