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Applied Sciences
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Synchrotron- and FEL-Based X-ray Methods for Battery Studies
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Synchrotron- and FEL-Based X-ray Methods for Battery Studies

A special issue of Applied Sciences (ISSN 2076-3417). This special issue belongs to the section "Energy Science and Technology".

Deadline for manuscript submissions: closed (30 June 2021) | Viewed by 10980

Special Issue Editors

Dr. Marco Giorgetti

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Guest Editor
Department of Industrial Chemistry, University of Bologna, Viale del Risorgimento 4, 40136 Bologna, Italy
Interests: electrodes for energy; cathode and anode materials for advanced batteries; characterization of materials and electrodes by core level spectroscopies; metal hexacyanoferrates
Special Issues, Collections and Topics in MDPI journals
Dr. Giuliana Aquilanti

E-Mail Website
Guest Editor
Elettra-Sincrotrone Trieste, Strada Statale 14 km, km 163.5 in AREA Science Park, 34149 Trieste, Italy
Interests: structural characterization of advanced materials for energy storage; structural characterization of matter under extreme pressure and temperature conditions
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The purpose of this Special Issue is to provide an up-to-date overview of advanced analytical techniques available in large-scale facilities such as synchrotrons and free-electron lasers for the study of battery devices. The ultra-bright radiation from the infrared to hard X-rays range available at those international laboratories permits us to check, for instance, the electronic structure of selected atomic species and the local and average structure of electrode materials by using scattering and absorption techniques. Key factors governing the modification of the electrode/electrolyte interfaces can be studied by microscopy and also by surface-sensitive techniques such as photoelectron spectroscopy. The intriguing possibility of performing operando data acquisition (i.e. during charging and discharging loops of the battery) gives access to visualization of the full electrochemical process in realistic conditions. This Special Issue also focuses on advanced and efficient methods to extract all the relevant information in operando spectroscopic and crystallographic data by using chemometric tools. Everybody working in these specific fields is strongly encouraged to submit a contribution.

Prof. Dr. Marco Giorgetti
Dr. Giuliana Aquilanti
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Applied Sciences is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2400 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • batteries
  • diffraction
  • EXAFS
  • XANES
  • photoelectron spectroscopy
  • electrode electrolyte interface
  • total scattering techniques
  • reaction mechanism
  • operando
  • microscopy
  • charge and discharge dynamic
  • data analysis
  • chemometry

Published Papers (5 papers)

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Research

10 pages, 3033 KiB  
Article
Operando XAS of a Bifunctional Gas Diffusion Electrode for Zn-Air Batteries under Realistic Application Conditions
by Emanuele Marini, Danilo Oliveira De Souza, Giuliana Aquilanti, Michael Liebert, Francesca Rossi and Benedetto Bozzini
Appl. Sci. 2021, 11(24), 11672; https://doi.org/10.3390/app112411672 - 09 Dec 2021
Cited by 5 | Viewed by 1988
Abstract
In this study, operando X-ray absorption spectroscopy (XAS) measurements were carried out on a newly developed O2 bi-functional gas diffusion electrode (GDE) for rechargeable Zn-air batteries, consisting of a mixture of α-MnO2 and carbon black. The architecture and composition of the [...] Read more.
In this study, operando X-ray absorption spectroscopy (XAS) measurements were carried out on a newly developed O2 bi-functional gas diffusion electrode (GDE) for rechargeable Zn-air batteries, consisting of a mixture of α-MnO2 and carbon black. The architecture and composition of the GDE, as well as the electrochemical cell, were designed to achieve optimum edge-jumps and signal-to-noise ratio in the absorption spectra for the Mn K-edge at current densities that are relevant for practical conditions. Herein, we reported the chemical changes that occur on the MnO2 component when the GDE is tested under normal operating conditions, during both battery discharge (ORR) and charge (OER), on the background of more critical conditions that simulate oxygen starvation in a flooded electrode. Full article
(This article belongs to the Special Issue Synchrotron- and FEL-Based X-ray Methods for Battery Studies)
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19 pages, 8284 KiB  
Article
Soft X-ray Transmission Microscopy on Lithium-Rich Layered-Oxide Cathode Materials
by Andrea Sorrentino, Laura Simonelli, Arefehsadat Kazzazi, Nina Laszczynski, Agnese Birrozzi, Angelo Mullaliu, Eva Pereiro, Stefano Passerini, Marco Giorgetti and Dino Tonti
Appl. Sci. 2021, 11(6), 2791; https://doi.org/10.3390/app11062791 - 21 Mar 2021
Cited by 5 | Viewed by 2375
Abstract
Energy-dependent full field transmission soft X-ray microscopy (TXM) is able to give a full picture at the nanometer scale of the chemical state and spatial distribution of oxygen and other elements relevant for battery materials, providing pixel-by-pixel absorption spectrum. We show different methods [...] Read more.
Energy-dependent full field transmission soft X-ray microscopy (TXM) is able to give a full picture at the nanometer scale of the chemical state and spatial distribution of oxygen and other elements relevant for battery materials, providing pixel-by-pixel absorption spectrum. We show different methods to localize chemical inhomogeneities in Li1.2Mn0.56Ni0.16Co0.08O2 particles with and without VOx coating extracted from electrodes at different states of charge. Considering the 3d(Mn,Ni)-2p(O) hybridization, it has been possible to discriminate the chemical state of Mn and Ni in addition to the one of O. Different oxidation states correspond to specific features in the O-K spectra. To localize sample regions with specific compositions we apply two different methods. In the first, the pixel-by-pixel ratios of images collected at different key energies clearly highlight local inhomogeneities. In the second, introduced here for the first time, we directly correlate corresponding pixels of the two images on a xy scatter plot that we call phase map, where we can visualize the distributions as function of thickness as well as absorption artifacts. We can select groups of pixels, and then map regions with similar spectral features. Core-shell distributions of composition are clearly shown in these samples. The coating appears in part to frustrate some of the usual chemical evolution. In addition, we could directly observe several further aspects, such as: distribution of conducting carbon; inhomogeneous state of charge within the electrode; molecular oxygen profiles within a particle. The latter suggests a surface loss with respect to the bulk but an accumulation layer at intermediate depth that could be assigned to retained O2. Full article
(This article belongs to the Special Issue Synchrotron- and FEL-Based X-ray Methods for Battery Studies)
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10 pages, 3184 KiB  
Article
Structural Effects of Anomalous Current Densities on Manganese Hexacyanoferrate for Li-Ion Batteries
by Angelo Mullaliu, Stéphanie Belin, Lorenzo Stievano, Marco Giorgetti and Stefano Passerini
Appl. Sci. 2020, 10(21), 7573; https://doi.org/10.3390/app10217573 - 27 Oct 2020
Viewed by 2097
Abstract
A battery management system (BMS) plays a pivotal role in providing optimal performance of lithium-ion batteries (LIBs). However, the eventual malfunction of the BMS may lead to safety hazards or reduce the remaining useful life of LIBs. Manganese hexacyanoferrate (MnHCF) was employed as [...] Read more.
A battery management system (BMS) plays a pivotal role in providing optimal performance of lithium-ion batteries (LIBs). However, the eventual malfunction of the BMS may lead to safety hazards or reduce the remaining useful life of LIBs. Manganese hexacyanoferrate (MnHCF) was employed as the positive electrode material in a Li-ion half-cell and subjected to five cycles at high current densities (10 A gMnHCF−1) and to discharge at 0.1 A gMnHCF−1, instead of classical charge/discharge cycling with initial positive polarization at 0.01 A gMnHCF−1, to simulate a current sensor malfunctioning and to evaluate the electrochemical and structural effects on MnHCF. The operando set of spectra at the Mn and Fe K-edges was further analyzed through multivariate curve resolution analysis with an alternating least squares algorithm (MCR–ALS) and extended X-ray absorption fine structure (EXAFS) spectroscopy to investigate the structural modifications arising during cycling after the applied electrochemical protocol. The coulombic efficiency in the first cycle was dramatically affected; however, the local structural environment around each photo absorber recovered during charging. The identification of an additional spectral contribution in the electrochemical process was achieved through MCR-ALS analysis, and the Mn-local asymmetry was thoroughly explored via EXAFS analysis. Full article
(This article belongs to the Special Issue Synchrotron- and FEL-Based X-ray Methods for Battery Studies)
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11 pages, 3164 KiB  
Article
Identifying the Degradation Mechanism in Commercial Lithium Rechargeable Batteries via High-Energy X-ray Compton Scattering Imaging
by Kosuke Suzuki, Yuji Otsuka, Naruki Tsuji, Kazushi Hoshi, Yoshiharu Sakurai and Hiroshi Sakurai
Appl. Sci. 2020, 10(17), 5855; https://doi.org/10.3390/app10175855 - 24 Aug 2020
Cited by 5 | Viewed by 1780
Abstract
Synchrotron-based high-energy X-ray Compton scattering imaging is a promising technique for non-destructively and quantitatively investigating commercialized lithium rechargeable batteries. We apply the Compton scattering imaging technique to commercial coin-type lithium rechargeable cells (VL2020) to non-destructively identify the degradation mechanism of the cell. The [...] Read more.
Synchrotron-based high-energy X-ray Compton scattering imaging is a promising technique for non-destructively and quantitatively investigating commercialized lithium rechargeable batteries. We apply the Compton scattering imaging technique to commercial coin-type lithium rechargeable cells (VL2020) to non-destructively identify the degradation mechanism of the cell. The correlations between the Compton scattering intensity and line-shape of the Compton scattering X-ray energy spectrum (S-parameter) obtained from this technique produce unique distributions that characterize the aged cell. These distributions in the aged cell indicate that the stable phase of the anode formed through the overvoltage charge–discharge cycle. This stable phase prevents lithium reactions, producing microbubbles with the decomposition of the electrolyte. Full article
(This article belongs to the Special Issue Synchrotron- and FEL-Based X-ray Methods for Battery Studies)
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10 pages, 1435 KiB  
Article
Revisiting the Sodiation Mechanism of TiO2 via Operando X-ray Absorption Spectroscopy
by Marcus Fehse, Aurélien Henry, Andrea Zitolo, Bruno Boury, Nicolas Louvain and Lorenzo Stievano
Appl. Sci. 2020, 10(16), 5547; https://doi.org/10.3390/app10165547 - 11 Aug 2020
Cited by 7 | Viewed by 2086
Abstract
The sodiation mechanism of TiO2 anatase was thoroughly investigated via X-ray absorption spectroscopy under operando conditions. The data set was analysed via an innovative and smart approach based on chemometric tools that allows the unbiased and reliable extraction of the maximum amount [...] Read more.
The sodiation mechanism of TiO2 anatase was thoroughly investigated via X-ray absorption spectroscopy under operando conditions. The data set was analysed via an innovative and smart approach based on chemometric tools that allows the unbiased and reliable extraction of the maximum amount of meaningful information. The resulting data analysis reveals that the electrochemical sodiation mechanism is mainly based on the reduction of Ti4+ to Ti3+, going along with the irreversible amorphisation of the pristine anatase structure. At least one semi-amorphous intermediate is formed during the first discharge, whose local structure resembles those obtained at the end of the charge. Full article
(This article belongs to the Special Issue Synchrotron- and FEL-Based X-ray Methods for Battery Studies)
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