scholarly journals Studies of Lithium-Oxygen Battery Electrodes by Energy- Dependent Full-Field Transmission Soft X-Ray Microscopy

10.5772/66978 ◽  
2017 ◽  
Author(s):  
Dino Tonti ◽  
Mara Olivares-Marín ◽  
Andrea Sorrentino ◽  
Eva Pereiro
Keyword(s):  
Full Field ◽  
X Ray ◽  
Lithium Oxygen Battery ◽  
Energy Dependent

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

2021 ◽  
Vol 11 (6) ◽  
pp. 2791
Author(s):  
Andrea Sorrentino ◽  
Laura Simonelli ◽  
Arefehsadat Kazzazi ◽  
Nina Laszczynski ◽  
Agnese Birrozzi ◽  
...  
Keyword(s):  
Chemical State ◽  
Transmission Microscopy ◽  
Full Field ◽  
Battery Materials ◽  
X Ray ◽  
Full Picture ◽  
Phase Map ◽  
The One ◽  
Energy Dependent ◽  
First Time

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.

SIGMAL: A Program for Calculating L-Shell lonization Cross-Sections

1981 ◽  
Vol 39 ◽  
pp. 198-199 ◽  
Author(s):  
R.F. Egerton
Keyword(s):  
Cross Sections ◽  
Fortran Program ◽  
Absorption Data ◽  
X Ray ◽  
Atomic Electrons ◽  
Energy Dependent ◽  
Hydrogenic Model ◽  
Electron Energy Loss ◽  
X Ray Absorption ◽  
Shell Ionization

SIGMAL is a short (∼ 100-line) Fortran program designed to rapidly compute cross-sections for L-shell ionization, particularly the partial crosssections required in quantitative electron energy-loss microanalysis. The program is based on a hydrogenic model, the L1 and L23 subshells being represented by scaled Coulombic wave functions, which allows the generalized oscillator strength (GOS) to be expressed analytically. In this basic form, the model predicts too large a cross-section at energies near to the ionization edge (see Fig. 1), due mainly to the fact that the screening effect of the atomic electrons is assumed constant over the L-shell region. This can be remedied by applying an energy-dependent correction to the GOS or to the effective nuclear charge, resulting in much closer agreement with experimental X-ray absorption data and with more sophisticated calculations (see Fig. 1 ).

Full-Field Calcium K-Edge X-ray Absorption Near-Edge Structure Spectroscopy on Cortical Bone at the Micron-Scale: Polarization Effects Reveal Mineral Orientation

2016 ◽  
Vol 88 (7) ◽  
pp. 3826-3835 ◽  
Author(s):  
Bernhard Hesse ◽  
Murielle Salome ◽  
Hiram Castillo-Michel ◽  
Marine Cotte ◽  
Barbara Fayard ◽  
...  
Keyword(s):  
Cortical Bone ◽  
Edge Structure ◽  
Full Field ◽  
Polarization Effects ◽  
X Ray ◽  
X Ray Absorption

scholarly journals Sample Environment for Operando Hard X-ray Tomography—An Enabling Technology for Multimodal Characterization in Heterogeneous Catalysis

Catalysts ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 459
Author(s):  
Johannes Becher ◽  
Sebastian Weber ◽  
Dario Ferreira Sanchez ◽  
Dmitry E. Doronkin ◽  
Jan Garrevoet ◽  
...  
Keyword(s):  
Heterogeneous Catalysis ◽  
Synchrotron Radiation ◽  
Contrast Imaging ◽  
Co2 Methanation ◽  
Full Field ◽  
X Ray ◽  
Spatially Resolved ◽  
Oxidation Of Methane ◽  
Unique Source ◽  
Sample Environment

Structure–activity relations in heterogeneous catalysis can be revealed through in situ and operando measurements of catalysts in their active state. While hard X-ray tomography is an ideal method for non-invasive, multimodal 3D structural characterization on the micron to nm scale, performing tomography under controlled gas and temperature conditions is challenging. Here, we present a flexible sample environment for operando hard X-ray tomography at synchrotron radiation sources. The setup features are discussed, with demonstrations of operando powder X-ray diffraction tomography (XRD-CT) and energy-dispersive tomographic X-ray absorption spectroscopy (ED-XAS-CT). Catalysts for CO2 methanation and partial oxidation of methane are shown as case studies. The setup can be adapted for different hard X-ray microscopy, spectroscopy, or scattering synchrotron radiation beamlines, is compatible with absorption, diffraction, fluorescence, and phase-contrast imaging, and can operate with scanning focused beam or full-field acquisition mode. We present an accessible methodology for operando hard X-ray tomography studies, which offer a unique source of 3D spatially resolved characterization data unavailable to contemporary methods.

Energy-dependent dead-time correction in digital pulse processors applied to silicon drift detector's X-ray spectra

2018 ◽  
Vol 25 (2) ◽  
pp. 484-495 ◽  
Author(s):  
Suelen F. Barros ◽  
Vito R. Vanin ◽  
Alexandre A. Malafronte ◽  
Nora L. Maidana ◽  
Marcos N. Martins
Keyword(s):  
Dead Time ◽  
Pulse Height ◽  
Height Distribution ◽  
Pulse Height Distribution ◽  
Dead Time Correction ◽  
Time Model ◽  
X Ray ◽  
Digital Pulse ◽  
Analytical Correction ◽  
Energy Dependent

Dead-time effects in X-ray spectra taken with a digital pulse processor and a silicon drift detector were investigated when the number of events at the low-energy end of the spectrum was more than half of the total, at counting rates up to 56 kHz. It was found that dead-time losses in the spectra are energy dependent and an analytical correction for this effect, which takes into account pulse pile-up, is proposed. This and the usual models have been applied to experimental measurements, evaluating the dead-time fraction either from the calculations or using the value given by the detector acquisition system. The energy-dependent dead-time model proposed fits accurately the experimental energy spectra in the range of counting rates explored in this work. A selection chart of the simplest mathematical model able to correct the pulse-height distribution according to counting rate and energy spectrum characteristics is included.

Full-field X-ray diffraction microscopy using polymeric compound refractive lenses

2014 ◽  
Vol 47 (6) ◽  
pp. 1882-1888 ◽  
Author(s):  
J. Hilhorst ◽  
F. Marschall ◽  
T. N. Tran Thi ◽  
A. Last ◽  
T. U. Schülli
Keyword(s):  
Imaging Techniques ◽  
Light And Electron Microscopy ◽  
Added Value ◽  
Acquisition Time ◽  
Imaging Method ◽  
X Ray Diffraction ◽  
Polymeric Compound ◽  
Full Field ◽  
X Ray ◽  
Diffraction Imaging

Diffraction imaging is the science of imaging samples under diffraction conditions. Diffraction imaging techniques are well established in visible light and electron microscopy, and have also been widely employed in X-ray science in the form of X-ray topography. Over the past two decades, interest in X-ray diffraction imaging has taken flight and resulted in a wide variety of methods. This article discusses a new full-field imaging method, which uses polymer compound refractive lenses as a microscope objective to capture a diffracted X-ray beam coming from a large illuminated area on a sample. This produces an image of the diffracting parts of the sample on a camera. It is shown that this technique has added value in the field, owing to its high imaging speed, while being competitive in resolution and level of detail of obtained information. Using a model sample, it is shown that lattice tilts and strain in single crystals can be resolved simultaneously down to 10−3° and Δa/a= 10−5, respectively, with submicrometre resolution over an area of 100 × 100 µm and a total image acquisition time of less than 60 s.

scholarly journals Performance and optimization of X-ray grating interferometry

2014 ◽  
Vol 372 (2010) ◽  
pp. 20130027 ◽  
Author(s):  
T. Thuering ◽  
M. Stampanoni
Keyword(s):  
Interference Fringe ◽  
Refraction Angle ◽  
Fringe Visibility ◽  
X Ray ◽  
Analytical Formulae ◽  
Grating Interferometer ◽  
Differential Phase Contrast ◽  
Energy Dependent ◽  
Application Specific ◽  
Contrast Image

The monochromatic and polychromatic performance of a grating interferometer is theoretically analysed. The smallest detectable refraction angle is used as a metric for the efficiency in acquiring a differential phase-contrast image. Analytical formulae for the visibility and the smallest detectable refraction angle are derived for Talbot-type and Talbot–Lau-type interferometers, respectively, providing a framework for the optimization of the geometry. The polychromatic performance of a grating interferometer is investigated analytically by calculating the energy-dependent interference fringe visibility, the spectral acceptance and the polychromatic interference fringe visibility. The optimization of grating interferometry is a crucial step for the design of application-specific systems with maximum performance.

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