In this paper, non-treated ACF (Activated Carbon Fiber) /$TiO_2$ and Zn-treated ACF/$TiO_2$ were prepared. The prepared composites were characterized in terms of their structural crystallinity, elemental identification and photocatalytic activity. XRD patterns of the composites showed that the non-treated ACF/$TiO_2$ composite contained only typical single and clear anatase forms while the Zn-treated ACF/$TiO_2$ contained a mixed anatase and rutile phase with a unique ZnO peak. SEM results show that the titanium complex particles are uniformly distributed on and around the fiber and that the titanium complex particles are more regularly distributed on and around the ACF surfaces upon an increase of the $ZnCl_2$ concentration. These EDX spectra show the presence of peaks from the C, O and Ti elements. Moreover, peaks of the Zn element were observed in the Zn-treated ACF/$TiO_2$ composites. The prominent photocatalytic activity of the Zn-treated ACF/$TiO_2$ can be attributed to the three different effects of photo-degradation: doping, absorptivity by an electron transfer, and adsorptivity of porous ACFs between the Zn-$TiO_2$ and Zn-ACF.