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A novel three-dimensional photocatalyst, TiO2 particulate film immobilized on activated carbon fibers (TiO2/ACFs),was prepared by liquid phase deposittion. The photocatalyst was characterized by SEM, XRD, BET surface area and photodegradation of methylene blue solution. TiO2 particulate film, with a thickness of nearly 200 nm and grain sizes of 30～50 nm, was deposited on almost each carbon fiber. The inner space between adjacent fibers remained as unmodified ACFs,therefore, both UV illumination and polluted solutions were allowed to pass through the felt-form photocatalyst to form a three-dimensional environment for photocatalytic reactions. With BET surface areas of 400～600 m2/g, the TiO2/ACFs exhibited an enhanced adsorption of pollutants for photocatalysis. Comparative degradations indicated that photocatalytic activity of the TiO2/ACFs was slightly higher than that of Degussa P-25 TiO2. Two special properties, the three-dimensional structure and combined effects of ACFs adsorption and titanias photodegradation, made contribution to high photocatalytic activity. Additionally, the TiO2/ACFs exhibited high stability and potentially application for practical usage.