The research of synthesis of impregnated TiO2 Ouw natural clay with the study of calcination temperature has been done. The calcination process was carried out at temperature variations of 200, 300, and 400 oC. Characterization of the structure was performed by using X-ray diffraction (XRD), scanning electron microscope (SEM) and infrared (IR) spectrophotometer. The result of characterization with XRD showed that the impregnated TiO2 clay at 200 oC has the highest crystallinity. Calcination at 300 oC resulted in the loss of a montmorillonite reflection peak, while calcination at 400 °C resulted in the loss of two montmorillonite reflections and a drastic decrease in intensity. The crystalline phase of TiO2 formed was a combination of the crystalline phases of rutile and anatase, with the rutile crystalline phase being more dominant. The SEM characterization results showed a more even distribution of TiO2 in calcined clay. Calcination at 200 oC resulted in a more even distribution of TiO2 than calcination at 300 oC and 400 oC temperatures