The influence of mechanical activation (MA) and initial reagents on the synthesis, structure and electrochemical performance of LiNiO2, LiNi1-xAlxO2, LiNi1-yСоyO2 and LiNi1-y-xCoyAlxO2 (y = 0.2; 0.3; x = 0.05) was studied. NiO, α- and β-modification of hydroxides Ni(OH)2 и Ni1-y, as well as LiOH и Li2CO3 were used.