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A structural relaxation study has been carried out on Lix(Ni0.874Co0.090Al0.036)O2 after the electrochemical lithium was extraction down to x = 0.12. These relaxation analyses have been carried out using X-ray diffraction coupled with the Rietveld analysis, assuming two phases (H2 and H3) and co-existence with R 3 ¯ m symmetry. The mole fraction of the H3 phase seemed not to vary largely during the relaxation time. As for the lattice constants, both H2 and H3 phases gradually increased the a-axis with the relaxation time. On the other hand, H2 and H3 phases increased and decreased the c-axis, respectively. The results are compared with that of previously reported Ni-rich NCA. [ABSTRACT FROM AUTHOR]