NaBiO3/BiOCl composite photocatalysts with heterostructure have been prepared by a novel in situ formation approach, by using NaBiO3 and hydrochloric acid aqueous solutions as the raw materials Under visible light (lambda > 400 nm) irradiation, the photocatalytic activity of Rhodamine B over NaBiO3/BiOCl photocatalysts has been evaluated The results demonstrate that the combination of NaBiO3 and BiOCl has a higher photocatalytic activity compared with single NaBiO3 or BiOCl photocatalyst, due to more effective photo-excited electron-hole separation by the heterojunction semiconductor structure and also higher absorption capacity of NaBiO3. (C) 2010 Elsevier B V. All rights reserved.