Operando laboratory XAS on battery materials using the DANOISE cell in a von H'amos spectrometer.

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Bibliographic Details
Title: Operando laboratory XAS on battery materials using the DANOISE cell in a von H'amos spectrometer.
Authors: Praetz, Sebastian1 sebastian.praetz@tu-berlin.de, Johansen, Morten2, Kober, Delf3, Tesic, Marko1, Schlesiger, Christopher1, Ravnsbæk, Dorthe Bomholdt2, Kanngießer, Birgit1
Source: JAAS (Journal of Analytical Atomic Spectrometry). Sep2025, Vol. 40 Issue 9, p2447-2461. 15p.
Subjects: X-ray absorption near edge structure, Lithium-ion batteries, Storage batteries, Electrodes, X-ray spectrometers, Electrode testing, X-ray absorption spectra
Abstract: This work presents laboratory-based operando X-ray absorption spectroscopy (XAS) measurements on electrodes for rechargeable batteries. Using the "Developed in Aarhus: New Operando In-house Scattering Electrochemical" (DANOISE) cell, operando XAS measurements were performed with two von H'amos spectrometers, optimized for X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). Selected battery electrodes, including commercial LiFePO4 (LFP) for Liion batteries and layered transition metal oxides, NaxTMO2 (TM = Fe, Mn), electrodes for Na-ion batteries, were measured to present a proof of principal for the applicability of these spectrometers in battery research. The von H'amos spectrometers used in this study offer a high efficiency and the ability to measure a large spectral bandwidth (up to 1500 eV beyond the edge). Fe K-edge XANES measurements of LFP with an acquisition time of 15 minutes per spectrum successfully captured the transition of Fe species to FePO4 during cycling. Additionally, Mn K-edge XANES measurements on Naion battery materials highlight the challenges associated with Na-ion batteries, particularly due to their higher absorption compared to Li-ion counterparts. Nevertheless, the Mn K-edge was successfully measured, allowing for oxidation state determination in the material. Fe K-edge EXAFS measurements on Na-ion battery materials revealed the transition of Fe species during charging, within an acquisition time of 15 to 25 minutes. [ABSTRACT FROM AUTHOR]
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Database: Engineering Source
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Abstract:This work presents laboratory-based operando X-ray absorption spectroscopy (XAS) measurements on electrodes for rechargeable batteries. Using the "Developed in Aarhus: New Operando In-house Scattering Electrochemical" (DANOISE) cell, operando XAS measurements were performed with two von H'amos spectrometers, optimized for X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). Selected battery electrodes, including commercial LiFePO4 (LFP) for Liion batteries and layered transition metal oxides, NaxTMO2 (TM = Fe, Mn), electrodes for Na-ion batteries, were measured to present a proof of principal for the applicability of these spectrometers in battery research. The von H'amos spectrometers used in this study offer a high efficiency and the ability to measure a large spectral bandwidth (up to 1500 eV beyond the edge). Fe K-edge XANES measurements of LFP with an acquisition time of 15 minutes per spectrum successfully captured the transition of Fe species to FePO4 during cycling. Additionally, Mn K-edge XANES measurements on Naion battery materials highlight the challenges associated with Na-ion batteries, particularly due to their higher absorption compared to Li-ion counterparts. Nevertheless, the Mn K-edge was successfully measured, allowing for oxidation state determination in the material. Fe K-edge EXAFS measurements on Na-ion battery materials revealed the transition of Fe species during charging, within an acquisition time of 15 to 25 minutes. [ABSTRACT FROM AUTHOR]
ISSN:02679477
DOI:10.1039/d5ja00155b