Layered Na0.7[Ni0.05Mn0.95]O2 compounds have been synthesized by a sol-gel method, using glycolic acid as a chelating agent. Na0.7[Ni0.05Mn0.95]O2 precursors w ere used to prepare layered lithium manganese oxides by ion exchange for Na by Li, using LiBr in hexanol. Powder X-ray diffraction shows the layered Na0.7[Ni0.05Mn0.95]O2 has an O3 type structure, which exhibits a large reversible capacity of approximately 190 mA h g-1 in the 2.4-4.5 V range. Na0.7[Ni0.05Mn0.95]O2 powders undergo transformation to spinel during cycling.