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10. Influence of Polymorphism on the Electrochemical Behavior of Dilithium (2,3-Dilithium-oxy)-terephthalate vs. Li.

Author

Bernard, Lou, Jouhara, Alia, Quarez, Eric, Levieux-Souid, Yanis, Le Caër, Sophie, Tran-Van, Pierre, Renault, Stéven, and Poizot, Philippe

Subjects
STORAGE batteries, DECARBOXYLATION, CATHODES, CRYSTALS, MOIETIES (Chemistry)
Abstract

Organic electrode materials offer obvious opportunities to promote cost-effective and environmentally friendly rechargeable batteries. Over the last decade, tremendous progress has been made thanks to the use of molecular engineering focused on the tailoring of redox-active organic moieties. However, the electrochemical performance of organic host structures relies also on the crystal packing, like the inorganic counterparts, which calls for further efforts in terms of crystal chemistry to make a robust redox-active organic center electrochemically efficient in the solid state. Following our ongoing research aiming at elaborating lithiated organic cathode materials, we report herein on the impact of polymorphism on the electrochemical behavior of dilithium (2,3-dilithium-oxy-)terephthalate vs. Li. Having isolated dilithium (3-hydroxy-2-lithium-oxy)terephthalate through an incomplete acid-base neutralization reaction, its subsequent thermally induced decarboxylation mechanism led to the formation of a new polymorph of dilithium (2,3-dilithium-oxy-)terephthalate referred to as Li4-o-DHT (β-phase). This new phase is able to operate at 3.1 V vs. Li+/Li, which corresponds to a positive potential shift of +250 mV compared to the other polymorph formerly reported. Nevertheless, the overall electrochemical process characterized by a sluggish biphasic transition is impeded by a large polarization value limiting the recovered capacity upon cycling. [ABSTRACT FROM AUTHOR]

Published
2022
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12. Mass Spectrometry Analysis of NMC622/Graphite Li-Ion Cells Electrolyte Degradation Products after Storage and Cycling.

Author

Rigaud, Sébastien, Martinez, Ana Cristina, Lombard, Tristan, Grugeon, Sylvie, Tran-Van, Pierre, Pilard, Serge, and Laruelle, Stephane

Subjects
ELECTROLYTES, PRINCIPAL components analysis, TRITON X-100, MASS spectrometry, COMPARATIVE literature
Abstract

With the aim of establishing a data simultaneous comparison, the Principal Component Analysis (PCA) statistical tool was applied to LiNi0.6Mn0.2Co0.2O2/graphite Li-ion cells electrolyte's decomposition products detected by UHPLC-ESI-HRMS. Herein, we illustrate how the chemometric tool associated with mass spectrometry data can be relevant to provide information about the presence of unusual molecules. Indeed, pristine Triton X-100 surfactant molecules used in the electrode elaboration process were detected after the impregnation stage. However, as they chemically react and oxidize at a potential lower than 4.5 V vs Li/Li+, only surfactant derivatives and classical ageing molecules were observed, respectively, after storage and cycling stages at 55 °C, leading to a triangle-type correlation circle. On the other hand, global schemes of LiPF6-based electrolyte degradation pathways were elaborated from a comparative study with literature to help interpret results in future electrolyte ageing studies. [ABSTRACT FROM AUTHOR]

Published
2022
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14. Multiscale Morphological and Electrical Characterization of Charge Transport and Charge Transfer Limitations to Power Performance of Positive Electrode for Li-Ion Batteries

Author

Besnard, Nicolas, Tran-Van, Pierre, Etiemble, Aurélien, Maire, Éric, Douillard, Thierry, dubrunfaut, olivier, Franger, Sylvain, Badot, Jean-Claude, Lestriez, B., Technocentre Renault [Guyancourt], RENAULT, Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), Laboratoire Génie électrique et électronique de Paris (GeePs), Université Paris-Sud - Paris 11 (UP11)-Université Pierre et Marie Curie - Paris 6 (UPMC)-CentraleSupélec-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC), Laboratoire de Chimie de la Matière Condensée de Paris (site ENSCP) (LCMCP (site ENSCP)), Centre National de la Recherche Scientifique (CNRS)-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF (institution))-Institut de Chimie du CNRS (INC), Institut des Matériaux Jean Rouxel (IMN), Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM), Université Paris-Sud - Paris 11 (UP11)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Pierre et Marie Curie - Paris 6 (UPMC)-Collège de France (CdF (institution))-Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL)-Université Paris sciences et lettres (PSL)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), and Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[SPI.NRJ]Engineering Sciences [physics]/Electric power, ComputingMilieux_MISCELLANEOUS, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

International audience

Published
2018

16. Contribution of the dielectric spectroscopy to the multiscale study of the electrode materials

Author

Besnard, Nicolas, Lestriez, Bernard, Etiemble, Aurélien, Douillard, Thierry, Dubrunfaut, Olivier, Tran-Van, Pierre, Laurent, Gautier, Franger, Sylvain, Badot, Jean-Claude, Maire, Eric, Technocentre Renault [Guyancourt], RENAULT, Institut des Matériaux Jean Rouxel (IMN), Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS), Consortium Lyon Saint-Etienne de Microscopie (CLYM), École normale supérieure de Lyon (ENS de Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Université de Lyon-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet - Saint-Étienne (UJM), Laboratoire Génie électrique et électronique de Paris (GeePs), Université Paris-Sud - Paris 11 (UP11)-Université Pierre et Marie Curie - Paris 6 (UPMC)-CentraleSupélec-Centre National de la Recherche Scientifique (CNRS), Institut de Chimie Moléculaire et des Matériaux d'Orsay (ICMMO), Université Paris-Sud - Paris 11 (UP11)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL), Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), École normale supérieure - Lyon (ENS Lyon)-École Centrale de Lyon (ECL), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Université Jean Monnet [Saint-Étienne] (UJM), and Université Paris-Sud - Paris 11 (UP11)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)

Subjects
[SPI]Engineering Sciences [physics], ComputingMilieux_MISCELLANEOUS, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

International audience

Published
2016

17. Multi-Scale Characterization of Electronic and Ionic Limitations to Power Performance of Composite Electrodes Toward Ultra-High Surface Capacities

Author

Lestriez, Bernard, Etiemble, Aurélien, Besnard, Nicolas, Jimenez-Manero, Pablo, Tran Van, Pierre, dubrunfaut, olivier, Gaubicher, Joël, Guyomard, Dominique, Badot, Jean-Claude, Maire, Éric, Institut des Matériaux Jean Rouxel (IMN), Université de Nantes - UFR des Sciences et des Techniques (UN UFR ST), Université de Nantes (UN)-Université de Nantes (UN)-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN), Matériaux, ingénierie et science [Villeurbanne] (MATEIS), Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut National des Sciences Appliquées de Lyon (INSA Lyon), Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA), Laboratoire Génie électrique et électronique de Paris (GeePs), Université Paris-Sud - Paris 11 (UP11)-Université Pierre et Marie Curie - Paris 6 (UPMC)-CentraleSupélec-Centre National de la Recherche Scientifique (CNRS), Technocentre Renault [Guyancourt], RENAULT, Ecole Nationale Supérieure de Chimie de Paris - Chimie ParisTech-PSL (ENSCP), Université Paris sciences et lettres (PSL), Université de Nantes (UN)-Université de Nantes (UN)-Ecole Polytechnique de l'Université de Nantes (EPUN), Université de Nantes (UN)-Université de Nantes (UN)-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS), Université Claude Bernard Lyon 1 (UCBL), and Université de Lyon-Institut National des Sciences Appliquées (INSA)-Institut National des Sciences Appliquées (INSA)-Centre National de la Recherche Scientifique (CNRS)

Subjects
[SPI]Engineering Sciences [physics], ComputingMilieux_MISCELLANEOUS, [SPI.MAT]Engineering Sciences [physics]/Materials
Abstract

By using a set of advanced techniques such as the broad band dielectric spectroscopy, X-Ray and FIB-SEM computed tomography, it will be described which factor(s) (material properties, engineering parameters) mainly influence the rate discharging behavior of NMC- or LFP-based composite electrodes. This fundamental understanding will be rationalized to disclose ultra-high surface capacities electrodes (more than 10 mAh / cm²) with reasonable rate performance.

Published
2016

19. Multiscale Morphological and Electrical Characterization of Charge Transport Limitations to the Power Performance of Positive Electrode Blends for Lithium-Ion Batteries.

Author

Besnard, Nicolas, Etiemble, Aurélien, Douillard, Thierry, Dubrunfaut, Olivier, Tran‐Van, Pierre, Gautier, Laurent, Franger, Sylvain, Badot, Jean‐Claude, Maire, Eric, and Lestriez, Bernard

Subjects
LITHIUM-ion batteries, ELECTRODES, ELECTRIC properties of materials, FOCUSED ion beams, SCANNING electron microscopy
Abstract

In this work, exhaustive characterizations of 3D geometries of LiNi1/3Mn1/3Co1/3O2 (NMC), LiFePO4 (LFP), and NMC/LFP blended electrodes are undertaken for rational interpretation of their measured electrical properties and electrochemical performance. X-ray tomography and focused ion beam in combination with scanning electron microscopy tomography are used for a multiscale analysis of electrodes 3D geometries. Their multiscale electrical properties are measured by using broadband dielectric spectroscopy. Finally, discharge rate performance are measured and analyzed by simple, yet efficient methods. It allows us to discriminate between electronic and ionic wirings as the performance limiting factors, depending on the discharge rate. This approach is a unique exhaustive analysis of the experimental relationships between the electrochemical behavior, the transport properties within the electrode, and its 3D geometry. [ABSTRACT FROM AUTHOR]

Published
2017
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20. Ultrathin Cu(In, Ga)Se2 solar cells.

Author

Naghavi, Negar, Jehl, Zacharie, Erfurth, Felix, Guillemoles, Jean-Francois, Donsanti, Frederique, Gerard, Isabelle, Tran-Van, Pierre, Bouttemy, Muriel, Etcheberry, Arnaud, Pelouard, Jean-Luc, Collin, Stephane, Colin, Clement, Pere-Laperne, Nicolas, Dahan, Nir, Greffet, Jean-Jacques, Morel, Boris, Djebbour, Zakaria, Darga, Arouna, Mencaraglia, Denis, and Voorwinden, Georg

Abstract

Within the UltraCIS project we have started to explore the possibility of reducing down the thickness of the Cu(In, Ga)Se2 (CIGSe) layer to the sub-micron level (0.1μm) while maintaining a high efficiency level of solar cells. The three main approaches we used are: — Reducing the CIGSe thickness by chemical etching combining the thickness reduction and smoothing effect of the absorber. Efficiency higher than 10 % on small area cells with an absorber thickness of 0.5 μm are obtained. Losses were attributed exclusively to the reduced photocurrent and the loss on texturation of the absorber — Optical management by front contact texturation or by replacement of the back contact by the “lift-off” of CIGSe layer from the Mo layer and deposition of a new reflective back contact. — Application of plasmonic structures to CIGSe solar cells enabling light confinement at the subwavelength scale [ABSTRACT FROM PUBLISHER]

Published
2011
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22. Lithium-Ion Batteries: Multiscale Morphological and Electrical Characterization of Charge Transport Limitations to the Power Performance of Positive Electrode Blends for Lithium-Ion Batteries (Adv. Energy Mater. 8/2017).

Author

Besnard, Nicolas, Etiemble, Aurélien, Douillard, Thierry, Dubrunfaut, Olivier, Tran‐Van, Pierre, Gautier, Laurent, Franger, Sylvain, Badot, Jean‐Claude, Maire, Eric, and Lestriez, Bernard

Subjects
LITHIUM-ion batteries, COMPOSITE materials, STORAGE batteries, ELECTRODES, ENERGY storage
Abstract

A better understanding of the charge transport (ions and electrons) kinetics limitations through the electrode is required to improve the Li‐ion battery's energy and power density in view of electrical cars deployment. In article number 1602239, Bernard Lestriez and co‐workers connect for the first time the parameters describing the microstructure of electrodes with both measurements of their transport properties and their electrochemical performance. [ABSTRACT FROM AUTHOR]

Published
2017
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23. High reactivity of the nickel-rich LiNi1-x-yMnxCoyO2 layered materials surface towards H2O/CO2 atmosphere and LiPF6-based electrolyte.

Author

Martinez, Ana Cristina, Grugeon, Sylvie, Cailleu, Dominique, Courty, Matthieu, Tran-Van, Pierre, Delobel, Bruno, and Laruelle, Stephane

Subjects
*INDUCTIVELY coupled plasma atomic emission spectrometry, *ELECTROCHEMICAL electrodes, *TRANSITION metal oxides, *SURFACES (Technology), *ELECTROLYTE analysis
Abstract

Storage of nickel-rich LiNi 1-x-y Mn x Co y O 2 positive active materials under improper environmental conditions brings about undesirable surface reactions causing poor Li-ion cell electrochemical performances and gas generation. In this paper, a detailed stepwise investigation of the increasing reactivity of 532, 622, 811 and 901 NMC materials towards a specific H 2 O/CO 2 atmosphere is reported. Water-soluble salts as lithium carbonate, hydroxide and sulfates are accurately quantified thanks to acid-base titration and inductively coupled plasma atomic emission spectroscopy techniques. On the other hand, the presence of insoluble species as transition metal oxyhydroxides and oxides is unveiled through a thermal decomposition study using thermogravimetric mass spectrometer coupling technique. Their formation and thermal decomposition mechanisms are proposed after careful analysis of the characteristic mass loss and O 2 , CO 2 and H 2 O evolution profile in the 50–500 °C region. Interestingly, the results also highlight an in situ lithiated layered oxide material reformation reaction. To assess their chemical reactivity towards LiPF 6 -based electrolyte, the latter was analyzed through 19F nuclear magnetic resonance after storage with various reference salts and 811 NMC. LiPO 2 F 2 is detected from storage tests with Li 2 CO 3 , Li 2 O and Li 2 SO 4 , and fluorophosphate-type molecules are detected from LiOH; this experiment can help discriminate between LiOH and Li 2 O as NMC surface species. • NMCs surface species composition before and after H 2 O/CO 2 exposure is elucidated. • Warder's titration method allows for an accurate quantification of OH− and CO 3 2−. • ICP-AES, IR and SEM/EDX data indicate the presence Li or Na sulfates. • The amount of basic species increases in Ni-rich NMCs surfaces. • Li 2 O is postulated instead of LiOH through 19F NMR analysis of the electrolyte. [ABSTRACT FROM AUTHOR]

Published
2020
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24. Effect of lithiation potential and cycling on chemical and morphological evolution of Si thin film electrode studied by ToF-SIMS.

Author

Pereira-Nabais C, Światowska J, Rosso M, Ozanam F, Seyeux A, Gohier A, Tran-Van P, Cassir M, and Marcus P

Abstract

Si thin films obtained by plasma enhanced chemical vapor deposition (PECVD) were used to investigate chemical and morphological modifications induced by lithiation potential and cycling. These modifications were thoughtfully analyzed by time-of-flight secondary ion mass spectrometry (ToF-SIMS) depth profiling, which allows to distinguish the surface and bulk processes related to the formation of the solid electrolyte interphase (SEI) layer, and Li-Si alloying, respectively. The main results are a volume expansion/shrinkage and a dynamic behavior of the SEI layer during the single lithiation/delithiation process and multicycling. Trapping of lithium and other ions corresponding to products of electrolyte decomposition are the major reasons of electrode modifications. It is shown that the SEI layer contributes to 60% of the total volume variation of Si electrodes (100 nm). The apparent diffusion coefficient of lithium (DLi) calculated from the Fick's second law directly from Li-ion ToF-SIMS profiles is of the order of ∼5.9 × 10(-15) cm(2).s(-1). This quite low value can be explained by Li trapping in the bulk of electrode material, at the interfaces, continuous growth of the SEI layer and increase of SiO2 quantity. These modifications can result in limitation the ionic transport of Li.

Published
2014
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