LiCoO 2 and LiMn 2 O 4 compounds were synthesized using two different methods, viz., low-temperatureaided hydrothermal and high-temperature-assisted coprecipitation method. Keeping the reaction parameters such as type of precursors chosen and the medium of reaction as same for both the hydrothermal and co-precipitation methods, the effect of temperature in producing LiCoO 2 and LiMn 2 O 4 with varying physical as well as electrochemical properties has been studied. As expected, the effect of lowtemperature-involved hydrothermal method rendered finer particles of nanocrystalline nature with minimum strain, and the high-temperature synthesis of co-precipitation method produced slightly enhanced particle size with an increased strain value. The effect of size-grown particles resulting from co-precipitation method exhibited inferior electrochemical properties such as increasing resistance of the cell upon cycling and a significant decline in capacity behavior, irrespective of LiCoO 2 or LiMn 2 O 4 cathodes. On the other hand, hydrothermal synthesis of LiCoO 2 and LiMn 2 O 4 has exhibited acceptable specific capacity with an admissible capacity fade behavior and negligible internal resistance of the cell, thus qualifying the same as better-performing cathodes. Hence, the effect of low temperature in producing LiCoO 2 and LiMn 2 O 4 cathodes with facile intercalation and de-intercalation of lithium is demonstrated.