LiNiO2 was prepared by reaction of stoichiometric amounts of thoroughly mixed LiOH· H2O and preoxidation nanometer scale Ni3O2(OH)4 powders in O2 at the temperature of 700℃ for 6h. The products were tested by XRD, XPS, SEM and electrochemistry methods. It was shown that product was LiNiO2 single phase, and the valence of nickel was + 3; the average size of it was 40nm; its initial charge specific capacity is 168mAh· g- 1 and the coulomb efficiency is 90% ; the second charge specific capacity is 160mAh· g- 1 and the coulomb efficiency is 96% .