A series of molybdenum titanium oxides (TiO2-MoO3) were successfully prepared by hydrothermal method using P25 and TiCl4 as titanium resource, respectively. The particle size and morphology of molybdenum titanium oxides was controlled by adding thiourea as surfactant. The catalytic activity of the obtained materials was evaluated by degradation of NO under simulated solar light irradiation. The results showed that the morphology of obtained molybdenum titanium oxide can be significantly controlled by adding thiourea. And the samples with novel curly petal-like layered structure exhibited superior catalytic activity. Trapping experiments revealed that center dot O-2(-) was the main active specie in the catalytic system. Also the catalyst had superior stability and reusability. Graphic