The defect specific technique of positron–electron annihilation is utilized in an appropriate electrochemical cell for operando monitoring of vacancy-type defect formation which occurs in battery electrodes upon charging, using the cathode material LiNi1/3Mn1/3Co1/3O2 as a case study. The variation of the positron lifetime with charging-induced Li ion extraction indicates the formation of divacancies and vacancy agglomerates in a progressive amount as well as a reordering of vacancy agglomerates to one-dimensional vacancy chains at the end of charging. A remarkable correlation of the charging-induced variation of the positron lifetime with that of Li ion diffusion data in the literature has been found.

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