Products of thermal decomposition of lithium permanganate LiMnO 4 ·3H 2 O, which are formed in temperature range 160-900°C, have been characterized by powder XRD and chemical analysis. It has been found that the decomposition of the permanganate results in the formation of an equimolar mixture of manganate(IV) Li 2 MnO 3 and stoichiometric spinel LiMn 2 O 4 at the temperatures above 700°C. Intermediate products with spinel structure are formed at lower temperatures with oxidation number of manganese being between +4 and +3.5. These compounds can be related to overstoichiometric spinel phases with general formula Li a [Mn (1+0.5a) Li (1−0.5a) ]O 4 , where a>1. Electrochemical properties of these intermediates with regard to the reaction of Li extraction were investigated. The data are of interest for the development of synthesis methods for mixed oxides containing lithium and manganese with lithium permanganate as the lithiating reagent.
The equilibrium phase composition has been studied in two (pseudo)binary cross-sections of the Li-Mn-CoO system at 800°C in ambient air atmosphere: I-LiMn 2-x Co x O n (0≤x≤2) and II-LiMn x Co 1-x O n (0≤x≤1). Section I contains a homogeneous spinel-structured phase in the composition range 0≤x≤1, with the lattice parameter decreasing with increasing Co content. The compositions become 2-phase for 1
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The synthesis method of lithiated d-metal oxides using molten formate mixtures as precursors has been developed and the isothermal (800°C) cross section of pseudo ternary Li-Mn-Co oxide system under ambient oxygen pressure has been investigated by XRD, 7 Li NMR, and galvanostatic electrochemical methods. Special attention has been paid to the compositions inside the quadrangle restricted by solid solutions LiCoO 2 -LiCo 0.85 Mn 0.15 O 2 with the layered structure of α-NaFeO 2 and solid solutions LiMn 2 O 4 -LiMnCoO 4 with the structure of spinel. It was found that, depending on the composition, three types of equilibrium phases could be formed: spinels Li[Li,Mn,Co] 2 O 4 with a part of Li atoms in octahedral sites, cation-deficit layered compounds Li 1 − δ [Co,Mn]O 2 , and Li 2 MnO 3 . Areas of (co)existence of these phases were plotted on the composition plane of the pseudo-ternary Li-Mn-Co system. Electrochemical properties of the compositions inside the quadrangle LiCoO 2 -LiCo 0.85 Mn 0.15 O 2 -LiMn 2 O 4 -LiMnCoO 4 are determined by the content and average oxidation number of Mn atoms, which is higher than in the normal spinels Li[Mn, Co] 2 O 4 . Thus, the specific capacities of the polyphase compositions are lower in comparison with the binary solid solutions Li[Mn,Co] 2 O 4 or pure LiCoO 2 .
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