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We report herein on the synthesis of “layered-layered” integrated xLi2MnO3⋅(1−x)LiMn1/3Ni1/3Co1/3normalO2 materials ( x=0.3 , 0.5, and 0.7) using the self-combustion reaction in solutions containing metal nitrates and sucrose. The nanoparticles of these materials were obtained by further annealing of the as-prepared product in air at 700°C for 1 h and submicrometric particles were obtained by further annealing at 900°C for 22 h. The effect of composition on the electrochemical performance was explored in this work. By a rigorous study with high resolution transmission electron microscopy (HRTEM), it became clear that the syntheses with the above stoichiometries produce two-phase materials comprising nanodomains of both rhombohedral LiNiO2 -like and monoclinic Li2MnO3 structures, which are closely integrated and interconnected with one another at the atomic level. Stable reversible capacities ∼220mAh/g were obtained with composite electrodes containing submicrometer particles of 0.5Li2MnO3⋅0.5LiMn1/3Ni1/3Co1/3normalO2 . Structural aspects, activation of the monoclinic component, and stabilization mechanisms are thoroughly discussed using Raman spectroscopy, solid-state NMR, HRTEM, and X-ray diffraction (including Rietveld analysis) in conjunction with electrochemical measurements. This work provides a further indication that this family of integrated compounds contains the most promising cathode materials for high energy density Li-ion batteries.

We report on a rigorous comparative study of nano-and microparticles of LiMn 1.5 Ni 0.5 O 4 spinel as cathode materials for Li-ion batteries. The stability of these materials in LiPF 6 /alkyl carbonate solutions in temperatures up to 70°C was explored. Capacity, cycling, rate capabilities, and impedance behavior were also studied. The methods included X-ray diffraction, Raman, X-ray photelectron, Fourier transform infrared, and electron paramagnetic resonance spectroscopies, and electron microscopy, in conjunction with standard electrochemical techniques: voltammetry, chronopotentiometry, and impedance spectroscopy. These materials show an impressive stability in solutions at elevated temperature. The use of nanomaterials was advantageous for obtaining a better rate capability of LiMn 1.5 Ni 0.5 O 4 electrodes. LiMn 1.5 Ni 0.5 O 4 particles develop a unique surface chemistry in solutions that passivates and protects them from detrimental interactions with solution species at elevated temperatures.

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