Abstract Heterostructures based on Ag 3 PO 4 nanoparticles and TiO 2 nanobelts were prepared by a coprecipitation method. The crystalline structures were characterized by X-ray diffraction measurements. Electron microscopic studies showed that the Ag 3 PO 4 nanoparticles and TiO 2 nanobelts were in intimate contact which might be exploited to facilitate charge transfer between the two semiconductor materials. In fact, the heterostructures exhibited markedly enhanced photocatalytic activity as compared with unmodified TiO 2 nanobelts or commercial TiO 2 colloids in the photodegradation of methyl orange under UV irradiation. This was accounted for by the improved efficiency of interfacial charge separation thanks to the unique alignments of their band structures. Remarkably, whereas the photocatalytic activity of the heterostructure was comparable to that of Ag 3 PO 4 nanoparticles alone, the heterostructures exhibited significantly better stability and reusability in repeated tests than the Ag 3 PO 4 nanoparticles.