Layered Li-Ni-Mn-O compounds were successfully synthesized by an emulsion drying method, in which the emulsion makes it possible to intermix cations in atomic scale and therefore leads to homogeneous and fine oxide products. The as-synthesized powders were crystallized into a well-ordered alpha-NaFeO2 (R (3) over bar m) structure. The calculated lattice parameters varied by changing the lithium amounts. The lattice parameters of Li1.13Ni0.5Mn0.5O2+z Showed smaller a- and c-axes comparing to those of the LiNi0.5Mn0.5O2, whereas the c/a ratio remained constant for Li1+xNi0.5Mn0.5O2+z (0 less than or equal to x less than or equal to 0.13) compounds. Comparing to LiNi0.5Mn0.5O2 and Li1+xNi0.5Mn0.5O2+z electrodes, the delivered capacity for the Li1.13Ni0.5Mn0.5O2+z was much higher that that of the LiNi0.5Mn0.5O2. The lithium excess Li1+xNi0.5Mn0.5 O2+z sample exhibited very stable cyclability with high capacity of about 175 mA h (g oxide)(-1) after the 50th cycle at 25 degreesC (I= 20 mA g(-1)) and 50 degreesC (75.5 mA g(-1)), which indicates that structural stability of the lithium excess Li1-xNi0.5Mn0.5O2+z is superior to that of the stoichiometric LiNi0.5Mn0.5O2. (C) 2003 Elsevier B.V. All rights reserved.