The present work focused on the synthesis and characterization of T1CdI(3) nanostructures through a new mechanical mixture of the reactants method for the first time. In this work, thallium nitrate, cadmium nitrate and lithium iodide were chosen as starting reagents. The preparation of CdI2 and TII for synthesis of TICdI3 were performed at ambient condition. The morphology, phase structure, and phase purity of TICdI3 can be controlled by the TII:CdI2 ratio and also adjusting type of surfactant. In our experimental conditions, the ideal ratios between TII:CdI2 was 1:1, Also the ideal surfactant was SDS. The nanostructures were characterized by using XRD, SEM, TEM, EDS and FT-IR. The photocatalytic activity of the synthesized products has been compared in the photodegradation activity of methyl orange (MO) and methylene blue (MB). (C) 2016 Elsevier B.V. All rights reserved: