Single phase LiMn2O4 spinel powders have been prepared by solution combustion synthesis at 400 and 500°C using nitrate-acetate mixture raw materials without any fuels. The effect of single or double calcination has been studied contrastively. The phase composition and micro morphology are investigated by X-ray diffraction (XRD) and scanning electric microscope (SEM). The XRD results indicate that single phase LiMn2O4 can be obtained by single calcination at 400°C and 500°C, but there is Mn2O3 impurity in the sample prepared by double calcination at 500°C. SEM investigation exhibits that the particle size increases with raising calcination temperature or double calcination. The electrochemical performance tests indicates that the initial capacity, cyclic performance and rate capability of the samples prepared by single calcination are better than these of the samples prepared by double calcination.