Nanosized LiNi1/3Co1/3Al1/3O2 with an alpha-NaFeO2 structure has been successfully synthesized via a water-in-oil microemulsion method. Well-crystallized LiNi1/3Co1/3Al1/3O2 was obtained after heating at 800 degrees C for merely 3 h. The particle size of the microemulsion-derived powders was around 30 nm. The results of electrochemical analysis revealed that the synthesized powders exhibited higher discharge capacity at elevated temperatures than at room temperature. The Co3+/Co4+ redox reactions are considered to play an important role in the discharge capacity and capacity retention of synthesized LiNi1/3Co1/3Al1/3O2. (c) 2005 Elsevier B.V. All rights reserved.