We present the synthesis, characterization, and electrode behavior of LiNi 0.5 Mn 1.5 O 4 spinels prepared by the wet-chemical method via citrate precursors. The phase evolution was studied as a function of nickel substitution and upon intercalation and deintercalation of Li ions. Characterization methods include X-ray diffraction, SEM, Raman, Fourier transform infrared, superconducting quantum interference device, and electron spin resonance.