Correlative Confocal Raman and Scanning Probe Microscopy in the Ionically Active Particles of LiMn2O4 Cathodes
authors Alikin, D; Slautin, B; Abramov, A; Rosato, D; Shur, V; Tselev, A; Kholkin, A
nationality International
journal MATERIALS
author keywords low-frequency electrochemical strain microscopy; confocal Raman microscopy; scanning probe microscopy; lithium manganate; LiMn2O4; quantitative electrochemical strain microscopy; batteries; cathodes
keywords ATOMIC-FORCE MICROSCOPY; LITHIUM-ION DIFFUSION; THIN-FILM CATHODE; ELECTROCHEMICAL STRAIN; ACTIVATION-ENERGY; BATTERY CATHODES; NANOSCALE; TRANSPORT
abstract In this contribution, a correlative confocal Raman and scanning probe microscopy approach was implemented to find a relation between the composition, lithiation state, and functional electrochemical response in individual micro-scale particles of a LiMn2O4 spinel in a commercial Li battery cathode. Electrochemical strain microscopy (ESM) was implemented both at a low-frequency (3.5 kHz) and in a high-frequency range of excitation (above 400 kHz). It was shown that the high-frequency ESM has a significant cross-talk with topography due to a tip-sample electrostatic interaction, while the low-frequency ESM yields a response correlated with distributions of Li ions and electrochemically inactive phases revealed by the confocal Raman microscopy. Parasitic contributions into the electromechanical response from the local Joule heating and flexoelectric effect were considered as well and found to be negligible. It was concluded that the low-frequency ESM response directly corresponds to the confocal Raman microscopy data. The analysis implemented in this work is an important step towards the quantitative measurement of diffusion coefficients and ion concentration via strain-based scanning probe microscopy methods in a wide range of ionically active materials.
publisher MDPI
issn 1996-1944
year published 2019
volume 12
issue 9
digital object identifier (doi) 10.3390/ma12091416
web of science category Materials Science, Multidisciplinary
subject category Materials Science
unique article identifier WOS:000469757500057
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