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3. Original Layered OP4-(Li,Na)xCoO2 Phase: Insights on Its Structure, Electronic Structure, and Dynamics from Solid State NMR

Author

Gillian R. Goward, Marie Guignard, Yohan Biecher, Romain Berthelot, Dany Carlier, Danielle L. Smiley, Claude Delmas, François Fauth, Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Department of Chemistry & Chemical Biology, McMaster University [Hamilton, Ontario], European Synchrotron Radiation Facility (ESRF), Réseau sur le stockage électrochimique de l'énergie (RS2E), Université de Picardie Jules Verne (UPJV)-Institut de Chimie du CNRS (INC)-Aix Marseille Université (AMU)-Université de Pau et des Pays de l'Adour (UPPA)-Université de Nantes (UN)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS)-Sorbonne Université (SU)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC), Université de Nantes (UN)-Aix Marseille Université (AMU)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Université de Picardie Jules Verne (UPJV)-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Pau et des Pays de l'Adour (UPPA)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM), and Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Fermi contact interaction, Rietveld refinement, Chemistry, Ionic bonding, [CHIM.MATE]Chemical Sciences/Material chemistry, 02 engineering and technology, Electronic structure, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Inorganic Chemistry, Delocalized electron, Crystallography, Solid-state nuclear magnetic resonance, Magic angle spinning, Lamellar structure, Physical and Theoretical Chemistry, 0210 nano-technology
Abstract

International audience; The OP4-(Li/Na)xCoO2 phase is an unusual lamellar oxide with a 1:1 alternation between Li and Na interslab spaces. In order to probe the local structure, electronic structure, and dynamics, 7Li and 23Na magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy was performed in complementarity to X-ray diffraction and electronic and magnetic properties measurements. 7Li MAS NMR showed that NMR shifts result from two contributions: the Fermi contact and the Knight shifts due to the presence of both localized and delocalized electrons, which is really unusual. 7Li MAS NMR clearly shows several Li environments, indicating that, moreover, Co ions with different local electronic structures are formed, probably due to the arrangement of the Na+ ions in the next cationic layer. 23Na MAS NMR showed that some Na+ ions are located in the Li layer, which was not previously considered in the structural model. The Rietveld refinement of the synchrotron XRD led to the OP4-[Li0.42Na0.05]Na0.32CoO2 formula for the material. In addition, 7Li and 23Na MAS NMR spectroscopies provide information about the cationic mobility in the material: Whereas no exchange is observed for 7Li up to 450 K, the 23Na spectrum already reveals a single average signal at room temperature due to a much larger ionic mobility.

Published
2020
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4. Alkali-Glass Behavior in Honeycomb-Type Layered Li3–xNaxNi2SbO6 Solid Solution

Author

Emmanuelle Suard, Paula Sanz-Camacho, Yohan Biecher, Matthieu Saubanère, Coélio Vallée, Gwenaëlle Rousse, Bernard Fraisse, Dany Carlier, Romain Berthelot, Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM ICMMM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Centre National de la Recherche Scientifique (CNRS)-Université de Montpellier (UM)-Université Montpellier 1 (UM1)-Université Montpellier 2 - Sciences et Techniques (UM2)-Institut de Chimie du CNRS (INC), Réseau sur le stockage électrochimique de l'énergie (RS2E), Université de Picardie Jules Verne (UPJV)-Institut de Chimie du CNRS (INC)-Aix Marseille Université (AMU)-Université de Pau et des Pays de l'Adour (UPPA)-Université de Nantes (UN)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS)-Sorbonne Université (SU)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM), Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Institut Laue-Langevin (ILL), ILL, Chimie du solide et de l'énergie (CSE), Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS), ANR-10-LABX-0076,STORE-EX,Laboratory of excellency for electrochemical energy storage(2010), Institut Charles Gerhardt Montpellier - Institut de Chimie Moléculaire et des Matériaux de Montpellier (ICGM), Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Aix Marseille Université (AMU)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Université de Picardie Jules Verne (UPJV)-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Pau et des Pays de l'Adour (UPPA)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), and Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA)

Subjects
Diffraction, Layered oxides, solid-solution, 010405 organic chemistry, Neutron diffraction, Oxide, chemistry.chemical_element, honeycomb ordering, [CHIM.MATE]Chemical Sciences/Material chemistry, [CHIM.INOR]Chemical Sciences/Inorganic chemistry, 010402 general chemistry, Alkali metal, 01 natural sciences, alkali mixed occupancy, 0104 chemical sciences, Inorganic Chemistry, Crystallography, chemistry.chemical_compound, chemistry, Honeycomb, Lithium, Density functional theory, Physical and Theoretical Chemistry, Solid solution
Abstract

International audience; Layered oxide compositions Li3–xNaxNi2SbO6 have been prepared by solid-state synthesis. A complete solid solution is evidenced and characterized by X-ray and neutron diffraction as well as 7Li and 23Na solid-state nuclear magnetic resonance spectroscopy. The transition-metal layer is characterized by the classic honeycomb Ni2+/Sb5+ ordering, whereas a more uncommon randomly mixed occupancy of lithium and sodium is evidenced within the alkali interslab space. In situ X-ray diffraction and density functional theory calculations show that this alkali disordered feature is entropically driven. Fast cooling then appears as a synthesis root to confine bidimensional alkali glass within crystalline layered oxides.

Published
2019
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5. Original Layered OP4-(Li,Na)

Author

Yohan, Biecher, Danielle L, Smiley, Marie, Guignard, François, Fauth, Romain, Berthelot, Claude, Delmas, Gillian R, Goward, and Dany, Carlier

Abstract

The OP4-(Li/Na)

Published
2020

6. Alkali-Glass Behavior in Honeycomb-Type Layered Li

Author

Coélio, Vallée, Matthieu, Saubanère, Paula, Sanz-Camacho, Yohan, Biecher, Bernard, Fraisse, Emmanuelle, Suard, Gwenaëlle, Rousse, Dany, Carlier, and Romain, Berthelot

Abstract

Layered oxide compositions Li

Published
2019

7. Density functional theory-assisted 31P and 23Na magic-angle spinning nuclear magnetic resonance study of the Na3V2(PO4)2F3–Na3V2(PO4)2FO2 solid solution: unraveling Its local and electronic structures

Author

NGUYEN, Long H. B., SANZ-CAMACHO, Paula, BROUX, Thibault, OLCHOWKA, Jacob, MASQUELIER, Christian, CROGUENNEC, Laurence, CARLIER-LARREGARAY, Dany, Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire réactivité et chimie des solides - UMR CNRS 7314 (LRCS), Université de Picardie Jules Verne (UPJV)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Réseau sur le stockage électrochimique de l'énergie (RS2E), Université de Picardie Jules Verne (UPJV)-Institut de Chimie du CNRS (INC)-Aix Marseille Université (AMU)-Université de Pau et des Pays de l'Adour (UPPA)-Université de Nantes (UN)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS)-Sorbonne Université (SU)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM), Advanced Lithium Energy Storage Systems - ALISTORE-ERI (ALISTORE-ERI), Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), The authors acknowledge the French RS2E Network for the funding of L.H.B.N.’s Ph.D. thesis, the RS2E and Alistore-ERI networks for the funding of T.B.’s postdoctoral fellowship, and the financial support of Région Nouvelle Aquitaine of the French National Research Agency (STORE-EX Labex Project ANR-10-LABX-76-01 and SODIUM Descartes project ANR-13-DESC-0001-02) and of the European Union’s Horizon 2020 research and innovation program under the grant agreement no. 646433-NAIADES. The Mésocentre de Calcul Intensif Aquitain (MCIA) and the modeling center of ISM are acknowledged for computing facilities. The authors want to thank Yohan Biecher (ICMCB-CNRS) for his help with DMfit., ANR-13-DESC-0001,SODIUM,Batteries à ions sodium pour des robots télécommandés(2013), Université de Picardie Jules Verne (UPJV)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Aix Marseille Université (AMU)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Université de Picardie Jules Verne (UPJV)-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Pau et des Pays de l'Adour (UPPA)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), and Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA)

Subjects
first- principles DFT calculations, Na3V2(PO4)2F3, Fermi contact, structural distortion * Corresponding author: D Carlier (DanyCarlier@icmcbcnrsfr), electron spin transfer, solid-state NMR, [CHIM.MATE]Chemical Sciences/Material chemistry, Na3V2(PO4)2FO2
Abstract

International audience; The local and electronic structures of Na3V2(PO4)2F3–Na3V2(PO4)2FO2 electrode materials have been investigated by a combination of 23Na and 31P magic-angle spinning NMR spectroscopy and density functional theory calculations. The spin distributions and the 31P NMR Fermi contact shifts in these materials are calculated based on the projector augmented wave approach implemented in the VASP code. Upon oxygen substitution, V4+ ions are formed and involved in highly covalent vanadyl bonds. We show that they exhibit a very specific electronic structure with a single electron on the 3dxy orbital perpendicular to the bi-octahedra axis. The V3+ ions, on the other hand, exhibit a partial occupation of the t2g orbitals by two electrons. The peculiar electronic structure of the V ions is at the origin of the complex spin transfer mechanisms observed in the Na3V2(PO4)2F3–Na3V2(PO4)2FO2 materials and results in the existence of several 23Na and 31P MAS NMR resonances. Owing to the proper signal assignment achieved using DFT calculations, we could estimate the degree of oxygen substitution for fluorine in the materials and discuss the local distribution of V3+/V4+ ions. Furthermore, through the 31P NMR study on the Na3V2(PO4)2FO2 composition, we here demonstrate that a 31P NMR resonance close to 0 ppm can also be observed in paramagnetic materials if there is no proper orbital overlap for the electron spin transfer to occur. Thanks to the proper signal assignment achieved using DFT calculations, we couldestimate the degree of substitution of oxygen for fluorine in the materialsand discuss the local distribution of V3+/V4+ions

Published
2019
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8. Monitoring the crystal structure and the electrochemical properties of Na3(VO)2(PO4)2F through Fe3+ substitution

Author

Stéphanie Belin, Jacob Olchowka, François Fauth, Antonella Iadecola, Mathieu Duttine, Long H. B. Nguyen, Paula Sanz Camacho, Dany Carlier, Laurence Croguennec, Christian Masquelier, Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB), Université de Bordeaux (UB)-Institut Polytechnique de Bordeaux-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Laboratoire réactivité et chimie des solides - UMR CNRS 7314 (LRCS), Université de Picardie Jules Verne (UPJV)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Réseau sur le stockage électrochimique de l'énergie (RS2E), Université de Picardie Jules Verne (UPJV)-Institut de Chimie du CNRS (INC)-Aix Marseille Université (AMU)-Université de Pau et des Pays de l'Adour (UPPA)-Université de Nantes (UN)-Université de Montpellier (UM)-Centre National de la Recherche Scientifique (CNRS)-Sorbonne Université (SU)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université Fédérale Toulouse Midi-Pyrénées-Université Fédérale Toulouse Midi-Pyrénées-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM), Advanced Lithium Energy Storage Systems - ALISTORE-ERI (ALISTORE-ERI), Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Synchrotron SOLEIL (SSOLEIL), Centre National de la Recherche Scientifique (CNRS), ALBA Synchrotron light source [Barcelone], The authors acknowledge the RS2E Network for the funding of LHBN’s Ph.D. thesis. The European Union’s Horizon 2020 research and innovation program under the Grant Agreement No. 646433-NAIADES, the French National Research Agency (STORE-EX Labex Project ANR-10-LABX-76-01 and SODIUM Descartes project ANR-13-DESC-0001-02) and the Région Nouvelle Aquitaine are acknowledged for their financial support. The authors also thank Cathy DENAGE, Emmanuel PETIT, Eric LEBRAUD, Alain WATTIAUX, and Yohan BIECHER (ICMCB) for their technical support. The synchrotron diffraction experiments were performed at the MSPD beamline at ALBA Synchrotron with the collaboration of ALBA staff and CALIPSOplus (Grant 730872) funding. XAS experiments were performed on the ROCK beamline at SOLEIL synchrotron, which is benefiting from a public grant overseen by the French National Research Agency as part of the 'Investissements d’Avenir' program (reference: ANR-10-EQPX-45)., ANR-10-EQPX-0045,ROCK,Spectromètre EXAFS Rapide pour Cinétiques Chimiques(2010), ANR-10-LABX-0076,STORE-EX,Laboratory of excellency for electrochemical energy storage(2010), ANR-13-DESC-0001,SODIUM,Batteries à ions sodium pour des robots télécommandés(2013), European Project: 646433,H2020,H2020-LCE-2014-3,NAIADES(2015), Université de Picardie Jules Verne (UPJV)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Aix Marseille Université (AMU)-Université de Haute-Alsace (UHA) Mulhouse - Colmar (Université de Haute-Alsace (UHA))-Collège de France (CdF (institution))-Université de Picardie Jules Verne (UPJV)-Ecole Nationale Supérieure de Chimie de Montpellier (ENSCM)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université de Pau et des Pays de l'Adour (UPPA)-Institut de Chimie du CNRS (INC)-Université de Montpellier (UM)-Sorbonne Université (SU)-Centre National de la Recherche Scientifique (CNRS)-Institut National Polytechnique (Toulouse) (Toulouse INP), Université de Toulouse (UT)-Université de Toulouse (UT)-Institut polytechnique de Grenoble - Grenoble Institute of Technology (Grenoble INP ), Université Grenoble Alpes (UGA)-Université Grenoble Alpes (UGA), and Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
Diffraction, Materials science, Na3V2(PO4)2F3, Synchrotron X-Ray Diffraction, 02 engineering and technology, Crystal structure, 010402 general chemistry, Electrochemistry, 01 natural sciences, sol−gel synthesis, General Materials Science, Fe3+ substitution, Na + diffusivity, Substitution (logic), sol-gel synthesis, [CHIM.MATE]Chemical Sciences/Material chemistry, 021001 nanoscience & nanotechnology, 0104 chemical sciences, Na3(VO)2(PO4)2F, Crystallography, Solid-state nuclear magnetic resonance, Fe 3+ -substitution, sodium-ion batteries, solid-state NMR, synchrotron X-ray diffraction, 0210 nano-technology, Na+ diffusivity
Abstract

International audience; We here present the synthesis of a new material, Na3(VO)Fe(PO4)2F2, by the sol–gel method. Its atomic and electronic structural descriptions are determined by a combination of several diffraction and spectroscopy techniques such as synchrotron X-ray powder diffraction and synchrotron X-ray absorption spectroscopy at V and Fe K edges, 57Fe Mössbauer, and 31P solid-state nuclear magnetic resonance spectroscopy. The crystal structure of this newly obtained phase is similar to that of Na3(VO)2(PO4)2F, with a random distribution of Fe3+ ions over vanadium sites. Even though Fe3+ and V4+ ions situate on the same crystallographic position, their local environment can be studied separately using 57Fe Mössbauer and X-ray absorption spectroscopy at Fe and V K edges, respectively. The Fe3+ ion resides in a symmetric octahedral environment, while the octahedral site of V4+ is greatly distorted due to the presence of the vanadyl bond. No electrochemical activity of the Fe4+/Fe3+ redox couple is detected, at least up to 5 V, whereas the reduction of Fe3+ to Fe2+ has been observed at ∼1.5 V versus Na+/Na through the insertion of 0.5 Na+ into Na3(VO)Fe(PO4)2F2. Comparing to Na3(VO)2(PO4)2F, the electrochemical profile of Na3(VO)Fe(PO4)2F2 in the same cycling condition shows a smaller polarization which could be due to a slight improvement in Na+ diffusion process thanks to the presence of Fe3+ in the framework. Furthermore, the desodiation mechanism occurring upon charging is investigated by operando synchrotron X-ray diffraction and operando synchrotron X-ray absorption at V K edge.

Published
2019
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