Nanoparticles of Li-Ni, Li-(Ni,Cu) and Li-Cr layered oxides, with potential applications as cathode materials in lithium batteries, have been prepared by solid-state reaction and sol-gel method. The combination of structural analysis and magnetic characterization allowed the clear identification of the phases present in the synthesized nanoparticles. The main component of Li-Ni oxide nanoparticles is the electrochemically active and ferrimagnetic phase Li1-zNi1+zO2, whereas those of Li-Cr oxide are the antiferromagnetic phases LiCrO2 and Cr2O3. A small substitution of Cu for Ni in Li-Ni oxide determines the formation of nanoparticles in which the main phase is the antiferromagnetic phase Li1-zNi1+zO2. Operation tests in lithium batteries and post-mortem analysis, aimed at assessing the potential of metal oxide nanoparticles as cathode materials, were performed on all samples.