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Batteries 2018, 4(2), 25; https://doi.org/10.3390/batteries4020025

The Electrochemical Sodiation of Sb Investigated by Operando X-ray Absorption and 121Sb Mössbauer Spectroscopy: What Does One Really Learn?

1
ICGM, Université de Montpellier, CNRS, 34095 Montpellier, France
2
Dutch-Belgian (DUBBLE), ESRF-The European Synchrotron, 38043 Grenoble, France
3
Faculty of Applied Sciences, Delft University of Technology, 2600 AA Delft, The Netherlands
4
Alistore European Research Institute, Université de Picardie Jules Verne, 80039 Amiens, France
5
GreenMat, CESAM, Institute of Chemistry B6, University of Liège, 4000 Liège, Belgium
6
Synchrotron Soleil, Saint-Aubin, 91192 Gif-sur-Yvette, France
7
Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37813, USA
8
Reseau sur le Stockage Electrochimique de l’Energie (RS2E), CNRS, 80039 Amiens, France
*
Author to whom correspondence should be addressed.
Received: 4 May 2018 / Revised: 24 May 2018 / Accepted: 28 May 2018 / Published: 30 May 2018
(This article belongs to the Special Issue Sodium-Ion Battery: Materials and Devices)
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Abstract

In this study, we want to highlight the assets and restrictions of X-ray absorption spectroscopy (XAS) and Mössbauer spectroscopy for investigating the mechanism of the electrochemical reaction of antimony electrode materials vs. Na. For this, operando XAS was carried out during the first one and a half cycles, and the whole set of measured data was analysed using a statistical-chemometric approach, while low temperature Mössbauer spectroscopy measurements were carried out ex situ on selected samples stopped at different points of the electrochemical reaction. Complementary ab initio calculations were performed to support the experimental findings. Both techniques show that, upon the first sodiation, most Sb reacts with Na to form disordered Na 3 Sb. This step is accompanied by the formation of amorphous Sb as an intermediate. Upon inversion of the current Na 3 Sb is desodiated and an amorphous Sb phase, distinct from the pristine bulk Sb state, is gradually formed. However, both XAS and Mössbauer spectroscopy were unable to spot the formation of intermediate Na x Sb phases, which were evinced in previous works by operando Pair Distribution Function analyses. The results shown here clearly assign such failure to the intrinsic inability of both techniques to identify these intermediates. View Full-Text
Keywords: X-ray absorption spectroscopy; Mössbauer spectroscopy; DFT calculations; chemometrics; MCR-ALS; Na-ion batteries; alloy reaction; Sb X-ray absorption spectroscopy; Mössbauer spectroscopy; DFT calculations; chemometrics; MCR-ALS; Na-ion batteries; alloy reaction; Sb
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Darwiche, A.; Fehse, M.; Mahmoud, A.; La Fontaine, C.; Fraisse, B.; Hermann, R.P.; Doublet, M.-L.; Monconduit, L.; Sougrati, M.T.; Ben Yahia, M.; Stievano, L. The Electrochemical Sodiation of Sb Investigated by Operando X-ray Absorption and 121Sb Mössbauer Spectroscopy: What Does One Really Learn? Batteries 2018, 4, 25.

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