Photocatalytic hydrogen production with nickel oxide intercalated K4Nb6O17 under visible light irradiation

Nickel oxide nanoclusters were intercalated to layered niobate, K₄Nb₆O₁₇, to improve the photocatalytic hydrogen production for water splitting under visible light irradiation. A K₄Nb₆O₁₇–SSRx (Ni/Nb ratio range of 0.8–5%) series of nickel oxide intercalated layered niobates was prepared by a two-step solid-state reaction and characterized by Extended X-ray Absorption Fine Structure (EXAFS), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Energy Dispersive Spectrometer (EDS), X-ray Photoelectron Spectroscopy (XPS) and Ultraviolet–visible spectroscopy (UV–vis). The photocatalytic reaction was carried out in a quartz reactor irradiated under a 500-W halogen lamp. The K₄Nb₆O₁₇–SSR0.2 catalyst exhibited a much higher photocatalytic activity for water splitting than unloaded K₄Nb₆O₁₇ catalyst and NiO_y/K₄Nb₆O₁₇ catalyst prepared by the conventional impregnation method. The high catalytic performance was attributed to the well dispersed nickel oxide nanoclusters intercalated into the bulk structure of K₄Nb₆O₁₇ catalyst and the lack of NiO particles on the external particle surface.