Well-crystallized Li4Mn5O12 powder has been prepared by heating a eutectic mixture of lithium acetate LiOAc and manganese nitrate Mn(NO3)2 at 700°C for 1-3 days in an O2 atmosphere. The Li and Mn content in the final products was determined from atomic absorption spectroscopy. The tetravalent manganese in the final product was found to be 95% based on the active oxygen content determined by KMnO4 titration. The structure of Li4Mn5O12 crystallites was refined by the Rietveld method from powder X-ray diffraction data as a cubic spinel, a = 8.1616(5) Å, space group Fd3̄m. Li4Mn5O12 crystallites are stable at temperatures up to 600°C in oxygen but decompose to spinel LiMn2O4 and monoclinic Li2MnO3 at temperatures higher than 530°C in N2.
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