Abstract: We have found a new synthesizing method by means of studying the effects of the synthesizing conditions on the structures of LiNiO ₂ and LiAlO₂, respectively, and successfully synthesized Al doped LiN i_1xAl_xO₂(x=0~1.0) solids solutions. T he sintering experimental results show that the samples with low Al content must be synthesized in the oxygen atmosphere. Al doping can not only inhibit the lithium deficiency but decrease the forming temperature of the products and their dependency on oxygen during synthesizing them. From XRD results we found out that all the samples crystallized in the α-NaFeO₂ structure. The lattice parameters change with incr easing Alcontentviz axis a is shortened, larger the c/a ratio is increased and crystal volume V₀ is decreased. These changes show that the syn thesized samples well crystallized in the layer structure.

Key words: structure of α-NaFeO₂ form, solid solution, formati on enthalpy