The Fe-ACF/TiO 2 composites were prepared by a sol-gel method and were characterized by nitrogen adsorption, Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), and Energy Dispersive X-ray (EDX). The Fe-ACF/TiO 2 composites were developed for the decomposition of organic dyes by using a UV lamp. The decomposition effect was investigated under various conditions, such as three selected non-biodegradable organic dyes like Methylene Blue (MB), Methyl Orange (MO), Rhodamine B (Rh.B), and in the presence of Fe and hydrogen peroxide (H 2 O 2 ). The photocatalytic activity was derived from possible combination effects, such as (1) adsorption of ACF, (2) generation of electron/hole by TiO 2 , (3) photo-Fenton reaction of Fe, and (4)