A novel AgCl/AgIO 4 composite was fabricated via an in-suit synthetic method. The as-prepared samples have been characterised by using X-ray diffraction, transmission electron microscopy, scanning electron microscopy, UV-vis diffuse reflectance spectroscopy, X-ray photoelectron spectroscopy and electrochemical impedance spectroscopy. Rhodamine B dilute solution was used to discuss the photocatalytic activities of the as-prepared composites under the visible light irradiation. Experimental results showed that with increasing the contents of AgIO 4 the photocatalytic activity of the as-prepared hybrids was first increased and then decreased. When the molar ratio of AgCl to AgIO 4 was 1:5, in 30 min, the as-prepared composites with the bandgap of 1.21 eV exhibited the highest photocatalytic activity and possessed 96.3% of degradation efficiency. That was increased by 71.5 and 27.9% compared with AgCl and AgIO 4 , respectively. Moreover, AgCl was linked with AgIO 4 via chemical bonds rather than physical contact at the interfaces of these two semiconductors. In addition, a possible photocatalytic degradation mechanism for the as-prepared hybrids was also presented.