The paper describes a new technique of molten salt synthesis (MSS) that is based on the direct oxidation of halide ions with molecular oxygen in thermally stable halide melts to prepare nanoparticles of complex oxides. Lithium cobaltate (LiCoO2) was chosen as a model compound for testing this method. Synthesis was achieved in LiCl–CoCl2 melts at 600 and 700 °C, respectively, under a dry-air atmosphere. Fourier transform infrared (FTIR) and Raman spectroscopies, x-ray diffraction (XRD), and transmission electron microscopy (TEM) were used to study the products obtained. The route suggested results in the formation of stoichiometric high-temperature (HT) LiCoO2 powders.