A novel type of nanostructured LiMn2O4 microsphere was successfully synthesized by wet ball milling combined with high-temperature calcinations. The prepared materials were characterized by XRD, SEM, BET surface area measurement, electrochemical galvanostatic cycling tests, EIS, and XRF. The results show that the well-shaped microspheres with a diameter of approximately 0.5–2 μm are composed of reorganized nanoparticles. The LiMn2O4 microspheres have a high tap density of 2.8 g cm−3, and as electrodes, these micro/nanostructured spheres show excellent rate capability and cycle stability, resulting in a high volumetric energy density, even at elevated temperature. These materials are promising for power battery applications.
