Spinel LiMn2O4 (Fd3m) is a material that can be applied as cathodes in rechargeable lithium-ion batteries. LiMn2O4 and doped LiMn1.9 Ti0.1-xSnxO4 (x = 0.005) powder were prepared by the sol-gel method (SG). The thermal decomposition behaviour of the precursor were studied by using Simultaneous Thermogravimetry Analysis (STA). The thermal decomposition process occurred in three stages. Based on the STA results, the samples were annealed at 700°C in air for 24h and the annealed samples were characterized by X-Ray diffraction (XRD) to confirm the phase and purity of the materials. © 2017 Author(s).