Abstract: | Composites of (001)‐face‐exposed TiO2 ((001)‐TiO2) and CuO were synthesized in water vapor environment at 250°C with various Cu/Ti molar ratios (RCu/Ti). The resulting CuO/(001)‐TiO2 composites were characterized using a variety of techniques. The synthesis under high‐temperature vapor allows close contact between CuO and (001)‐TiO2, which results in the formation of heterojunctions, as evidenced by the shift of valence band maximum towards the forbidden band of TiO2. An appropriate ratio of CuO can enhance the absorption of visible light and promote the separation of photogenerated carriers, which improve the photocatalytic performance. The degradation rate constant Kapp increased from 5.5 × 10?2 to 8.1 × 10?2 min?1 for RCu/Ti = 0.5. Additionally, the results showed that superoxide radicals (?O2?) play a major role in the photocatalytic degradation of methylene blue. |