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A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday

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A special issue of Inorganics (ISSN 2304-6740).

Deadline for manuscript submissions: closed (28 February 2022) | Viewed by 53932

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Prof. Dr. Christian M. Julien

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Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie (IMPMC), Sorbonne Université, CNRS-UMR 7590, 4 Place Jussieu, 75252 Paris, France
Interests: energy storage; solid-state ionics; lithium batteries; thin films
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Prof. Dr. Alain Mauger

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‎Inst Mineral Phys Mat & Cosmochim IMPMC, CNRS, Sorbonne University, UMR 7590, 4 Pl Jussieu, F-75252 Paris, France
Interests: materials science; energy storage and conversion; Li-ion batteries; Na-ion batteries
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

This Special Issue is to celebrate the outstanding career of one of the most world-renowned experts in electrochemistry, Dr Michel Armand, on the occasion of his 75th anniversary. He is the father of many advances that led to the development of lithium-ion batteries, now considered a solution to switch from oil to green energy and limit global warning. Armand is at the origin of the concept: in the 1970s, Armand proposed the fabrication of a battery based on two different intercalation materials for both cathodes and anodes; this battery was named the rocking-chair battery (later the lithium-ion battery) due to the shuttle of ions from one electrode to another during the charge–discharge process. Then, he made major contributions to the three components of the batteries: the two electrodes and the electrolyte.

First, in collaboration with Duclot, he demonstrated in the late seventies the suitability of graphite as an intercalated negative electrode. He is thus the father of this negative electrode used in commercial Li-ion batteries today. Then, in the early eighties, Armand pioneered the development of a polymer electrolyte based on polyethylene oxide-lithium salts (PEO:Li), at the origin of the all-solid-state lithium batteries that fed Bolloré's Buecars® and Bluebuses®, and considered a promising battery of the next generation. In 1991, Armand’s group reported a novel salt: lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), now used in a new class of single-ion solid polymer and solvent-in-salt electrolytes, all results offering evidence that Armand played and is still playing a major role in the development of lithium-ion batteries.

Let us go back, however, to the seventies, when efforts were devoted to the search for materials able to intercalate lithium without destroying the crystalline structure to build positive electrodes. Armand et al. demonstrated that Prussian-blue materials, such as iron cyanide bronzes M_0.5Fe(CN)₃ fulfilled the purpose. Armand also pioneered the use of several inorganic materials and transition metal oxides and described the first solid-state battery using β-alumina as a solid electrolyte. In 1997, John Goodenough proposed LiFePO₄; however, this material is insulating—a problem that needed to be solved prior to practical application. The solution was found by Armand’s group, by coating the LiFePO₄ nanoparticles with a thin layer of conducting carbon, and in 2020, the global lithium iron phosphate battery market size exceeded US$ 5.20 billion.

This short introduction only aims to testify to the impact of the work that marked the career of Armand in electrochemistry, to celebrate his 75th birthday. This is of course incomplete, not only because Michel Armand never stops, but also because he is the co-author of more than 500 publications and many patents.

Contributions in this Special Issue will outline recent developments related to the chemistries of lithium-ion and sodium-ion batteries, including cathode and anode materials, organic electrodes, solid-state electrolytes, solid polymers, and solvent-in-salt electrolytes and other chemistries, such as Li-S and Li-air batteries.

We are pleased to invite you to submit a manuscript to this Special Issue; regular articles, communications, and reviews are all welcome.

Prof. Dr. Christian Julien
Prof. Dr. Alain Mauger
Guest Editors

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Published Papers (13 papers)

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13 pages, 4331 KiB

Open AccessArticle

Stabilizing the (003) Facet of Micron-Sized LiNi_0.6Co_0.2Mn_0.2O₂ Cathode Material Using Tungsten Oxide as an Exemplar

by Yang Li, Liubin Ben, Hailong Yu, Wenwu Zhao, Xinjiang Liu and Xuejie Huang

Inorganics 2022, 10(8), 111; https://doi.org/10.3390/inorganics10080111 - 3 Aug 2022

Cited by 7 | Viewed by 2667

Abstract

The structural stability of layered LiNi_1-x-yCo_xMn_yO₂ cathode materials is critical for guaranteeing their excellent electrochemical cycling performance, particularly at elevated temperatures. However, the notorious H₂–H₃ phase transition along with associated large changes in the c-axis or (003) facet is the fundamental origin of the anisotropic and abrupt change in the unit cell and the degradation of the cycling performance. In this study, we coat micron-sized LiNi_0.6Co_0.2Mn_0.2O₂ (NCM) with tungsten oxide via atomic layer deposition and investigate the atomic-to-microscopic structures in detail via advanced characterization techniques, such as Cs-corrected scanning transmission electron microscopy. The results reveal that coated tungsten oxide is predominately accumulated on the (003) facet of NCM, with the migration of a small amount of W⁶⁺ into this facet, resulting in a reduction of Ni³⁺ to Ni²⁺ and the formation of a rock-salt-like structure on the surface. The electrochemical cycling performance of tungsten-oxide-coated NCM is significantly improved, showing a capacity retention of 86.8% after 300 cycles at 55 °C, compared to only 69.4% for the bare NCM. Through further structural analysis, it is found that the initial tungsten-oxide-coating-induced (003) facet distortion effectively mitigates the expansion of the c-lattice during charge, as well as oxygen release from the lattice, resulting in a lowered strain in the cathode lattices and a crack in the cathode particles after prolonged cycling. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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11 pages, 2439 KiB

Open AccessArticle

Enhancing the Performance of Ceramic-Rich Polymer Composite Electrolytes Using Polymer Grafted LLZO

by Pierre Ranque, Jakub Zagórski, Grazia Accardo, Ander Orue Mendizabal, Juan Miguel López del Amo, Nicola Boaretto, Maria Martinez-Ibañez, Hugo Arrou-Vignod, Frederic Aguesse, Michel Armand and Shanmukaraj Devaraj

Inorganics 2022, 10(6), 81; https://doi.org/10.3390/inorganics10060081 - 13 Jun 2022

Cited by 7 | Viewed by 3522

Abstract

Solid-state batteries are the holy grail for the next generation of automotive batteries. The development of solid-state batteries requires efficient electrolytes to improve the performance of the cells in terms of ionic conductivity, electrochemical stability, interfacial compatibility, and so on. These requirements call for the combined properties of ceramic and polymer electrolytes, making ceramic-rich polymer electrolytes a promising solution to be developed. Aligned with this aim, we have shown a surface modification of Ga substituted Li₇La₃Zr₂O₁₂ (LLZO), to be an essential strategy for the preparation of ceramic-rich electrolytes. Ceramic-rich polymer membranes with surface-modified LLZO show marked improvements in the performance, in terms of electrolyte physical and electrochemical properties, as well as coulombic efficiency, interfacial compatibility, and cyclability of solid-state cells. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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8 pages, 2005 KiB

Open AccessArticle

Quantifying Lithium Ion Exchange in Solid Electrolyte Interphase (SEI) on Graphite Anode Surfaces

by Janet S. Ho, Zihua Zhu, Philip Stallworth, Steve G. Greenbaum, Sheng S. Zhang and Kang Xu

Inorganics 2022, 10(5), 64; https://doi.org/10.3390/inorganics10050064 - 17 May 2022

Cited by 2 | Viewed by 3180

Abstract

Solid Electrolyte Interphase (SEI) has been identified as the most important and least understood component in lithium-ion batteries. Despite extensive studies in the past two decades, a few mysteries remain: what is the chemical form of and degree of mobility of Li⁺ in the interphase? What fraction of Li⁺ is permanently immobilized in the SEI, while the rest are still able to participate in the cell reactions via the ion-exchange process with Li⁺ in the electrolyte? This study attempted to answer, in part, these questions by using ⁶Li and ⁷Li-isotopes to label SEIs and electrolytes, and then quantifying the distribution of permanently immobilized and ion-exchangeable Li⁺ with solid-state NMR and ToF-SIMS. The results showed that the majority of Li⁺ were exchanged after one SEI formation cycle, and a complete exchange after 25 cycles. Ion exchange by diffusion based on concentration gradient in the absence of applied potential also occurred simultaneously. This knowledge will provide a foundation for not only understanding but also designing better SEIs for future battery chemistries. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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16 pages, 4828 KiB

Open AccessArticle

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

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

Inorganics 2022, 10(5), 62; https://doi.org/10.3390/inorganics10050062 - 10 May 2022

Cited by 3 | Viewed by 2891

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. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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13 pages, 5484 KiB

Open AccessArticle

Interfaces between Ceramic and Polymer Electrolytes: A Comparison of Oxide and Sulfide Solid Electrolytes for Hybrid Solid-State Batteries

by Dominic Spencer Jolly, Dominic L. R. Melvin, Isabella D. R. Stephens, Rowena H. Brugge, Shengda D. Pu, Junfu Bu, Ziyang Ning, Gareth O. Hartley, Paul Adamson, Patrick S. Grant, Ainara Aguadero and Peter G. Bruce

Inorganics 2022, 10(5), 60; https://doi.org/10.3390/inorganics10050060 - 26 Apr 2022

Cited by 7 | Viewed by 6406

Abstract

Hybrid solid-state batteries using a bilayer of ceramic and solid polymer electrolytes may offer advantages over using a single type of solid electrolyte alone. However, the impedance to Li⁺ transport across interfaces between different electrolytes can be high. It is important to determine the resistance to Li⁺ transport across these heteroionic interfaces, as well as to understand the underlying causes of these resistances; in particular, whether chemical interphase formation contributes to giving high resistances, as in the case of ceramic/liquid electrolyte interfaces. In this work, two ceramic electrolytes, Li₃PS₄ (LPS) and Li_6.5La₃Zr_1.5Ta_0.5O₁₂ (LLZTO), were interfaced with the solid polymer electrolyte PEO₁₀:LiTFSI and the interfacial resistances were determined by impedance spectroscopy. The LLZTO/polymer interfacial resistance was found to be prohibitively high but, in contrast, a low resistance was observed at the LPS/polymer interface that became negligible at a moderately elevated temperature of 50 °C. Chemical characterization of the two interfaces was carried out, using depth-profiled X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry, to determine whether the interfacial resistance was correlated with the formation of an interphase. Interestingly, no interphase was observed at the higher resistance LLZTO/polymer interface, whereas LPS was observed to react with the polymer electrolyte to form an interphase. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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15 pages, 5594 KiB

Open AccessArticle

Synergistic Effect of Co and Mn Co-Doping on SnO₂ Lithium-Ion Anodes

by Adele Birrozzi, Angelo Mullaliu, Tobias Eisenmann, Jakob Asenbauer, Thomas Diemant, Dorin Geiger, Ute Kaiser, Danilo Oliveira de Souza, Thomas E. Ashton, Alexandra R. Groves, Jawwad A. Darr, Stefano Passerini and Dominic Bresser

Inorganics 2022, 10(4), 46; https://doi.org/10.3390/inorganics10040046 - 1 Apr 2022

Cited by 6 | Viewed by 3132

Abstract

The incorporation of transition metals (TMs) such as Co, Fe, and Mn into SnO₂ substantially improves the reversibility of the conversion and the alloying reaction when used as a negative electrode active material in lithium-ion batteries. Moreover, it was shown that the specific benefits of different TM dopants can be combined when introducing more than one dopant into the SnO₂ lattice. Herein, a careful characterization of Co and Mn co-doped SnO₂ via transmission electron microscopy coupled with energy-dispersive X-ray spectroscopy and X-ray diffraction including Rietveld refinement is reported. Based on this in-depth investigation of the crystal structure and the distribution of the two TM dopants within the lattice, an ex situ X-ray photoelectron spectroscopy and ex situ X-ray absorption spectroscopy were performed to better understand the de-/lithiation mechanism and the synergistic impact of the Co and Mn co-doping. The results specifically suggest that the antithetical redox behaviour of the two dopants might play a decisive role for the enhanced reversibility of the de-/lithiation reaction. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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11 pages, 3619 KiB

Open AccessArticle

Ionic Conductivity of LiSiON and the Effect of Amorphization/Heterovalent Doping on Li⁺ Diffusion

by Siyuan Wu, Ruijuan Xiao, Hong Li and Liquan Chen

Inorganics 2022, 10(4), 45; https://doi.org/10.3390/inorganics10040045 - 31 Mar 2022

Cited by 3 | Viewed by 2850

Abstract

The search for and design of suitable superior lithium ion conductors is a key process for developing solid state batteries. In order to realize a large range of applications, we researched the ionic conductivity of LiSiON, an example oxynitride mainly composed of elements with high abundance and a similar mixed anion size. Both its amorphous and heterovalent-doped phases were studied through density functional theory simulations. The Li⁺ ion diffusion behaviors and related properties are discussed. These elements are abundant in nature, and we found that amorphization or doping with P obviously enhanced the ionic conductivity of the system. General strategies to improve the kinetic properties of a candidate structure are presented, to help in the design of solid state electrolytes for lithium batteries. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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12 pages, 2895 KiB

Open AccessArticle

Enabling Stable Interphases via In Situ Two-Step Synthetic Bilayer Polymer Electrolyte for Solid-State Lithium Metal Batteries

by Ying Liu, Fang Fu, Chen Sun, Aotian Zhang, Hong Teng, Liqun Sun and Haiming Xie

Inorganics 2022, 10(4), 42; https://doi.org/10.3390/inorganics10040042 - 29 Mar 2022

Cited by 8 | Viewed by 3050

Abstract

Poly(ethylene oxide) (PEO)-based electrolyte is considered to be one of the most promising polymer electrolytes for lithium metal batteries. However, a narrow electrochemical stability window and poor compatibility at electrode-electrolyte interfaces restrict the applications of PEO-based electrolyte. An in situ synthetic double-layer polymer electrolyte (DLPE) with polyacrylonitrile (PAN) layer and PEO layer was designed to achieve a stable interface and application in high-energy-density batteries. In this special design, the hydroxy group of PEO-SPE can form an O-H^---N hydrogen bond with the cyano group in PAN-SPE, which connects the two layers of DLPE at a microscopic chemical level. A special Li⁺ conducting mechanism in DLPE provides a uniform Li⁺ flux and fast Li⁺ conduction, which achieves a stable electrolyte/electrode interface.LiFePO₄/DLPE/Li battery shows superior cycling stability, and the coulombic efficiency remains 99.5% at 0.2 C. Meanwhile, LiNi_0.6Co_0.2Mn_0.2O₂/DLPE/Li battery shows high specific discharge capacity of 176.0 mAh g⁻¹ at 0.1 C between 2.8 V to 4.3 V, and the coulombic efficiency remains 95% after 100 cycles. This in situ synthetic strategy represents a big step forward in addressing the interface issues and boosting the development of high-energy-density lithium-metal batteries. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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21 pages, 7268 KiB

Open AccessArticle

Improved Electrochemical Behavior and Thermal Stability of Li and Mn-Rich Cathode Materials Modified by Lithium Sulfate Surface Treatment

by Hadar Sclar, Sandipan Maiti, Rosy Sharma, Evan M. Erickson, Judith Grinblat, Ravikumar Raman, Michael Talianker, Malachi Noked, Aleksandr Kondrakov, Boris Markovsky and Doron Aurbach

Inorganics 2022, 10(3), 39; https://doi.org/10.3390/inorganics10030039 - 20 Mar 2022

Cited by 5 | Viewed by 4857

Abstract

High-energy cathode materials that are Li- and Mn-rich lithiated oxides—for instance, 0.35Li₂MnO₃^.0.65LiNi_0.35Mn_0.45Co_0.20O₂ (HE-NCM)—are promising for advanced lithium-ion batteries. However, HE-NCM cathodes suffer from severe degradation during cycling, causing gradual capacity loss, voltage fading, and low-rate capability performance. In this work, we applied an effective approach to creating a nano-sized surface layer of Li₂SO₄ on the above material, providing mitigation of the interfacial side reactions while retaining the structural integrity of the cathodes upon extended cycling. The Li₂SO₄ coating was formed on the surface of the material by mixing it with nanocrystalline Li₂SO₄ and annealing at 600 °C. We established enhanced electrochemical behavior with ~20% higher discharge capacity, improved charge-transfer kinetics, and higher rate capability of HE-NCM cathodes due to the presence of the Li₂SO₄ coating. Online electrochemical mass spectrometry studies revealed lower CO₂ and H₂ evolution in the treated samples, implying that the Li₂SO₄ layer partially suppresses the electrolyte degradation during the initial cycle. In addition, a ~28% improvement in the thermal stability of the Li₂SO₄-treated samples in reactions with battery solution was also shown by DSC studies. The post-cycling analysis allowed us to conclude that the Li₂SO₄ phase remained on the surface and retained its structure after 100 cycles. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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13 pages, 4462 KiB

Open AccessArticle

Influence of Ti Substitution on Electrochemical Performance and Evolution of LiMn_1.5−x Ni_0.5Ti_xO₄ (x = 0.05, 0.1, 0.3) as a High Voltage Cathode Material with a Very Long Cycle Life

by Svetlana Niketic, Chae-Ho Yim, Jigang Zhou, Jian Wang and Yaser Abu-Lebdeh

Inorganics 2022, 10(1), 10; https://doi.org/10.3390/inorganics10010010 - 12 Jan 2022

Cited by 2 | Viewed by 2724

Abstract

The high voltage spinel material LiMn_1.5Ni_0.5O₄ (LMNO) has the potential to increase the energy density of lithium batteries. However, its battery performance suffers from poor long-term cycling and high-temperature stability. In order to overcome these limitations, we have studied the effect of partial substitution of Mn with Ti and LiMn_1.5−x Ni_0.5Ti_xO₄ (x = 0.05, 0.1, 0.3), LMNTO, materials have been synthesized in a newly modified sol-gel method and then characterized by TEM, SEM (EDX), AC Electrochemical Impedance Spectroscopy and Soft X-ray Spectromicroscopy. We have demonstrated that the long-term cycling limitation with these types of materials can be resolved and herein 2000 cycles at a high C-rate have been demonstrated in half cells. We have attributed this behavior to a possible charge compensation mechanism as evidenced by a Soft X-ray Spectromicroscopy study of delithiated LMNTO materials. This work takes high energy density batteries based on high voltage spinel material one step further towards commercialization, and it is believed that further improvement can be achieved using new electrolyte formulations. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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Review

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14 pages, 3764 KiB

Open AccessReview

Solid Polymer Electrolytes for Lithium Batteries: A Tribute to Michel Armand

by Alain Mauger and Christian M. Julien

Inorganics 2022, 10(8), 110; https://doi.org/10.3390/inorganics10080110 - 29 Jul 2022

Cited by 11 | Viewed by 4141

Abstract

In a previous publication, a tribute to Michel Armand was provided, which highlighted his outstanding contribution to all aspects of research and development of lithium-metal and lithium-ion batteries. This area is in constant progress and rather than an overview of the work of Armand et al. since the seventies, we mainly restrict this review to his contribution to advances in solid polymer electrolytes (SPEs) and their performance in all-solid-state lithium-metal batteries in recent years. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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51 pages, 12095 KiB

Open AccessReview

Remedies to Avoid Failure Mechanisms of Lithium-Metal Anode in Li-Ion Batteries

by Alain Mauger and Christian M. Julien

Inorganics 2022, 10(1), 5; https://doi.org/10.3390/inorganics10010005 - 31 Dec 2021

Cited by 4 | Viewed by 7009

Abstract

Rechargeable lithium-metal batteries (LMBs), which have high power and energy density, are very attractive to solve the intermittence problem of the energy supplied either by wind mills or solar plants or to power electric vehicles. However, two failure modes limit the commercial use of LMBs, i.e., dendrite growth at the surface of Li metal and side reactions with the electrolyte. Substantial research is being accomplished to mitigate these drawbacks. This article reviews the different strategies for fabricating safe LMBs, aiming to outperform lithium-ion batteries (LIBs). They include modification of the electrolyte (salt and solvents) to obtain a highly conductive solid–electrolyte interphase (SEI) layer, protection of the Li anode by in situ and ex situ coatings, use of three-dimensional porous skeletons, and anchoring Li on 3D current collectors. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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12 pages, 1436 KiB

Open AccessReview

In Situ and In Operando Techniques to Study Li-Ion and Solid-State Batteries: Micro to Atomic Level

by Maryam Golozar, Raynald Gauvin and Karim Zaghib

Inorganics 2021, 9(11), 85; https://doi.org/10.3390/inorganics9110085 - 22 Nov 2021

Cited by 8 | Viewed by 4906

Abstract

This work summarizes the most commonly used in situ techniques for the study of Li-ion batteries from the micro to the atomic level. In situ analysis has attracted a great deal of interest owing to its ability to provide a wide range of information about the cycling behavior of batteries from the beginning until the end of cycling. The in situ techniques that are covered are: X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), and Scanning Transmission Electron Microscopy (STEM). An optimized setup is required to be able to use any of these in situ techniques in battery applications. Depending on the type of data required, the available setup, and the type of battery, more than one of these techniques might be needed. This study organizes these techniques from the micro to the atomic level, and shows the types of data that can be obtained using these techniques, their advantages and their challenges, and possible strategies for overcoming these challenges. Full article

(This article belongs to the Special Issue A Themed Issue in Honor of Professor Michel Armand on the Occasion of His 75th Birthday)

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