This paper describes the glycine-nitrate-based solution combustion synthesis of LiNi0.5Mn1.5O4 as a high-voltage cathode material for lithium-ion batteries. The morphology, size, and crystallinity of the products were dependent on the synthesis conditions like glycine amount and calcination temperature and duration, as investigated in particular by X-ray diffraction and scanning electron microscopy, which likewise influenced their electrochemical properties. The electrochemical performance was characterized by galvanostatic charge-discharge cycling. The product obtained at a glycine/nitrate ratio of 1, which was calcined at 800°C for 24h, indicated the best charge-discharge cycling performance. The sample showed an initial discharge capacity of 124.9 mAh/g and could retained 97.20% of the capacity after 50 cycles at a charge-discharge rate of 1C. The sample also exhibited a good high-rate capability, indicating a high discharge capacity of 98 mAh/g at a rate of 10C.