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The performances of lithium-ion batteries are set by the electrodes materialscapacity to exchange lithium ions and electrons faster and reversibly. To thisgoal Ni-rich layered metal oxides, especially LiNiO2, are attractive electrodecandidate to achieve both high voltage and capacities. Despite itsattractiveness, several drawbacks for its industrialization are related todifferent form of surface and bulk instabilities. These instabilities are dueto redox process involving the charge transfer between cations and anions.Therefore, a fundamental understanding based on further experimental evidenceis required to resolve of charge transfer between the cation and anion from thesurface to the bulk in LiNiO2. Herein, we resolve the role of nickel and oxygenin the charge compensation process in LixNiO2 electrodes from the extremesurface down to 30 nm by energy-dependent core-level HAXPES supported by abinitio simulation. We emphasize the central role of oxygen in the bulk chargecompensation mechanism from LiNiO2 to NiO2 due to the negative charge transferand bond/charge-disproportionation characters of LiNiO2. This bulk behavior isin turn responsible for surface deoxygenation and nickel reduction upondelithiation.

Depth-resolving the redox compensation mechanism in LixNiO2