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The photocatalysts of Fe-ACF/$TiO_2$ compositeswere prepared by the sol-gel method and characterized by BET, XRD, SEM, and EDX. It showed that the BET surface area was related to adsorption capacity for each composite. The SEM results showed that ferric compound and titanium dioxide were distributed on the surfaces of ACF. The XRD results showed that Fe-ACF/$TiO_2$ composite only contained an anatase structure with a Fe mediated compound. EDX results showed the presence of C, O, and Ti with Fe peaks in Fe-ACF/$TiO_2$ composites. From the photocataytic degradation effect, $TiO_2$ on activated carbon fiber surface modified with Fe (Fe-ACF/$TiO_2$) could work in the photo-Fenton process. It was revealed that the photo-Fenton reaction gives considerable photocatalytic ability for the decomposition of methylene blue (MB) compared to non-treated ACF/$TiO_2$, and the photo-Fenton reaction was improved by the addition of $H_2O_2$. It was proved that the decomposition of MB under UV (365 nm) irradiation in the presence of $H_2O_2$ predominantly accelerated the oxidation of $Fe^{2+}$ to $Fe^{3+}$ and produced a high concentration of OH radicals.
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