We have synthesized LiMn 2−x Fe x O 4 (x = 0, 0.25, and 0.50) cathode materials for applications in Li ion rechargeable batteries via sol-gel method. We studied thermal characteristics of as synthesized materials using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). In order to optimize the synthesis conditions, we studied X-ray diffraction (XRD) of synthesized cathode materials at various temperatures, based on the transitions obtained from DSC/TGA. The XRD results can be co-related to the thermal behavior of the synthesized cathode materials and the synthesis conditions optimized.
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