Li0.55Na0.03Mn0.5Ni0.25Ti0.25O2was prepared via Na/Li ion exchange from Na0.7Mn0.5Ni0.25Ti0.25O2as a starting compound. Li0.55Na0.03Mn0.5Ni0.25Ti0.25O2is a layered rocksalt-type oxide with the O3 structure. The electrochemical lithium insertion/extraction properties of O3-Li0.55Na0.03Mn0.5Ni0.25Ti0.25O2exhibits a reversible capacity of approximately 190 mAh g-1in the voltage range between 2.0 and 4.8 V. The voltage profile consists of two plateaus around 4.0 and 3.0 V. The layered structure remains unchanged and does not transform to the spinel structure during cycling.