First results from in situ transmission electron microscopy studies of all-solid-state fluoride ion batteries

Fawey, Mohammed H.; Chakravadhanula, Venkata Sai Kiran; Reddy, M. Anji; Rongeat, Carine; Hahn, Horst; Fichtner, Maximilian; Kübel, Christian

doi:10.1016/j.jpowsour.2020.228283

Cited by 13 publications

(8 citation statements)

References 48 publications

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“…characterized the morphological and structural evolution of electrodes and their interfaces with a solid‐state electrolyte in an all‐solid‐state fluoride‐ion battery using in situ TEM and SEM (Figure 21b). [ 157 ] Copper clearly coarsened after the first cycle. Voids then formed in the Cu/C cathode and became more pronounced after failure (Figure 21b(i–iii)), indicating a strong volumetric change accompanying the electrochemical reaction.…”

Section: Materials and Devices Available For Electrochemical Activati...mentioning

confidence: 99%

“…b) STEM images of the electrolyte-cathode interface (i) pristine state, (ii) after the 1st cycle, (iii) after the 2nd charging; SEM images of the anode-electrolyte interface (iv), full cell (v), the electrolyte-cathode interface (vi) before cycling; SEM images of the anode-electrolyte interface (vii), full cell (viii), the electrolyte-cathode interface (ix) after cycling. Reproduced with permission [157]. Copyright 2020, Elsevier.…”

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confidence: 99%

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Electrochemical Activation, Sintering, and Reconstruction in Energy‐Storage Technologies: Origin, Development, and Prospects

Zhang

Pei

et al. 2022

Advanced Energy Materials

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Her research interests focus on the design of nano/micromaterials toward energy storage and conversion (i.e., Li-, Na-, and K-ion batteries) application. She joined Prof. Shibing Ni's group at the China Three Gorges University in 2020. Now she works as a lecturer at the College of Materials and Chemical Engineering, and concentrates on the morphological and structural evolution of electrode materials during cycling.

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Section: Materials and Devices Available For Electrochemical Activati...mentioning

confidence: 99%

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confidence: 99%

Electrochemical Activation, Sintering, and Reconstruction in Energy‐Storage Technologies: Origin, Development, and Prospects

Zhang

Pei

et al. 2022

Advanced Energy Materials

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“…A FIB based approach is commonly used to perform cross-section as discussed by Vasile et al [48] and does not require any pretreatment of the samples which makes it more advantageous over the other existing conventional techniques such as ion milling and ultramicrotomy techniques. FIB processed cross-section for all-solid-state samples is also used in other works by Wang et al [38] and Fawey et al [19,49] to investigate the interface effects while monitoring electrochemical and structural changes with high spatial resolution.…”

Section: Fib Lamella Fabrication and Connection To The Micro-chipmentioning

confidence: 99%

In Situ Liquid Electrochemical TEM Investigation of LiMn_1.5Ni_0.5O₄ Thin Film Cathode for Micro‐Battery Applications

et al. 2021

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Micro‐batteries are attractive miniaturized energy devices for new Internet of Things applications, but the lack of understanding of their degradation process during cycling hinders improving their performance. Here focused ion beam (FIB)‐lamella from LiMn1.5Ni0.5O4 (LMNO) thin‐film cathode is in situ cycled in a liquid electrolyte inside an electrochemical transmission electron microscope (TEM) holder to analyze structural and morphology changes upon (de)lithiation processes. A high‐quality electrical connection between the platinum (Pt) current collector of FIB‐lamella and the microchip's Pt working electrode is established, as confirmed by local two‐probe conductivity measurements. In situ cyclic voltammetry (CV) experiments show two redox activities at 4.41 and 4.58/4.54 V corresponding to the Ni2+/3+ and Ni3+/4+ couples, respectively. (S)TEM investigations of the cycled thin‐film reveal formation of voids and cracks, loss of contact with current collector, and presence of organic decomposition products. The 4D STEM ASTAR technique highlights the emergence of an amorphization process and a decrease in average grain size from 20 to 10 nm in the in situ cycled electrode. The present findings, obtained for the first time through the liquid electrochemical TEM study, provide several insights explaining the capacity fade of the LMNO thin‐film cathode typically observed upon cycling in a conventional liquid electrolyte.

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“…In studies concerning all-solid-state FIBs, metal/metal fluoride (M/MF x ) systems are regarded as attractive electrodes that can afford significantly high capacities through multielectron (de)fluorination processes, and it is possible to fabricate high-potential batteries by employing suitable combinations of working and counter electrodes. Therefore, the theoretical energy densities of all-solid-state FIBs with M/MF x electrodes can reach 5000 Wh L –1 or higher, substantially exceeding those of LIB materials. − However, limited by sluggish ion transport in the bulk of M/MF x materials as well as the electrolytes, all-solid-state FIBs exhibit low capacity and undergo significant polarization under mild temperatures. ,, Furthermore, the traditional bulk-type constructions of all-solid-state batteries lead to severe problems in electrode–electrolyte interfacial contacts and long diffusion distances because of large pellet thickness, which further worsen the kinetics of the electrochemical process. ,,− …”

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confidence: 99%

Cu–Pb Nanocomposite Cathode Material toward Room-Temperature Cycling for All-Solid-State Fluoride-Ion Batteries

Zhang

Yoshinari

Yamamoto

et al. 2021

ACS Appl. Energy Mater.

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All-solid-state fluoride-ion batteries (FIBs) are regarded as attractive alternatives to traditional energy storage systems because of their high energy density; however, they are not applicable at room temperature owing to sluggish ion transport in both the electrolyte and electrode. In this study, a rational design of a Cu–Pb nanocomposite is reported, which was tested as a room-temperature cathode material for all-solid-state FIBs. Following electrochemical pretreatment, self-generated PbF2 could act as a fast fluoride-ion conductor and consequently enhance the kinetics of the Cu/CuF2 phase transition process upon cycling. The detailed reaction mechanism and phase transition process were verified using the X-ray absorption near edge structure. The Cu–Pb nanocomposite could realize reversible (de)fluorination at room temperature with high performance and good cyclability.

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First results from in situ transmission electron microscopy studies of all-solid-state fluoride ion batteries

Cited by 13 publications

References 48 publications

Electrochemical Activation, Sintering, and Reconstruction in Energy‐Storage Technologies: Origin, Development, and Prospects

Electrochemical Activation, Sintering, and Reconstruction in Energy‐Storage Technologies: Origin, Development, and Prospects

In Situ Liquid Electrochemical TEM Investigation of LiMn_1.5Ni_0.5O₄ Thin Film Cathode for Micro‐Battery Applications

Cu–Pb Nanocomposite Cathode Material toward Room-Temperature Cycling for All-Solid-State Fluoride-Ion Batteries

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First results from in situ transmission electron microscopy studies of all-solid-state fluoride ion batteries

Cited by 13 publications

References 48 publications

Electrochemical Activation, Sintering, and Reconstruction in Energy‐Storage Technologies: Origin, Development, and Prospects

Electrochemical Activation, Sintering, and Reconstruction in Energy‐Storage Technologies: Origin, Development, and Prospects

In Situ Liquid Electrochemical TEM Investigation of LiMn1.5Ni0.5O4 Thin Film Cathode for Micro‐Battery Applications

Cu–Pb Nanocomposite Cathode Material toward Room-Temperature Cycling for All-Solid-State Fluoride-Ion Batteries

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In Situ Liquid Electrochemical TEM Investigation of LiMn_1.5Ni_0.5O₄ Thin Film Cathode for Micro‐Battery Applications