Michaël Deschamps

Conditions Extrêmes et Matériaux Haute Température et Irradiation

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Dominique Massiot

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Franck Fayon

Centre National de la Recherche Scientifique

Alexis Grimaud

Boston College

Sylvian Cadars

Centre National de la Recherche Scientifique

Elodie Salager

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Vincent Sarou‐Kanian

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Jean‐Marie Tarascon

Collège de France

Gwenaëlle Rousse

Collège de France

Valérie Montouillout

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Pierre Florian

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Cooperative Institutions

Centre National de la Recherche Scientifique

268

Réseau sur le Stockage Electrochimique de l'énergie

103

Conditions Extrêmes et Matériaux Haute Température et Irradiation

Université de Picardie Jules Verne

Université d'Orléans

Sorbonne Université

Collège de France

Chimie du Solide et Energie

Institut de Chimie

Commissariat à l'Énergie Atomique et aux Énergies Alternatives

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Superconcentrated Electrolytes Widens Insertion Electrochemistry to Soluble Layered Halides

Nicolas Dubouis Thomas Marchandier Gwenaëlle Rousse Florencia Marchini François Fauth

Insertion compounds provide the fundamental basis of today’s commercialized Li-ion batteries. Throughout history, intense research has focus on the design of stellar electrodes mainly relying on layered oxides or sulfides, and leaving aside the corresponding halides because of solubility issues. This is no longer true. In this work, we show for the first time the feasibility to reversibly intercalate electrochemically Li+ into VX3 compounds (X = Cl, Br, I) via the use of superconcentrated electrolytes, (5 M LiFSI in dimethyl carbonate), hence opening access to a novel family of LixVX3 phases. Moreover, through an electrolyte engineering approach we unambiguously prove that the positive attribute of superconcentrated electrolytes against solubility of inorganic compounds is rooted in a thermodynamic rather than a kinetic effect. The mechanism and corresponding impact of our findings enrich the fundamental understanding of superconcentrated electrolytes and constitute a crucial step in the design of novel insertion compounds with tunable properties for a wide range of applications beyond Li-ion batteries.

Fast ion conductor

10.26434/chemrxiv.14282021

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A Hydridoaluminate Additive Producing a Protective Coating on Ni‐Rich Cathode Materials in Lithium‐Ion Batteries

Advanced Energy Materials (2024)

Juan Forero-Saboya Ivan A. Moiseev Marina‐Lamprini Vlara Dominique Foix Michaël Deschamps

Abstract To enhance the energy density of Li‐ion batteries, high‐capacity and high‐voltage cathode materials are needed. Recently, Ni‐rich layered oxides have attracted attention as they can offer ≈200 mAh g −1 when cycled up to 4.3 V. However, cycling these materials in their full capacity range often leads to excessive reactivity with the electrolyte, resulting in particle cracking, transition metal dissolution, and oxygen loss. In this study, the use of lithium hydridoaluminates as electrolyte additives is explored for lithium‐ion batteries based on nickel‐rich cathode materials. Being mild reducing agents, these additives act as HF scavengers, avoiding transition metal dissolution from the cathode. Additionally, their oxidation results in the formation of an Al‐rich protective layer on the cathode, which dampens the surface reactivity, preventing surface reconstruction and impedance build‐up. This study further stresses the important role of the cathode‐electrolyte interface phenomena on the capacity degradation of Ni‐rich cathode materials and provides a novel avenue for controlling this reactivity, thus extending their cycling life.

Reactivity

10.1002/aenm.202402051

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Correlating Intermolecular Cross-Relaxation Rates with Distances and Coordination Numbers in Ionic Liquids

The Journal of Physical Chemistry Letters (2018)

Pierre‐Alexandre Martin Fangfang Chen Maria Forsyth Michaël Deschamps Luke A. O’Dell

The HOESY NMR experiment is commonly used to probe ion associations in ionic liquids and their mixtures. The parameter measured in this experiment is the heteronuclear cross-relaxation rate σ, which has dimensions of s-1. For intramolecular NOEs this scales as r-6 where r is the internuclear distance, but in the intermolecular case (as typically probed in studies of ionic liquids), theory predicts a more complex behavior including a distance dependence that is affected by the relative frequencies of the nuclei involved. Specifically, for nuclei with similar resonance frequencies such as 1H and 19F, it has been predicted that intermolecular NOEs will be sensitive to longer range distances than for nuclei with very different frequencies such as 1H and 7Li. In this contribution, we test this theory using a combination of quantitative HOESY analysis and molecular dynamics simulations carried out on two different ionic liquid electrolyte systems. In agreement with theoretical predictions, we find excellent correlations between the experimentally measured 1H-7Li NOEs and carbon-lithium distances below 4 Å, while longer distances (>6 Å) must be considered in order to obtain good correlations between 1H-19F NOEs and carbon-fluorine coordination numbers. This demonstrates the utility of HOESY NMR in understanding structure and interactions in ionic liquids while also illustrating that care must be taken in interpreting the measured cross-relaxation rates.

Heteronuclear molecule

10.1021/acs.jpclett.8b03021

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1D MRI, high resolution 2D and spin counting NMR for batteries and supercapacitors

Michaël Deschamps Elodie Salager Benjamin Porcheron Vincent Sarou‐Kanian

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Developing Operando Liquid-State NMR Spectroscopy of the Electrolyte Inside an Operating Li-ion Battery to Follow Its State of Charge

Khashayar Bagheri Vincent Sarou‐Kanian Michaël Deschamps Elodie Salager

State of charge

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Chasing Aqueous Biphasic Systems from Simple Salts by Exploring the LiTFSI/LiCl/H₂O Phase Diagram

ACS Central Science (2019)

Nicolas Dubouis Chanbum Park Michaël Deschamps Soufiane Abdelghani-Idrissi Matej Kanduč

Aqueous biphasic systems (ABSs), in which two aqueous phases with different compositions coexist as separate liquids, were first reported more than a century ago with polymer solutions. Recent observations of ABS forming from concentrated mixtures of inorganic salts and ionic liquids raise the fundamental question of how "different" the components of such mixtures should be for a liquid-liquid phase separation to occur. Here we show that even two monovalent salts sharing a common cation (lithium) but with different anions, namely, LiCl and lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), may result in the formation of ABSs over a wide range of compositions at room temperature. Using a combination of experimental techniques and molecular simulations, we analyze the coexistence diagram and the mechanism driving the phase separation, arising from the different anion sizes. The understanding and control of ABS may provide new avenues for aqueous-based battery systems.

Imide

10.1021/acscentsci.8b00955

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Atomic Layer Fluorination of the Li₄Ti₅O₁₂ Surface: A Multiprobing Survey

ACS Applied Energy Materials (2019)

Youn Charles‐Blin Delphine Flahaut Jean‐Bernard Ledeuil Katia Guérin Marc Dubois

Li4Ti5O12 (LTO) particles are successfully modified by an atomic layer fluorination process using a one-shot solvent-free synthesis performed with a solid-state fluorinating agent, xenon difluoride, at room temperature. LTO is reported as a promising anode material for lithium-ion batteries (LIBs) where high charging rates and long cycle life are required, because of its high potential preventing lithium dendrite deposition. The fluorination leads to the formation of passivating "Li—F" environments at the particle surface using the lowest amount of fluorine reported in the literature. Thanks to a multiprobing strategy, the impact of the fluorination on nonmodified, noncoated LTO has been characterized from the bulk to the extreme surface. The XRD patterns as well as the Raman spectra show no structural modification of the bulk while the combination of the XPS and NMR analysis gives insights about the impact of the fluorination on the entirety of the material. Auger fluorine chemical mapping displays the spatial distribution of a fluorinated layer all around the LTO particles.

Xenon difluoride

Fluorine

Difluoride

Surface layer

Surface Modification

10.1021/acsaem.9b01191

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Phase separation in sodium silicates observed by solid-state MAS-NMR

Journal of Non-Crystalline Solids (2014)

Laura Martel Dominique Massiot Michaël Deschamps

Magic angle spinning

Magic angle

Metastability

10.1016/j.jnoncrysol.2014.02.015

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1H and 19F ultra-fast MAS double-quantum single-quantum NMR correlation experiments using three-spin terms of the dipolar homonuclear Hamiltonian

Mexican International Conference on Computer Science (2011)

Michaël Deschamps Franck Fayon Sylvian Cadars Anne‐Laure Rollet Dominique Massiot

Measuring internuclear distances through dipolar interaction is a major challenge for solid-state nuclear magnetic resonance (NMR) spectroscopy. Obtaining reliable interatomic distances provides an access to the local structure in ordered or disordered solids. We show that at magic angle spinning (MAS) frequencies larger than ca. 50 kHz, some of the three-spin terms of the homogeneous homonuclear dipolar Hamiltonian can be used to promote the creation of double-quantum coherences between neighbouring 1H or 19F spins without using dipolar recoupling pulse sequences in the Dipolar Homonuclear Homogeneous Hamiltonian (DH3) double-quantum/single-quantum correlation experiment. This makes it possible to probe inter-nuclear spatial proximity with limited risk of probe or sample damage from radio-frequency (RF) irradiation, and is fully appropriate for fast repetition rate offering sensitivity gains in favourable cases. Experimental demonstrations are supported by multi-spin numerical simulations, which points to new possibilities for the characterization of spin-system geometries.

Homonuclear molecule

Hamiltonian (control theory)

Magic angle spinning

Flip angle

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NMR of materials up to the nanometer scale

HAL (Le Centre pour la Communication Scientifique Directe) (2012)

Dominique Massiot Sylvian Cadars Michaël Deschamps Franck Fayon Valérie Montouillout

Nanometre

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