Bauxite deposits for production of alumina are lacking in Nigeria and there is an aluminium smelter plant in the country which requires alumina for its operation. Development of alternative alumina resource using clays that are abundant in the country is the focus of this paper. The thermal activation of Ibere clay from southeastern Nigeria for optimal leaching of alumina was investigated. The clay assayed 28.52% Al₂O₃ and 51.6% SiO₂, comprising mainly kaolinite mineral and quartz or free silica. The alumina locked up in the clay structure was rendered acid-soluble by thermal activation which transformed the clay from its crystalline nature to an amorphous, anhydrous phase or metakaolinite. The clay samples were heated at calcination temperatures of 500°C, 600°C, 700°C, 800°C, and 900°C at holding times of 30, 60, and 90 minutes. Uncalcined clay samples and samples calcined at 1000°C (holding for 60 minutes) were used in the control experiments. The result of leaching the clay calcines in 1 M hydrochloric acid solution at room temperature, showed that the clay calcines produced at 600°C (holding for 60 minutes) responded most to leaching. Samples calcined for 60 minutes also responded better than those held for 30 or 90 minutes. Based on activation energy studies, it was observed that calcines produced at 600°C (for 60 minutes) had both the highest leaching response (50.27% after 1 hour at leaching temperature of 100°C) and the lowest activation energy of 24.26 kJ/mol. It is concluded therefore that Ibere kaolinite clay should be best calcined for alumina dissolution by heating up to 600°C and holding for 60 minutes at that temperature. The clay deposit has potential for use as alternative resource for alumina production in Nigeria where bauxite is scarce.