Sulfur speciation in Li–S batteries determined by operando laboratory X-ray emission spectroscopyRajh, Ava (Avtor) Vižintin, Alen (Avtor) Hoszowska, Joanna (Avtor) Dominko, Robert (Avtor) Kavčič, Matjaž (Avtor) X-ray emission spectroscopylithium−sulfur batteriesoperando measurementsoxidation statevon Hamos spectrometerIn this work, operando sulfur X-ray emission measurements on a Li−S battery cathode were performed using a laboratory setup as an alternative to more common synchrotron radiation based absorption studies. Photoexcitation by an X-ray tube was used. Valence-to-core Kβ X-ray emission spectra were recorded with a wavelength dispersive crystal spectrometer in von Hamos geometry, providing excellent energy resolution and good detection efficiency. The setup was used to record ex situ S Kβ emission spectra from S cathodes from the Li−S battery and also under operando conditions. Average S oxidation state within the battery cathode during battery cycling was determined from the shape of the Kβ emission spectra. A more detailed S species characterization was performed by fitting a linear combination of previously measured laboratory synthesized standards to the measured spectra. Relative amounts of different S species in the cathode were determined during the cycling of the Li−S battery. The main advantage of X-ray emission spectroscopy is that it can be performed on concentrated samples with S loading comparable to a real battery. The approach shows great promise for routine laboratory analysis of electrochemical processes in Li−S batteries and other sulfur-based systems under operando conditions.20242024-12-12 13:07:12Članek v reviji165866UDK: 544.5/.6ISSN pri članku: 2574-0962DOI: 10.1021/acsaem.4c02330COBISS_ID: 218392579sl