On high-temperature evolution of passivation layer in Li–10 wt % Mg alloy via in situ SEM-EBSD

Kaboli, Shirin; Noël, P.; Clément, Daniel; Demers, Hendrix; Paolella, Andrea; Bouchard, Patrick; Goodenough, John B.; Zaghib, Karim

doi:10.1126/sciadv.abd5708

Cited by 15 publications

(12 citation statements)

References 35 publications

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“…S8). Scanning electron microscopy–electron backscatter diffraction–energy-dispersive spectroscopy (SEM-EBSD-EDS) was used to investigate the morphology of Al-HCGB-Li foil and the distribution of Al atoms in Al-HCGB-Li ( 39 ). The surface of Al-HCGB-Li foils is flat and smooth (Fig.…”

Section: Resultsmentioning

confidence: 99%

Inhibiting intercrystalline reactions of anode with electrolytes for long-cycling lithium batteries

Shi

Zhou

et al. 2022

Sci. Adv.

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The life span of lithium batteries as energy storage devices is plagued by irreversible interfacial reactions between reactive anodes and electrolytes. Occurring on polycrystal surface, the reaction process is inevitably affected by the surface microstructure of anodes, of which the understanding is imperative but rarely touched. Here, the effect of grain boundary of lithium metal anodes on the reactions was investigated. The reactions preferentially occur at the grain boundary, resulting in intercrystalline reactions. An aluminum (Al)–based heteroatom-concentrated grain boundary (Al-HCGB), where Al atoms concentrate at grain boundary, was designed to inhibit the intercrystalline reactions. In particular, the scalable preparation of Al-HCGB was demonstrated, with which the cycling performance of a pouch cell (355 Wh kg −1 ) was significantly improved. This work opens a new avenue to explore the effect of the surface microstructure of anodes on the interfacial reaction process and provides an effective strategy to inhibit reactions between anodes and electrolytes for long–life-span practical lithium batteries.

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Section: Resultsmentioning

confidence: 99%

Inhibiting intercrystalline reactions of anode with electrolytes for long-cycling lithium batteries

Shi

Zhou

et al. 2022

Sci. Adv.

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“…The in situ SEM heat treatment of the alloy showed no change in the morphology of the surface passivation layer above the melting point while the bulk was melted. They employed electron backscatter diffraction (EBSD) crystal orientation mapping, which showed the formation of new grains after melting, confirming their observation [43].…”

Section: Chemical and Crystallographic Analysismentioning

confidence: 54%

“…Kaboli et al [43] used an in situ SEM technique to monitor the evolution of the passivation layer for Li-10 Mg alloy as a potential anode material at high temperature. The in situ SEM heat treatment of the alloy showed no change in the morphology of the surface passivation layer above the melting point while the bulk was melted.…”

Section: Chemical and Crystallographic Analysismentioning

confidence: 99%

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

2021

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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.

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“…We propose the mechanism of lithiophilicity from the cross-sectional point of view in the schematics in Figure B,C: In the case of the Cu@Zn sample in contact with a molten Li metal in (B) at RT (I), the Li metal passivation layer is in contact with the Zn film; hence, the Cu interface is composed of an oxide film in contact with the Zn film. At 300 °C (II), the Li 2 CO 3 /LiOH passivation layer cracks and the molten Li metal gets in contact with the Zn film, forming a metastable ternary Li-Cu-Zn alloy that spreads over the oxide-rich Cu interface, while the colder passivation layer on top remains solid (as observed in Movie S1). During solidification (III), two reaction happens: (a) the first reaction is at the interface of Cu when the Cu oxide reacts with Li, releasing large Cu-rich particles and forming Li oxide at the interface, and (b) the second reaction occurs near the colder top edge of the molten Li metal where Li solidification results in segregation of Cu and Zn by locking them into intermetallic particles (Movie S2).…”

Section: Discussionmentioning

confidence: 99%

Unraveling the Origin of Lithiophilicity toward a Molten Li Metal: Zn Metal as Trojan Horse

Kaboli

Zhu

Clément

et al. 2023

ACS Appl. Energy Mater.

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In this work, we investigated the origin of lithiophilicity of a Cu foil substrate modified by a sputtered Zn thin film (Cu@Zn) in contact with a molten Li metal to understand the reaction mechanism between Li and Cu@Zn. We studied the reaction between the molten Li metal and the Cu surface during Li solidification via in situ scanning electron microscopy (SEM), subsequently performed post-mortem energy dispersive spectroscopy (EDS) and Grazing Incidence X-ray Diffraction (GIXRD) on the coatings to analyze the chemistry of the reaction products, and compared the results for different thicknesses of nanometric Zn films (5–50 nm). For the first time in the literature, we report the existence of a metastable ternary Li-Cu-Zn alloy at 300 °C after the reaction of Cu@Zn with the molten Li metal. We also report the segregation of Cu and Zn by formation of Cu-Zn intermetallic compounds during the cooling down step. The results of our in situ study are pivotal to clarify the interfacial reactions occurring between a lithiophilic current collector and a molten Li metal and have utmost importance for designing advanced anode materials for future solid-state battery applications.

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On high-temperature evolution of passivation layer in Li–10 wt % Mg alloy via in situ SEM-EBSD

Cited by 15 publications

References 35 publications

Inhibiting intercrystalline reactions of anode with electrolytes for long-cycling lithium batteries

Inhibiting intercrystalline reactions of anode with electrolytes for long-cycling lithium batteries

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

Unraveling the Origin of Lithiophilicity toward a Molten Li Metal: Zn Metal as Trojan Horse

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