Submicrometer-sized LiCoO2 powders (see Figure) for potential applications in energy-storage devices are prepared by calcination starting from an amorphous Li/Co salt of poly(acrylic acid). LiCoO2 powders with an average grain size of 200 nm are obtained. They exhibit a specific capacity of up to 180 mA h g(-1) if charged at 4.5 V vs. Li/Li+. The macromorphology of the precursor fixed by spray-drying is preserved in the agglomerate of the grains obtained after calcination.