Journal
JOURNAL OF PHYSICS AND CHEMISTRY OF SOLIDS
Volume 148, Issue -, Pages -Publisher
PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.jpcs.2020.109732
Keywords
Ni-rich NCM; LixNi0.88Co0.08Mn0.04O2; Spectromicroscopy; Transition metal L3-edge; O K-Edge; Local averaged oxidation state
Funding
- Basic Science Research Program through the National Research Foundation of Korea - Korea government Ministry of Science, ICT and Future Planning (MSIP) [NRF-2015R1A5A1009962]
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In this study, primary particle samples of LixNi0.88Co0.08Mn0.04O2 lithium-ion battery cathode material were prepared using a sonication method. The oxidation states of Ni, Co, and Mn atoms were estimated and showed variations within different regions of the particles. Mn and Co were found to have average oxidation states around 4+ and 3+ respectively, while Ni exhibited varying oxidation states ranging from 2.5+ in pristine samples to 3.0-3.2+ in charged samples.
Pristine and charged (4.35 Vat 1st cycle charge) primary particle samples of LixNi0.88Co0.08Mn0.04O2 lithium-ion battery (LIB) cathode material have been prepared by a sonication method. The local oxidation states of Ni, Co, and Mn atoms within these samples have been estimated from the local Ni L-3-edge, Co L-3-edge, Mn L-3-edge, and O K-edge spectra measured by scanning transmission X-ray microscopy (STXM) with around 30 nm lateral space resolution. The average oxidation state of the Mn atoms has been estimated as about 4+, and that of the Co atoms as about 3+, over the whole particle area for both the pristine and charged samples. For the Ni atoms, with space integration over the particles, the average oxidation state was estimated as about 2.5+ for the pristine sample and 3.0-3.2+ for the charged sample. The space-resolved spectral features indicate that, for the pristine sample, the average oxidation state of the Ni atoms is 2.2-2.5+ in the outside (surface) area, and 2.9-3.0+ in the inside (bulk) area of the particles. For the charged particles, the average oxidation state of the Ni atoms ranged from about 2.4+ to 3.4+, although in most areas it was 3.0+ or higher. The O K-edge spectra, correspondingly, showed different features according to the sample and the location within the particles. The O K-edge spectral feature changes have been interpreted with reference to the hybridization between the 2p orbitals of O and the 3d orbitals of the Ni4+ -Ni2+, Co3+, and Mn4+ cations.
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