Lithium-ion batteries (LIBs) are widely recognised as essential parts of portable electronics, electric vehicles, and grid storage. As such, LIBs have considerable potential to contribute to our modern society, especially as a fundamental component in the development of a sustainable energy system [1]. Despite their success, many fundamental questions in the context of LIBs still puzzle researchers today. These involve interfaces and interphases [2]. For example, the structure and speciation of the potential- and surface-dependent electric double layer (EDL) (especially in advanced concentrated electrolytes) is currently not well understood. Relatedly, basic knowledge of multiple properties of the solid electrolyte interphase (SEI), a passivation layer formed on anode surfaces by electrolyte reduction products, needs to be unravelled to predict electrolyte behaviour as well as cell kinetics and lifetime [3]. To understand the structural properties of these solid-liquid interfaces and interphases, X-ray reflectivity (XRR) is a powerful method that employs model electrodes such as single crystals or thin films [4,5]. XRR provides surface sensitivity with sub-Ångström resolution, is non-destructive, allows probing buried nanoscale layers, and, importantly, can be carried out in operando modality [3]. One of the main challenges of XRR is that it is typically employed for a single electrochemical cell at a given time, and a single experiment takes on the order of several hours up to one day. In this scenario, the experiments are not photon-limited and continuous data collection is not necessary to obtain meaningful results because changes are slow towards later stages of the experiment (even though initial processes occur relatively fast). To overcome this limitation, we designed a high-throughput setup and corresponding experimental workflow, in which up to ten electrochemical cells can be measured via XRR and other surface-sensitive X-ray scattering methods (e.g., GISAXS and GIWAXS) quasi-simultaneously in an interleave fashion. We will present our novel experimental setup and first results.Literature:[1] G. Zubi, R. Dufo-López, M. Carvalho, & G. Pasaoglu,Renewable and Sustainable Energy Reviews, 89, 292-308, 2018.[2] K. Xu, Journal of Power Sources, 559, 232652, 2023.[3] C. Cao, H.-G. Steinrück, Encyclopedia of Solid-Liquid Interfaces, 391–416, Elsevier, 2024.[4] T. T. Fister, X. Hu, J. Esbenshade, ... & P. Fenter, Chemistry of Materials, 28(1), 47-54, 2016.[5] C. Cao, H.-G. Steinrück, B. Shyam, K. H. Stone, & M. F. Toney, Nano Letters, 16(12), 7394-7401, 2016.
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