LiNi0.5Mn1.5O4 powder was synthesized via sol–gel method and coated with ZnO in order to test the electrochemical cyclability of the material as a cathode for the secondary Li battery in the 5 V range at 55°C. The ZnO-coated LiNi0.5Mn1.5O4 powder nearly maintained its initial capacity of 137 mA h g−1 after 50 cycles whereas the uncoated powder was able to retain no more than 10% of the initial capacity after 30 cycles. TEM analysis of the cycled cathodes suggests that the formation of the graphitic surface phase, hindering the Li migration, may be responsible for the rapid capacity loss of the uncoated material while no such phase was observed on the surface of the ZnO coated LiNi0.5Mn1.5O4 powder.