In order to more easily separate TiO
2 photocatalyst from the treated wastewater, TiO
2 film was immobilized on the surface of activated carbon fibers (ACFs) by employing two kinds of coating procedures, dip-coating, and hydrothermal treatment. The effects of coating procedures on microstructure of TiO
2-coated ACFs (TiO
2/ACFs), such as morphology, porous property, crystal structure, and light absorption characteristics were investigated in detail. The adhesion property between TiO
2 film and ACFs was evaluated by ultrasonic vibration, and the photocatalytic activity of TiO
2/ACFs was tested by the photocatalytic decoloration of methylene blue solution. The results show that hydrothermal treatment presented many advantages to obtain high-performance TiO
2/ACFs photocatalyst in comparison with dip-coating. Hydrothermal treatment could improve the binding property between TiO
2 films and ACFs, which endowed the as-obtained TiO
2/ACFs photocatalyst with improved reusable performance, and TiO
2/ACFs synthesized by hydrothermal treatment presented higher photocatalytic activity.
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