LiNi0.5Mn1.5O4 was prepared through a solid-state reaction using various Ni precursors. The effect of precursors on the electrochemical performance of LiNi0.5Mn1.5O4 was investigated. LiNi0.5Mn1.5O4 made from Ni(NO3)2·6H2O shows the best charge–discharge performance. The reversible capacity of LiNi0.5Mn1.5O4 is about 145mAhg−1 and remained 143mAhg−1 after 10 cycles at 3.0–5.0V. The XRD results showed that the precursors and the dispersion methods had significant effect on their phase purity. Pure spinel phase can be obtained with high energy ball-milling method and Ni(NO3)2·6H2O as precursor. Trace amount of NiO and Li2MnO3 phase were detected in LiNi0.5Mn1.5O4 with manual-mixture method and using Ni(CH3COO)2·6H2O, NiO and Ni2O3 as precursors.