Mixtures of BaCO 3 –ZnO–TiO 2 were mechanically activated using high-energy planetary ball mill during 20, 40 and 80min. As the time of mechanical activation increased, the decrease in particle size was observed. The effect of milling on microstructure was investigated by scanning electron microscopy, as well. Sintering process was performed in air at 1100 and 1200°C for 2h. Various phases are present within mixtures sintered at 1100 and 1200°C, and almost pure BaZn 2 Ti 4 O 11 phase was obtained after 80min of milling and sintering at 1200°C for 2h.