Adaptation and improvement of an elemental mapping method for lithium ion battery electrodes and separators by means of laser ablation-inductively coupled plasma-mass spectrometry

Abstract

In this study, laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was applied to previously aged carbonaceous anodes from lithium ion batteries (LIBs). The electrodes were treated by cyclic aging in a lithium ion cell set-up with LiNiMnO (LNMO) cathodes and hard carbon (HC)/mesocarbon microbead (MCMB) anodes. An inhomogeneous transition metal deposition pattern could be induced by replacing the spacer in a standard coin cell set-up with a washer. The inhomogeneity pattern matched the dimension of the washer depicted by the hole in the center. These transition metal (TM) patterns were used to optimize higher lateral scanning speeds and frequencies on the spatial resolution of the mapping experiments using LA-ICP-MS. Higher scanning speeds had an observable influence on the resolution of the obtained image and an overall saving of 60% with regard to time and gas consumption could be achieved. Additionally, the optimized method was applied to the cathode and separator in order to visualize the distribution and deposition pattern, respectively.

Chromatographic Techniques in the Research Area of Lithium Ion Batteries: Current State-of-the-Art

“…Therefore, the analysis of the stoichiometry of the electrodes can reveal the loss of TMs due to the above-explained effects. While inductively coupled plasma-based methods are routinely used for this purpose, the addition of chromatographic methods can provide valuable information since certified reference materials are not available presently [59,[122][123][124][125].…”

Deciphering the lithium ion movement in lithium ion batteries: determination of the isotopic abundances of 6Li and 7Li

“…[30][31][32][33][34] For direct solid analysis, methods like glow discharge-mass spectrometry (GD-MS), laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), time of ight-secondary ion mass spectrometry (TOF-SIMS) and X-ray photoelectron spectroscopy (XPS). [35][36][37][38][39][40][41][42] Due to their capabilities of directly measuring the surface components, they represent promising approaches for analyzing new materials as well as the degradation of aged cells. Especially the GD-MS benets from unique traits such as a fast analysis time while maintaining a nanometric sputter-rate and the ability to perform an isotope analysis throughout the prole of an electrode.…”

Soft X-ray laser ablation for nano-scale chemical mapping microanalysis

“…As mentioned above, materials science is another domain potentially benetting from laser ablation for chemical pattern reconstruction. Harte et al 44 utilized laser ablation ICP-MS for the characterization of transition metal patterns in Li-ion batteries and carry out a parametric study of the optimum measurement conditions. A higher scanning speed has an observable inuence on the resolution of the obtained image and an overall saving of 60% with regard to time and gas consumption can be achieved.…”