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Summary We systematically investigated the effects of Mo doping on the structure, morphology, and the electrochemical performance of Li (NixMnyCo1‐x‐y‐zMz)O2 (NMC) cathode materials for Li‐ion batteries. Layered NMC cathodes were synthesized with the ratio of 111, 622, and 226 via spray pyrolysis yielding submicron‐sized aggregates in the shape of hollow spherical particles. We performed X‐ray diffraction analyses to determine the present phases and the ordering in structure. X‐ray diffraction pattern of Mo‐doped 111, 226, and 622 cathodes showed well‐defined [006]/[102] and [108]/[110] doublets, indicating the layered structure, and good hexagonal ordering. Galvanostatic charge/discharge and electrical impedance spectroscopy measurements were carried out to reveal the effect of Mo doping on the electrochemical performance of the cathodes. Charge/discharge measurements after 20 cycles indicated that the Mo‐doped 111 and 622 NMC cathodes performed a capacity retention of 80% and 81% respectively. Present findings reveal the stabilization effect of Mo in layered NMC structure, especially in the case of Ni‐rich NMC cathodes.