Electrochemical Na extraction/insertion of Na3V 2O2x(PO4)2F3-2 x

Paula Serras; Verónica Palomares; Javier Alonso; Neeraj Sharma; Juan Miguel López Del Amo; Pierre Kubiak; María Luisa Fdez-Gubieda; Teófilo Rojo

doi:10.1021/cm403679b

Electrochemical Na extraction/insertion of Na₃V ₂O_2x(PO₄)₂F_{3-2 x}

Paula Serras, Verónica Palomares, Javier Alonso, Neeraj Sharma, Juan Miguel López Del Amo, Pierre Kubiak, María Luisa Fdez-Gubieda, Teófilo Rojo

Research output: Contribution to journal › Article

70 Citations (Scopus)

Abstract

A mixed-valence V³⁺/V⁴⁺ composite material belonging to the Na₃V₂O_2x(PO₄)2F _3-2x/C family is synthesized and the electrochemical Na extraction/insertion mechanism is determined using a combination of high-resolution synchrotron X-ray diffraction (XRD) data, X-ray absorption spectroscopy (XAS), ²³Na and ¹⁹F solid state nuclear magnetic resonance (NMR), double titration (for the elucidation of the vanadium oxidation state), and electrochemical measurements. The vanadium oxidation state is found to be +3.8 for the as-prepared sample. Detailed analysis of the cathode structural evolution illustrated that the V⁴⁺/V⁵⁺ couple is active in this compound during electrochemical cycling between 2.8 V and 4.3 V. This study demonstrates how the sodium-ion extraction and insertion pathways in cathode materials can be followed (and verified) using several experimental techniques, especially when multiple potential oxidation states are present in the parent compound.

Original language	English
Pages (from-to)	4917-4925
Number of pages	9
Journal	Chemistry of Materials
Volume	25
Issue number	24
DOIs	https://doi.org/10.1021/cm403679b
Publication status	Published - 23 Dec 2013
Externally published	Yes

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Keywords

electrochemistry
mixed valence sodium vanadium fluorophosphate
sodium ion batteries
X-ray diffraction and X-ray absorption near edge structure

ASJC Scopus subject areas

Materials Chemistry
Chemical Engineering(all)
Chemistry(all)

Cite this

Serras, P., Palomares, V., Alonso, J., Sharma, N., López Del Amo, J. M., Kubiak, P., Fdez-Gubieda, M. L., & Rojo, T. (2013). Electrochemical Na extraction/insertion of Na₃V ₂O_2x(PO₄)₂F_{3-2 x} Chemistry of Materials, 25(24), 4917-4925. https://doi.org/10.1021/cm403679b

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abstract = "A mixed-valence V3+/V4+ composite material belonging to the Na3V2O2x(PO4)2F 3-2x/C family is synthesized and the electrochemical Na extraction/insertion mechanism is determined using a combination of high-resolution synchrotron X-ray diffraction (XRD) data, X-ray absorption spectroscopy (XAS), 23Na and 19F solid state nuclear magnetic resonance (NMR), double titration (for the elucidation of the vanadium oxidation state), and electrochemical measurements. The vanadium oxidation state is found to be +3.8 for the as-prepared sample. Detailed analysis of the cathode structural evolution illustrated that the V4+/V5+ couple is active in this compound during electrochemical cycling between 2.8 V and 4.3 V. This study demonstrates how the sodium-ion extraction and insertion pathways in cathode materials can be followed (and verified) using several experimental techniques, especially when multiple potential oxidation states are present in the parent compound.",

keywords = "electrochemistry, mixed valence sodium vanadium fluorophosphate, sodium ion batteries, X-ray diffraction and X-ray absorption near edge structure",

author = "Paula Serras and Ver{\'o}nica Palomares and Javier Alonso and Neeraj Sharma and {L{\'o}pez Del Amo}, {Juan Miguel} and Pierre Kubiak and Fdez-Gubieda, {Mar{\'i}a Luisa} and Te{\'o}filo Rojo",

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AU - Sharma, Neeraj

AU - López Del Amo, Juan Miguel

AU - Kubiak, Pierre

AU - Fdez-Gubieda, María Luisa

AU - Rojo, Teófilo

PY - 2013/12/23

Y1 - 2013/12/23

N2 - A mixed-valence V3+/V4+ composite material belonging to the Na3V2O2x(PO4)2F 3-2x/C family is synthesized and the electrochemical Na extraction/insertion mechanism is determined using a combination of high-resolution synchrotron X-ray diffraction (XRD) data, X-ray absorption spectroscopy (XAS), 23Na and 19F solid state nuclear magnetic resonance (NMR), double titration (for the elucidation of the vanadium oxidation state), and electrochemical measurements. The vanadium oxidation state is found to be +3.8 for the as-prepared sample. Detailed analysis of the cathode structural evolution illustrated that the V4+/V5+ couple is active in this compound during electrochemical cycling between 2.8 V and 4.3 V. This study demonstrates how the sodium-ion extraction and insertion pathways in cathode materials can be followed (and verified) using several experimental techniques, especially when multiple potential oxidation states are present in the parent compound.

AB - A mixed-valence V3+/V4+ composite material belonging to the Na3V2O2x(PO4)2F 3-2x/C family is synthesized and the electrochemical Na extraction/insertion mechanism is determined using a combination of high-resolution synchrotron X-ray diffraction (XRD) data, X-ray absorption spectroscopy (XAS), 23Na and 19F solid state nuclear magnetic resonance (NMR), double titration (for the elucidation of the vanadium oxidation state), and electrochemical measurements. The vanadium oxidation state is found to be +3.8 for the as-prepared sample. Detailed analysis of the cathode structural evolution illustrated that the V4+/V5+ couple is active in this compound during electrochemical cycling between 2.8 V and 4.3 V. This study demonstrates how the sodium-ion extraction and insertion pathways in cathode materials can be followed (and verified) using several experimental techniques, especially when multiple potential oxidation states are present in the parent compound.

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KW - sodium ion batteries

KW - X-ray diffraction and X-ray absorption near edge structure

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Access to Document

10.1021/cm403679b