The nanometer particles of two Fe x O y /TiO 2 's with high photocatalytic activities were obtained through hydrothermal treatment and impregnation method. The XRD result did not show the peaks assigned to the Fe components (for example Fe 2 O 3 , Fe 3 O 4 , FeO 3 , and Fe metal) on the external surface of the anatase structure in the Fe x O y /TiO 2 attained through hydrothermal treatment. This meant that Fe components were well incorporated into the TiO 2 anatase structure. In addition, it exhibited uniform anatase structure with particle size of below 50nm. The FeO 3 component on the external surface of the TiO 2 anatase structure was identified in the Fe-loaded TiO 2 prepared through the impregnation method. In particular, the FT-IR spectroscopy revealed that the Fe x O y /TiO 2 particle attained through hydrothermal treatment had higher hydrophilic property compared to the other catalysts. Together with the Fe component, they absorbed wavelength of above 370nm. The band slightly shifted to the right without tail broadness, which was the UV absorption of Fe oxide in the Fe x O y /TiO 2 particle attained through hydrothermal method. This meant that Fe components were well inserted into the framework of the TiO 2 anatase structure. Despite the red shift in UV-Vis absorption, however, CHCl 3 decomposition on the Fe x O y /TiO 2 catalyst was not largely enhanced compared to pure TiO 2 .