Identifying different states of lithiation of Li4Ti5O12spinel by energy-dispersive inelastic X-ray scattering (EDIXS) spectroscopy

The Li4Ti5O12 (LTO) compound has been investigated as an alternative negative electrode material for lithium ion batteries (LIBs), which are being used as energy storage devices in stationary systems as well as for electric vehicles due to their many interesting features. The LTO compound has shown remarkable Li-ion intercalation/de-intercalation reversibility, demonstrating also zero-strain volume change during the cycling process along with notable safety performance. Furthermore, LTO has a high voltage plateau in comparison with other negative material candidates, helping to avoid the deposition of metallic lithium in the dendrite form. Due to its performance and potential application in LIBs, a deep knowledge regarding the behavior of this LTO compound is of high interest. In this work, energy-dispersive resonant inelastic X-ray scattering (EDIXS) is used to fulfill this need. In addition, XANES measurements were carried out as complementary methodology. The results indicate that EDIXS can differentiate LTO chemical compounds (lithiated and de-lithiated) with high sensitivity, and is a reliable tool to perform chemical speciation analysis on such samples. In addition, the results confirm theoretical predictions regarding the composition of different oxidation states of titanium associated with different states of charge/lithiation of the LTO-spinel also. The proposed methodology can be easily applied to other lithium-based materials and beyond them, such as those based on sodium and novel technologies based on polyvalent cations including magnesium and aluminium. This journal isFil: Robledo, José Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Leani, Juan José. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Chauque, Susana. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; ArgentinaFil: Camara, Osvaldo Raul. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; ArgentinaFil: Sanchez, Hector Jorge. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Oliva, Fabiana Yolanda. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Investigaciones en Físico-química de Córdoba. Universidad Nacional de Córdoba. Facultad de Ciencias Químicas. Instituto de Investigaciones en Físico-química de Córdoba; Argentin

A Tool for GIXRF/XRR simulation and data analysis

Ponencia presentada en el Monte Carlo Simulation Tools for X-Ray Imaging and Fluorescence Workshop, 2014The IAEA has developed a beamline end-station facility that it is currently installed at the newly developed XRF beamline of Elettra Sincrotrone Trieste, ItalyThe end-station called Ultra High Vacuum Chamber (UHVC) is a multipurpose facility for applying simultaneously various complementary and advanced variants of X-Ray Spectrometry (XRS) techniques, including: Total Reflection X-ray Fluorescence Analysis (TXRF) Grazing Incidence/Exit XRF analysis (GIXRF- GEXRF) Near Edge X-ray Absorption Fine Structure (NEXAFS) X-ray Reflectometry (XRR) The current development of GIXRF/XRR simulations/analysis tool aims at assisting end-users in data processing and interpretation.Fil: Leani, Juan José. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; Argentina.Fil: Leani, Juan José. Nuclear Science and Instrumentation Laboratory, IAEA Laboratories; Austria.Física Atómica, Molecular y Química (física de átomos y moléculas incluyendo colisión, interacción con radiación, resonancia magnética, Moessbauer Efecto.

A multipurpose experimental facility for advanced X-ray Spectrometry applications

Ponencia presentada en la European Conference on X-Ray Spectrometry (EXRS). 2014Motivation, Ultra High Vacuum Chamber (UHVC) project: To support/enhance the training of scientists/engineers from developing countries in the operation of synchrotron radiation instrumentation; To provide beam time access for R&D projects and hands-on training in SR-XRS based techniques; To promote networking and knowledge sharing; To increase the quality and the competitiveness of the developing countries to apply beam time proposals at SR facilities; To contribute in the further development of XRS techniques in applications with socioeconomicalrelevance (characterization of energy storage/conversion materials, environmental, biological and biomedical applications)Fil: Leani, Juan José. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; Argentina.Fil: Leani, Juan José. Nuclear Science and Instrumentation Laboratory, IAEA Laboratories; Austria.Física Atómica, Molecular y Química (física de átomos y moléculas incluyendo colisión, interacción con radiación, resonancia magnética, Moessbauer Efecto.

The potential of eupraxia@sparc_lab for radiation based techniques

A proposal for building a Free Electron Laser, EuPRAXIA@SPARC_LAB, at the Laboratori Nazionali di Frascati, is at present under consideration. This FEL facility will provide a unique combination of a high brightness GeV-range electron beam generated in a X-band RF linac, a 0.5 PW-class laser system and the first FEL source driven by a plasma accelerator. The FEL will produce ultra-bright pulses, with up to 1012 photons/pulse, femtosecond timescale and wavelength down to 3 nm, which lies in the so called “water window”. The experimental activity will be focused on the realization of a plasma driven short wavelength FEL able to provide high-quality photons for a user beamline. In this paper, we describe the main classes of experiments that will be performed at the facility, including coherent diffraction imaging, soft X-ray absorption spectroscopy, Raman spectroscopy, Resonant Inelastic X-ray Scattering and photofragmentation measurements. These techniques will allow studying a variety of samples, both biological and inorganic, providing information about their structure and dynamical behavior. In this context, the possibility of inducing changes in samples via pump pulses leading to the stimulation of chemical reactions or the generation of coherent excitations would tremendously benefit from pulses in the soft X-ray region. High power synchronized optical lasers and a TeraHertz radiation source will indeed be made available for THz and pump–probe experiments and a split-and-delay station will allow performing XUV-XUV pump–probe experiments.Fil: Balerna, Antonella. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Bartocci, Samanta. Università degli studi di Sassari; ItaliaFil: Batignani, Giovanni. Università degli studi di Roma "La Sapienza"; ItaliaFil: Cianchi, Alessandro. Universita Tor Vergata; Italia. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Chiadroni, Enrica. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Coreno, Marcello. Istituto Nazionale Di Fisica Nucleare.; Italia. Istituto di Struttura della Materia; ItaliaFil: Cricenti, Antonio. Istituto di Struttura della Materia; ItaliaFil: Dabagov, Sultan. Istituto Nazionale Di Fisica Nucleare.; Italia. National Research Nuclear University; Rusia. Lebedev Physical Institute; RusiaFil: Di Cicco, Andrea. Universita Degli Di Camerino; ItaliaFil: Faiferri, Massimo. Università degli studi di Sassari; ItaliaFil: Ferrante, Carino. Università degli studi di Roma “La Sapienza”; Italia. Center for Life Nano Science @Sapienza; ItaliaFil: Ferrario, Massimo. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Fumero, Giuseppe. Università degli studi di Roma “La Sapienza”; ItaliaFil: Giannessi, Luca. Elettra-Sincrotrone Trieste; Italia. ENEA C.R. Frascati; ItaliaFil: Gunnella, Roberto. Universita Degli Di Camerino; ItaliaFil: Leani, Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Lupi, Stefano. Università degli studi di Roma “La Sapienza”; Italia. Istituto Nazionale di Fisica Nucleare (INFN) Sezione di Roma La Sapienza; ItaliaFil: Macis, Salvatore. Università degli Studi di Roma Tor Vergata; Italia. Istituto Nazionale di Fisica Nucleare (INFN) Sezione di Roma Tor Vergata; ItaliaFil: Manca, Rosa. Università degli studi di Sassari; ItaliaFil: Marcelli, Augusto. Istituto Nazionale Di Fisica Nucleare.; Italia. Consiglio Nazionale delle Ricerche; ItaliaFil: Masciovecchio, Claudio. Elettra-Sincrotrone Trieste; ItaliaFil: Minicucci, Marco. Universita Degli Di Camerino; ItaliaFil: Morante, Silvia. Universita Tor Vergata; Italia. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Perfetto, Enrico. Universita Tor Vergata; Italia. Consiglio Nazionale delle Ricerche; ItaliaFil: Petrarca, Massimo. Università degli studi di Roma "La Sapienza"; Italia. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Pusceddu, Fabrizio. Università degli studi di Sassari; ItaliaFil: Rezvani, Javad. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Robledo, José Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Rossi, Giancarlo. Centro Fermi—Museo Storico della Fisica e Centro Studi e Ricerche “Enrico Fermi”; Italia. Istituto Nazionale Di Fisica Nucleare.; Italia. Universita Tor Vergata; ItaliaFil: Sanchez, Hector Jorge. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Scopigno, Tullio. Center for Life Nano Science @Sapienza; Italia. Università degli studi di Roma "La Sapienza"; ItaliaFil: Stefanucci, Gianluca. Universita Tor Vergata; Italia. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Stellato, Francesco. Universita Tor Vergata; Italia. Istituto Nazionale Di Fisica Nucleare.; ItaliaFil: Trapananti, Angela. Universita Degli Di Camerino; ItaliaFil: Villa, Fabio. Istituto Nazionale Di Fisica Nucleare.; Itali

Energy dispersive inelastic X-ray scattering (EDIXS) spectroscopy: A review

This work presents an overview of a novel spectroscopic tool: Energy Dispersive Inelastic X-ray Scattering (EDIXS) spectroscopy. By the application of EDIXS, the local chemical environment of an element of interest can be characterized in a variety of experimental conditions. EDIXS makes use of core-level resonant inelastic X-ray scattering (RIXS), taking advantage of the benefits of an energy dispersive detection system and multivariate methods for the data analysis. As result, the proposed methodology presents a fast acquisition, energy-scanning free experiments, low self-absorption effects and an objective interpretation of the data. In this review a first section providing an introduction to the evolution of RIXS and the development of the EDIXS methodology is presented. After that, a theoretical frame from two different approaches is offered, presenting several aspects of the RIXS spectrum features and letting glimpse the origin of the peak fine structure, key issue of this technique. Next, an explanation of the different multivariate methods used for the data analysis is provided. By the end, a set of experimental results obtained with EDIXS are revised, including several irradiation geometries and setups (as total reflection, grazing incidence and even confocal) for a variety of samples. A brief summary with further discussions regarding the advantages of the presented methodology, including future perspectives as its applicability to different X-ray sources, are giving closure to the paper.Fil: Leani, Juan José. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; ArgentinaFil: Robledo, José Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; ArgentinaFil: Sanchez, Hector Jorge. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; Argentin

Quantitative speciation of manganese oxide mixtures by RIXS/RRS spectroscopy

Resonant inelastic X-ray scattering, also named X-ray resonant Raman scattering, was recently used to discriminate local chemical environments. By means of this novel technique, the speciation of samples could be attained in a variety of samples and experimental conditions. Until now, this discrimination methodology had been applied only to pure compounds, being the speciation possible by two different mathematical treatments. Nevertheless, the effectiveness/sensitivity of this technique has not been tested yet in samples containing mixtures of oxides of the same element. In this work, the first results of quantitative speciation of mixtures of manganese compounds, using resonant inelastic X-ray scattering/X-ray resonant Raman scattering spectroscopy, are presented. The results show that it is possible to discriminate and quantify oxide mixtures of the same element in slightly different proportions, allowing a quantitative speciation of compound mixtures in a variety of experimental conditions, presenting also several advantages over conventional spectroscopic techniques. Copyright © 2017 John Wiley & Sons, Ltd.Fil: Leani, Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; ArgentinaFil: Robledo, José Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; ArgentinaFil: Sanchez, Hector Jorge. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; Argentin

Exploratory Methodology for Retrieving Oxidation State Information from X-ray Resonant Raman Scattering Spectrometry

It has been observed recently that the resonant Raman scattering (RRS) peak of an X-ray spectrum contains information about the chemical environment of the irradiated matter. This information is extracted with complex processing of the spectrum data. Principal component analysis (PCA) is a statistical multivariate technique that allows exploring the variance-covariance structure of a set of data, through a few linear combinations of the original variables. This methodology can be applied to obtain information from RRS spectra. To analyze its potentiality, several measurements of different oxides in surface nanolayers were measured in total reflection conditions using synchrotron radiation. Multivariate analysis techniques, in particular, PCA, were used to obtain the information encrypted in the RRS peak, and to establish a new methodology, simpler and more accurate. The results show that multivariate analysis techniques are suitable for the analysis of this kind of spectra, foreseeing its application in future research.Fil: Robledo, José Ignacio. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Sanchez, Hector Jorge. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; Argentina. Consejo Nacional de Investigaciones Científicas y Técnicas; ArgentinaFil: Leani, Juan Jose. Nuclear Science And Instrumentation Laboratory; AustriaFil: Pérez, Carlos A.. Laboratorio Nacional de Luz Sincrotron; Brasi

3D-reconstruction of chemical state distributions in stratified samples by spatially resolved micro-X-ray resonant Raman spectroscopy

X-ray resonant Raman scattering was used, for the first time, in a confocal setup with the aim of determining different compounds of the same element in a copper-multilayer sample. This allowed us to resolve chemical environments with 3D-resolution using a detection system with low energy resolution. A stratified Cu-oxide-sample was studied in the Brazilian Synchrotron Light Laboratory (LNLS) using monochromatic radiation and an Energy Dispersive System (EDS) setup. The results are relevant since they allowed observing the presence of different oxide-layers, impossible to discriminate with conventional geometries of irradiation. They also permit the characterization of a compound present at a particular depth of the sample with micrometer resolution using a low-resolution system.Fil: Leani, Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Perez, Roberto Daniel. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; ArgentinaFil: Robledo, José Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; ArgentinaFil: Sanchez, Hector Jorge. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentin

Energy-Dispersive Total-Reflection Resonant Inelastic X-ray Scattering as a Tool for Elemental Speciation in Contaminated Water

This work presents a state-of the-art analytical methodology, by which chemical state information on metallic elements is obtained for liquid samples in a fast and simple manner. This method overcomes limitations of conventional X-ray techniques, such as X-ray absorption spectroscopy, by applying resonant inelastic X-ray scattering under total reflection geometry (TRIXS). TRIXS is particularly applicable for the analysis of small quantity of liquid samples deposited on polished reflectors. This feature is relevant for the chemical speciation of metallic trace elements contained in water samples, since the degree of their toxicity depends crucially on the concentration of specific chemical species included. The analytical merits of the proposed methodology were studied at Elettra Sincrotrone Trieste and at the Brazilian Synchrotron Light Laboratory. Contaminated water samples with low concentration of different chromium and manganese compounds were measured. Results prove the analytical potential of the TRIXS technique in characterizing different chemical species of metallic elements in water samples.Fil: Robledo, José Ignacio. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; ArgentinaFil: Leani, Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; ArgentinaFil: Karydas, Andreas G.. International Atomic Energy Agency; Austria. National Center for Scientific Research “Demokritos”. Institute of Nuclear and Particle Physics; GreciaFil: Migliori, A. International Atomic Energy Agency; AustriaFil: Pérez, Carlos A.. Brazilian Synchrotron Light Source; BrasilFil: Sanchez, Hector Jorge. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Córdoba. Instituto de Física Enrique Gaviola. Universidad Nacional de Córdoba. Instituto de Física Enrique Gaviola; Argentina. Universidad Nacional de Córdoba. Facultad de Matemática, Astronomía y Física; Argentin

A first evaluation of the analytical capabilities of the new X-ray fluorescence facility at International Atomic Energy Agency-Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis

Summarization: The aim of the work is to present a systematic evaluation of the analytical capabilities of the new X-ray fluorescence facility jointly operated between the International Atomic Energy Agency and the Elettra Sincrotrone Trieste for multipurpose total reflection X-ray fluorescence analysis. The analytical performance of the XRF beamline end-station (IAEAXspe) was systematically evaluated under TXRF excitation geometry by analyzing different types of aqueous (lake, waste and fresh water) and solid (soil, vegetal, biological) certified reference materials using an excitation energy of 13.0 keV (for the purpose of multielemental analysis). The results obtained for both types of samples in terms of limits of detection and accuracy were also compared with those obtained using laboratory X-ray tube based TXRF systems with different features (including Mo and W X-ray tube systems). Taking advantage of the possibility to work under high vacuum, the IAEAXspe set-up instrumental sensitivity was also determined using an excitation energy of 6.2 keV to explore the possibilities for light elements determination. A clear improvement of the element detection limits is achieved when comparing this facility to conventional X-ray tube based TXRF systems highlighting the benefits of using the monoenergetic synchrotron exciting radiation and the ultra-high vacuum chamber in comparison with conventional laboratory systems. The results of the present work are discussed in view of further exploitation of the facility for different environmental and biological related applications.Presented on