Soft X-ray Transmission Microscopy on Lithium-Rich Layered-Oxide Cathode Materials

Autor: Laura Simonelli, Andrea Sorrentino, Stefano Passerini, Arefehsadat Kazzazi, Eva Pereiro, Dino Tonti, Agnese Birrozzi, Angelo Mullaliu, Nina Laszczynski, Marco Giorgetti
Přispěvatelé: Ministerio de Ciencia, Innovación y Universidades (España), European Commission, Helmholtz Association, Sorrentino A., Simonelli L., Kazzazi A., Laszczynski N., Birrozzi A., Mullaliu A., Pereiro E., Passerini S., Giorgetti M., Tonti D.
Rok vydání: 2021
Předmět:
Chemical imaging
DDC 540 / Chemistry & allied sciences
Interkalation
Ratio of normal variable
full-field transmission microscopy
02 engineering and technology
01 natural sciences
lcsh:Technology
Spectral line
Batterie
lcsh:Chemistry
Coating
Microscopy
Intercalation
General Materials Science
Composition distribution
Arctangent
Computer science
information & general works

Absorption (electromagnetic radiation)
Instrumentation
lcsh:QH301-705.5
Fluid Flow and Transfer Processes
General Engineering
Stray light
Chemical mapping
021001 nanoscience & nanotechnology
lcsh:QC1-999
Computer Science Applications
composition distribution
ddc:540
Intercalations
chemical mapping
0210 nano-technology
Materials science
Absorption spectroscopy
batteries
Stray Radiation
engineering.material
010402 general chemistry
Molecular physics
ratio of normal variables
Batteries
Ratio of normal variables
intercalation
stray light
lcsh:T
Process Chemistry and Technology
Electric batteries
0104 chemical sciences
Chemical state
Full-field transmission microscopy
lcsh:Biology (General)
lcsh:QD1-999
arctangent
lcsh:TA1-2040
ddc:000
engineering
Particle
lcsh:Engineering (General). Civil engineering (General)
lcsh:Physics
Zdroj: Digital.CSIC. Repositorio Institucional del CSIC
instname
Applied Sciences, Vol 11, Iss 2791, p 2791 (2021)
Applied Sciences
Volume 11
Issue 6
Applied Sciences (Switzerland), 11 (6), Art.-Nr.: 2791
ISSN: 2076-3417
Popis: 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.
This research was funded by Spanish Government, through the “Severo Ochoa” Programme for Centers of Excellence in R&D (FUNFUTURE CEX2019-000917-S), and the projects MAT2017-91404-EXP, RTI2018-096273-B-I00 and RTI2018-097753-B-I00 with FEDER cofunding. D.T. participates in the FLOWBAT 2021 platforms promoted by the Spanish National Research Council (CSIC). The HIU authors acknowledge the basic funding from the Helmholtz Association.
Databáze: OpenAIRE