Multimodal and in-situ Chemical Imaging of Critical Surfaces and Interfaces in Advanced Batteries

Abstract

Interfaces play a critical role in the properties and lifetime of current generation and advanced batteries. However, detailed characterization of the critical interfaces during battery operation which can enable performance improvements and improved design has been a significant challenge requiring innovative technique development and creative experiments. This paper describes ways that information from a range of microscopy, spectroscopy, and spectrometry tools can be used to address important challenges associated with energy storage science and technology, in particular the development of advanced batteries for consumer use, transportation, and renewable storage. Expanding the types of measurements that can be made on operational model batteries has significantly expanded the type and quality of information that can be obtained. This paper first shows examples of approaches being used to collect in situ transmission electron microscopy (TEM), secondary ion mass spectrometry and x-ray photoelectron spectroscopy (XPS) data.The final section of the paper briefly shows two examples: the use of in situ XPS to examine solid-electrolyte interphase layers and a multimodal chemical imaging approach, including scanning TEM, atom probe tomography, scanning transmission x-ray microscopy, and x-ray adsorption near edge spectroscopy to understand the nanostructure and improve the performance of layered lithium transition metal oxide cathodes.

Practical guides for x-ray photoelectron spectroscopy: First steps in planning, conducting, and reporting XPS measurements

“…The nature of sample handling, the time between preparation and analysis, and environmental factors can all impact an analysis. 49, 92, 93 Some samples require handling in a glove box, 92, 94 some may require heating in vacuum to get to the desired state, 92, 95 while others may need cooling to avoid sample alteration or probe damage. 6, 96 XPS data can also be collected in a variety of modes, each with relevant protocols and considerations, 11 including survey (wide scan) spectra, selected-region high energy resolution (narrow scan) spectra, imaging, 88, 97 angle resolved 98 and sometimes the use of ion sputtering for depth profiling.…”