Crystalline calcium titanate was synthesized by mechanical activation of a mixture of CaO, obtained by then-nal treatment of CaCO3, and TiO2 in anatase or rutile form, in a planetary ball mill for 30, 60, 120 and 240 min.. The effect of milling on the solid-state reaction was followed by X-ray diffraction. Changes in powder size and morphology due to milling were determinate by SEM, while BET analysis was made to determine the specific surface area of powders. It was pointed out that the formation of calcium titanate was more easily achieved by mechanical activation synthesis of the mixture of calcium oxide and anatase modification of titanium oxide compared to the rutile form.