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Layered lithiated Co- and Ni-oxide powders and thin films with rhombohedral (R\({\bar 3}\)m) structure were prepared by a peroxo wet chemistry route from Li(I), Co(II) and Ni(II) acetate precursors and the addition of H2O2. XRD analysis revealed that xerogel films and powders possessed a typical layered structure. Layered (R\({\bar 3}\)m) Li0.99Co1.01O2 powder and Li0.97Co1.03O2 films were formed around 500°C, while Li0.93Ni1.07O2 powder and Li0.94Ni1.06O2 oxide films were prepared around 550°C. The stoichiometry of the oxide films and powders was dependent on the heat-treatment temperature. The structure of sols, gels, xerogels and thin films was established from XRD spectra and from the FT-IR spectra, confirming their layered structure.