In this study, we prepared the (Li_1-xNa_x)CoO_2±z (0.0 < x < 0.8, z ± 0.3) system by solid- state reaction. This process has become reproducible. The synthesis of polycrystalline powders in the (Li_1-xNa_x)CoO_2±z (0.0 < x < 0.8, z ± 0.3) system with x = 0.0 (LC) , 0.2 (LC2), 0.4 (LC4), 0.6 (LC6) and 0.8 (LC8) was designed to obtained 2 g of sample, using the following reagents Li₂CO₃, Na₂CO₃, and Co₃O₄. Subsequent thermal treatment, appropriate to each compound, was sufficient to yield the pure phase.

By Differential Thermal Analysis we attribute the changes for the dehydration, and decomposition of the carbonates. In Thermogravimetric Analysis the changes of weight decrease the temperature and we point those changes with varying the structure. This last observation was carried out by X – ray diffraction powder (XRD) with temperature to corroborated that the changes of weight correspond to the changes of the unit cell. It is observed a rhombohedral structure PDF 50-0553 by XRD analysis at ambient temperature in LC and LC2 composition. In the others LC4, LC6 and LC8 compositions we observed the Co₃O₄ reagent. The particle size and morphology of the polycrystals were examined by Scanning Electron Microscopy and EDX.

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