Rose-red color Nb 2 Zr 6 O 17 - x N x oxynitride photocatalyst was synthesized by thermal ammonolysis of Nb 2 Zr 6 O 17 at 1073 K. TEM image of Nb 2 Zr 6 O 17 - x N x sample showed prismatic pseudo orthorhombic shaped particles with clear edges and an average particle size in the range of 80–90 nm. The photocatalytic activities of the oxynitride samples were studied for hydrogen production by H 2 S splitting under visible light irradiation. The oxynitride Nb 2 Zr 6 O 17 - x N x gave the quantum yield of 13.5% in the production of hydrogen from decomposition of hydrogen sulfide under visible light irradiation.