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1.
Structural and chemical analysis of hard carbon negative electrode for Na-ion battery with X-ray Raman scattering and solid-state NMR spectroscopy
Ava Rajh, Matej Gabrijelčič, Blaž Tratnik, Klemen Bučar, Iztok Arčon, Marko Petric, Robert Dominko, Alen Vižintin, Matjaž Kavčič, izvirni znanstveni članek

Opis: This study explores the structural changes of hard carbon (HC) negative electrodes in sodium-ion batteries induced by insertion of Na ions during sodiation. X-ray Raman spectroscopy (XRS) was used to record both C and Na K-edge absorption spectra from bulk HC anodes carbonized at different temperatures and at several points during sodiation and desodiation. Comparing the [pi]*/[sigma]* regions in the C K-edge spectra sp2/sp3 hybridization ratio of material was determined. Higher carbonization temperatures led to increased order in graphitic structure and shorter bond lengths. Sodiation caused a decrease in graphitic layer order due to inserted Na ions. Complementary operando solid state 23Na nuclear magnetic resonance (ssNMR) studies confirmed the structural changes, while showing pore filling mechanism, which is not observed in ex situ measurements, primarily at higher carbonization temperatures. XRS analysis of Na K-edge spectra revealed systematic variations in the solid electrolyte interface (SEI) composition during cycling. Changes in XRS spectra were attributed to both SEI composition alterations, accompanied by the insertion/adsorption of Na ions at defect sites within the carbon structure.
Ključne besede: hard carbon, RIXS, carbon XANES, EXAFS, NMR, Na battery
Objavljeno v RUNG: 10.09.2024; Ogledov: 778; Prenosov: 1
.pdf Celotno besedilo (7,76 MB)
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2.
Study of Li-S batteries by S K-edge RIXS spectroscopy
Matjaž Kavčič, Matjaž Žitnik, Klemen Bučar, Marko Petrič, Iztok Arčon, Robert Dominko, Alen Vižintin, 2016, objavljeni povzetek znanstvenega prispevka na konferenci

Opis: Li-S batteries are considered as one of the most promising candidates for future batteries in applications where high energy density is required [1]. Despite that the general principle of operation is known for a long time [2], the lack of detailed understanding of relevant operation mechanisms has so far prevented their extensive use. A Li-S battery is composed of a lithium metal anode and a sulfur based cathode, separated by a porous separator wetted with electrolyte. During the battery cycle the reduction and oxidation of S to Li2S and back proceeds through a complicated equilibrium mixture of compounds that are typically dissolved in the electrolyte in the form of long and short chain polysulfides. In order to improve our understanding of polysulfide formation and its interactions within electrode, which are essential to achieve the long term cycling stability, development and application of new analytical tools is required. In this work sulfur K-edge resonant X-ray emission (RXES) measurements were performed on the Li-S battery in operando mode. The experiment was performed at the ID26 beamline at ESRF using the Johansson type tender x-ray emission spectrometer [3]. Full K-L RIXS maps were recorded on a set of chemically prepared Li2Sx sample standards characterized by different Li:S stoichiometric ratio, followed by the operando measurements on Li-S battery. Using the spectra recorded on Li2Sx standards two excitation energies were chosen and RXES spectra from the back of the battery cathode were sequentially acquired during one discharge cycle (C20). The relative amounts of each sulfur compound in the cathode during the discharge cycle were determined from the linear combination fit using measured reference standard spectra. Because of resonant excitation conditions the sensitivity for the polysulfide detection was significantly enhanced. Our work sets up S K-edge RIXS spectroscopy as an important analytical tool to study the mechanism of Li-polysulfide formation in the cathode and their interaction with the host matrix and electrolyte.
Ključne besede: RIXS, RXES, Li-S battery, operando, Sulphur K-edge XANES, Lithium polysulphides, Li2S
Objavljeno v RUNG: 28.06.2016; Ogledov: 6616; Prenosov: 0
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