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Lithium manganese spinels tend to aggregate upon annealing and do not allow for attaining high discharge rates when used as cathodes in lithium-ion batteries. To obtain spinel samples of lower aggregation and better highrate properties, precursors synthesized by means of a citric acid-aided route are suggested to be pyrolyzed in an inert atmosphere, instead of pyrolysis in air. The synthesis of nanosized Li[Li 0.033 Mn 1.967 ]O 4 is described, and its characteristics including X-ray diffraction, scanning electron microscopy, and porosity, as well as electrochemical test results are presented. The particle size of the materials obtained is smaller, the degree of aggregation is lower, and high-rate properties are better than for analogues pyrolyzed in air. In particular, sample Li||Li[Li 0.033 Mn 1.967 ]O 4 cells deliver *60 mAh g -1 at the current loads of 4,000 mA g -1

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