A visible-light active TiO2-xSx in rutile structure has been synthesized by means of a mechanochemical method. The method is composed of two steps: the first is grinding the mixture of sulfur and TiO2, and the second is calcining the ground sample at 673 K in an inert gas flow. XPS analysis confirms that sulfur has been successfully doped into TiO2. The calcined sample under irradiation of visible light with wave-length over 510 nm has shown good performance for NO gas destruction, suggesting its high photograph-reactivity.