A new type of nanocomposite containing SnO2 has been obtained by wet impregnation of dehydrated Mg/Al-hydrotalcite-type compounds with ethanolic solutions of SnCl4 center dot 2H(2)O. Tin chloride hydrolysis was achieved using NaOH or NH4OH aqueous solutions, at pH around 9, followed by the conversion into corresponding hydroxides through calcinations. The powder X-ray diffraction (PXRD) and UV-Vis diffuse reflectance (UV-DR) methods confirmed the structure of as-synthesized solids. The chemical composition and morphology of the synthesized materials were investigated by energy dispersive X-ray analysis (EDX), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The as-synthesized materials were used for photocatalytic studies showing a good activity for methylene blue decolourization, which varies with SnO2 content and used as a hydrolysing agent. The proposed mechanism is based on the shifting of flat band potential of SnO2 due to the interaction with Mg/Al-LDH, this being energetically favourable to the formation of hydroxyl radicals responsible for methylene blue degradation. (C) 2009 Elsevier B.V. All rights reserved.