K(1 - 2x)M(x)iNbO(5) (M=Mn,Ni) photocatalytic material was prepared through a successive ion-exchange reaction of KTiNbO5, which was synthesized by a solid-state reaction, with Mn2+ or Ni2+, respectively. The microstructure and the spectral response characteristic of K1 - 2xMxTiNbO5 were investigated by means of powder X-ray diffraction (XRD), laser Raman spectroscopy (LRS), and UV-vis diffuse reflectance spectrum (UV-vis DRS). The photocatalytic activities were evaluated by the oxidation of dimethyl sulfide (DMS) and ethyl mercaptan (EM) under natural light (NAT-L) and ultraviolet light (UV-L) irradiation, and the surface species were determined by technology of Fourier-transform infrared (FT-IR) spectroscopy. XRD patterns indicate that ion exchange has changed the interlayer distance. LRS spectra show that there is a significant interaction between the interlayer cation and the terminal Nb=O bond. DRS spectra reveal that an additional absorption edge, which locates at a longer wavelength region, can be observed for K1- 2xMxTiNbO5. For photocatalytic oxidation of DMS and EM, K1 - 2xNixTiNbO5 has an activity whether under NAT-L or UV-L irradiation. Based on the reactant structure feature and the product distribution, possible reaction pathways of the photocatalytic oxidation for DMS and EM used layered K1 - 2xMxTiNbO5 catalyst were proposed. (C) 2014 Elsevier B.V. All rights reserved.