Progressive chemical .delithiation of commercially available lithium cobalt oxide ([Formula: see text]) showed consecutive changes in the crystal properties. Rietveld refinement of high resolution X-ray and neutron diffraction revealed an increased lattice parameter c and a reduced lattice parameter a for chemically delithiated samples. Using electron microscopy we have also followed the changes in the texture of the samples towards what we have found is a critical layer stoichiometry of about [Formula: see text] with x=1/3 that causes the grains to exfoliate. The pattern of etches by delithiation suggests that unrelieved strain fields may produce chemical activity.
Keywords: Chemical delithiation; Intercalation; Li-ion Battery; Neutron diffraction; Rietveld refinement.