One of the major challenges in developing high-performance Li-O batteries is to understand the Li O formation and decomposition during battery cycling. In this study, this issue was investigated by synchrotron radiation powder X-ray diffraction. The evolution of Li O morphology and structure was observed under actual electrochemical conditions of battery operation. By quantitatively tracking Li O during discharge and charge, a two-step process was suggested for both growth and oxidation of Li O owing to different mechanisms during two stages of both oxygen reduction reaction and oxygen evolution reaction. From an observation of the anisotropic broadening of Li O in XRD patterns, it was inferred that disc-like Li O grains are formed rapidly in the first step of discharge. These grains can stack together so that they facilitate the nucleation and growth of toroidal Li O particles with a LiO -like surface, which could cause parasitic reactions and hinder the formation of Li O . During the charge process, Li O is firstly oxidized from the surface, followed by a delithiation process with a faster oxidation of the bulk by stripping the interlayer Li atoms to form an off-stoichiometric intermediate. This fundamental insight brings new information on the working mechanism of Li-O batteries.
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