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X-ray spectroscopies

This course is part of the programme
Materials Science

Objectives and competences

Main goal of the course is to gain knowledge to understand and use different x-ray methods for characterisation of atomic and molecular structure of materials. Students can choose adequate experimental methods for structural characterisation actively participate at experiments and critically evaluate the obtained results of the analysis.

Content

• Source of X-rays (classic and synchrotron radiation)
• Interaction of x-rays with matter (photoeffect, Compton effect, elastic scattering, Auger effect)
• Detectors for X-rays
• Optical elements for X-rays (mirrors, monochromators, (micro)focusing elements)
• X-ray diffraction, small angle scattering
• X-ray fluorescence
• X-ray absorption spectroscopy
• Introduction to analysis of atomic and molecular structure with x-ray spectroscopic methods.
• Micro-spectroscopy (combination of XAS and micro focusing of SR X-ray beam) and 2D elemental mapping with sub-micron resolution.
• In-situ in in-operando spectroscopic techniques with X-rays

Intended learning outcomes

Knowledge and understanding:
Students learn the principles of interaction of X- rays with matter. They gain knowledge about characteristics of most important X-ray sources (x-ray tubes, synchrotron radiation sources).
They understand the operation of main optical elements and detectors for X-rays. They understand the principles of X-ray diffraction (XRD), X-ray fluorescence and X-ray absorption spectroscopy, know the necessary experimental equipment, and understand basic methods for analysis and interpretation of measured spectra, and understand what kind of structural information about the investigated material can be obtained by individual spectroscopic methods.

Readings

  • Openly licensed textbooks at OpenStax, Rice University, Huston Texas, USA: https://openstax.org/subjects/science
  • University Physics: Volume 3. E-version
  • G. Bunker, "Introduction to XAFS: A Practical Guide to X-ray Absorption Fine Structure Spectroscopy", Cambridge University Press, 2010. Catalogue
  • Y. Iwasawa, K. Asakura, M. Tada, XAFS Techniques for catalysts, Nanomaterials, and Surfaces, Springer (2017). Catalogue
  • X-ray absorption spectroscopy (principles, applications, techniques of EXAFS, SEXAFS and XANES), edited by D.C. Konnigsberger and R. Prins, John Wiley and Sons, NY (1988).
  • F. Cvelbar, Merjenje ionizirajočega sevanja, DMFA – založništvo, Ljubljana 2003. Catalogue
  • D. A. Skoog, F. J. Holler, T. A. Nieman, Principles of Instrumental analysis, Saunders Colege Publishing, Philadelpia, 1998. Catalogue
  • W. H. Press, B. P. Flannery, S. A. Teukolsky, W. T. Vettering, Numerical Recipes, Cambridge University press, Cambridge, 1986. Catalogue
  • S. L. Meyer, Data analysis for scientists and engineers, J. Wiley and Sons (1975) Catalogue
  • I. Arčon, Introduction to XANES and EXAFS analysis. Nova Gorica: [I. Arčon], 2008. Catalogue
  • Katarina Vogel-Mikuš, Iztok Arčon, Peter Kump, Primož Pelicon, Marijan Nečemer, Primož Vavpetič, Špela Koren, Marjana Regvar, Analytical tools for exploring metal accumulation and tolerance in plants. Phytotechnologies : remediation of environmental contaminants. Boca Raton (FL): Taylor & Francis (2013) 443-495. E-version
  • B. Beckhoff, B. Kanngiesser, N. Langhoff R. Wedell H. Wolff, Handbook of Practical X-Ray Fluorescence Analysis, Springer-Verlag Berlin Heidelberg 2006, ISBN-10 3-540-28603-9 Springer Berlin, Heidelberg. E-version
  • Larch software and documentation (freeware XAS analysis software). E-version

Assessment

Homeworks and final oral exam.
During the course student prepares reports on the results of the analysis of XAS spectra in a written form and defends it orally in an open discussion with professor and students.

Lecturer's references

Prof. dr. Iztok Arčon je redni profesor za področje fizike, redno zaposlen na Univerzi v Novi Gorici v Laboratoriju za kvantno optiko. Njegova raziskovalno področje so analize atomske oziroma molekularne strukture novih funkcionalnih nano-materialov (različni (foto)katalizatorji, baterije in drugi materiali za shranjevanje energije, feroelektriki ) ter za raziskave onesnaženja okolja (prsti, vode in rastlin) s težkimi kovinami, z rentgensko absorpcijsko spektrometrijo s sinhrotronsko svetlobo. Raziskovalno delo opravlja pri različnih evropskih sinhrotronskih laboratorijih (Elettra v Trsu, Petra III v Hamburgu, ESRF v Grenoblu,
Soleil v Parizu). Za raziskovalno delo je v letu 2006 prejel Zoisovo priznanje za vrhunske
raziskovalne dosežke na področju rentgenske absorpcijske spektrometrije in leta 2020 Preglovo nagrado za izjemne dosežke na področju rentgenske absorpcijske spektrometrije. Do leta 2022 je objavil preko 200 znastvenih člankov v revijah z visokom faktorjem upliva. Njegovo delo je visoko citirano (preko 3500 čistih citatov), njegov Hirschev indeks je 30.

Prof. dr. Iztok Arčon is full professor for the field of physics, employed at the University of Nova Gorica, Laboratory for quantum optics, holding a position of the dean of Grauate school. His main research field is analysis of atomic and molecular structure of new functional materials (different catalysts and photocatalysts, cathode materials for Li-ion, Li-sulphur and Mg-sulphur batteries, ferroelectric and ferromagnetic ceramics, …) and analysis of environmental pollution (soil, water and plants), with X-ray absorption spectroscopy with synchrotron radiation (methods XANES, EXAFS), In addition, he uses synchrotron radiation for experimental study of multielectron photoexcitations in free and bound atoms, to provide information on collective motion of electrons in the atomic system, and exact atomic absorption background in EXAFS spectra. He obtained with coworkers over sixty research projects at different European synchrotron radiation laboratories (PETRA III at DESY, Hamburg; Elettra, Trieste; ESRF, Grenoble; Alba in Barcelona; Soleil, and previously Lure, Paris), and performed experiments with advanced sychrotron radiation techniques. Until 2022 he published more than 200 scientific papers in reviews with high impact factor and his work is highly cited (over 3500 citations). His Hirsch index is 30.
He received The Jožef Stefan Golden Emblem Prize Award in 1996 for his PhD thesis research work. In 2006 he was awarded the national “Zois award” for outstanding achievements in the field of X-ray absorption spectroscopy, and in 2020 he received Pregl Award of the National institute of Chemistry for Exceptional Achievements in the field of chemistry and related disciplines. https://www2.ung.si/~arcon/xas/aboutus/iarconcv.htm

Izbrane objave /selected publications
1) ZABILSKY, Maxim, ARČON, Iztok, DJINOVIĆ, Petar, TCHERNYCHOVA, Elena,
PINTAR, Albin. In-situ XAS study of catalytic N2ON2O decomposition
over CuO/CeO2CuO/CeO2 catalysts. ChemCatChem. 2021, vol. 13, iss. 7, str. 1814-1823,. DOI: 10.1002/cctc.202001829.
2) LUIN, Uroš, ARČON, Iztok, VALANT, Matjaž. Structure and population of complex ionic species in FeCl2FeCl2 aqueous solution by X-ray absorption spectroscopy. Molecules. Feb. 2022, vol. 27, iss. 3, str. 1-13, ilustr. ISSN 1420-3049. DOI: 10.3390/molecules27030642.
3) MAVER, Ksenija, ARČON, Iztok, FANETTI, Mattia, AL JITAN, Samar, PALMISANO,
Giovanni, VALANT, Matjaž, LAVRENČIČ ŠTANGAR, Urška. Improved photocatalytic activity of SnO2SnO2-TiO2TiO2 nanocomposite thin films prepared by low-temperature sol-gel method. Catalysis today.. DOI: 10.1016/j.cattod.2021.06.018
4) KODRE, Alojz, ARČON, Iztok, PADEŽNIK GOMILŠEK, Jana. Photoexcitation processes in atoms. V: CHANTLER, C. T. (ur.). International tables for crystallography. Volume I,
X-ray absorption spectroscopy and related techniques. 1st ed. Bognor Regis; Weinheim; Indianapolis: Wiley. 2021, str. 1-5, International tables for crystallography. ISBN 978-1- 119-43394-1. ISSN 1574-8707. DOI: 10.1107/S1574870720003511.
5) POTISEK, Mateja, LIKAR, Matevž, VOGEL-MIKUŠ, Katarina, ARČON, Iztok, GRDADOLNIK,
Jože, REGVAR, Marjana. 1,8-dihydroxy naphthalene (DHN) - melanin confers tolerance to cadmium in isolates of melanised dark septate endophytes. Ecotoxicology and environmental safety. 2021, vol. 222, str. 1-9. ISSN 0147-6513. DOI: 10.1016/j.ecoenv.2021.112493.
6) PONGRAC, Paula, ARČON, Iztok, CASTILLO MICHEL, Hiram, VOGEL-MIKUŠ, Katarina.
Mineral element composition in grain of awned and awnletted wheat (Triticum aestivum L.) cultivars : tissue-specific iron speciation and phytate and non-phytate ligand ratio.
Plants, ISSN 2223-7747, 2020, vol. 9, no. 1, str. 79-1-97-14, doi: 10.3390/plants9010079.
7) SCAFURI, Antonio, BERTHELOT, Romain, PIRNAT, Klemen, VIŽINTIN, Alen, BITENC, Jan,
AQUILANTI, Giuliana, FOIX, Dominique, DEDRYVÈRE, Rémi, ARČON, Iztok, DOMINKO, Robert, STIEVANO, Lorenzo. Spectroscopic insights into the electrochemical mechanism of rechargeable calcium/sulfur batteries. Chemistry of materials. 13 Oct. 2020, vol. 32, no.
19, str. 8266-8275, DOI: 10.1021/acs.chemmater.0c02074.