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In this work, we investigate the structural modifications occurring at the bulk, subsurface, and surface scales of LixNiyMnzCo1–y–zO2 (NMC; y, z = 0.8, 0.1 and 0.4, 0.3, respectively) cathode materials during the initial charge/discharge. Various analytical tools, such as X-ray diffraction, selected-area electron diffraction, electron energy-loss spectroscopy, and high-resolution electron microscopy, are used to examine the structural properties of the NMC cathode materials at the three different scales. Cutoff voltages of 4.3 and 4.8 V are applied during the electrochemical tests as the normal and extreme conditions, respectively. The high-Ni content NMC cathode materials exhibit unusual behaviors, which deviate from the general redox reactions during the charge or discharge. The transition metal (TM) ions in the high-Ni content NMC cathode materials, which are mostly Ni ions, are reduced at 4.8 V, even though TMs are usually oxidized to maintain charge neutrality upon the removal of Li. It was found tha...

chemistry of materials

Investigating the Reversibility of Structural Modifications of LixNiyMnzCo1–y–zO2 Cathode Materials during Initial Charge/Discharge, at Multiple Length Scales