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Ni-rich layered oxides, i.e., LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) and LiNiO 2 (LNO), were prepared using the two-step calcination procedure. The samples obtained at different calcination temperatures (750-950 °C for the NMC622 and 650-850 °C for the LNO cathode materials) were characterized using nitrogen physisorption, PXRD, SEM and DLS methods. The correlation of the calcination temperature, structural properties and electrochemical performance of the studied Ni-rich layered cathode materials was thoroughly investigated and discussed. It was determined that the optimal calcination temperature is dependent on the chemical composition of the cathode materials. With increasing nickel content, the optimal calcination temperature shifts towards lower temperatures. The NMC-900 calcined at 900 °C and the LNO-700 calcined at 700 °C showed the most favorable electrochemical performances. Despite their well-ordered structure, the materials calcined at higher temperatures were characterized by a stronger sintering effect, adverse particle growth, and higher Ni 2+ /Li + cation mixing, thus deteriorating their electrochemical properties. The importance of a careful selection of the heat treatment (calcination) temperature for each individual cathode material was emphasized., Competing Interests: The authors declare no conflict of interest.