The paper reports the results of a preparation of photocatalysts based on niobium pentaoxide (Nb 2 O 5 ). These materials have been obtained by calcination of a Nb 2 O 5 precursor with alkali metal hydroxides (Li, Na, K). The obtained materials have been characterized by several methods, i.e., XRD, DR-UV-vis, and FTIR/DRS. The photocatalytic decomposition of phenol as a model contaminant has been investigated in the presence of all the prepared photocatalytic materials under UV-light irradiation. Of all investigated samples, Na/Nb 2 O 5 has the highest activity.