Graduate School

Structural analysis of materials with x-ray absorption spectroscopy

This course is part of the programme:
Physics (Third Level)

Objectives and competences

The primary goal of this course is to give students the knowledge of modern synchrotron radiation (SR) x-ray absorption and emission spectroscopic methods for the autonomous characterization of the atomic and molecular structure of different materials, from preparation of project to obtain beamtime in SR laboratories, preparation and realization of the experiment, to quantitative analysis of measured spectra and interpretation of results.

Prerequisites

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Content (Syllabus outline)

    • Interaction of x-rays with matter
    • EXAFS and XANES spectroscopy
    • X-ray absorption measurements with synchrotron radiation in transmission and fluorescence mode, X-ray detectors, optic elements, in-situ experiments
    • Micro-spectroscopy (combination of XAS and micro focusing of SR X-ray beam)
    • Numerical analysis of EXAFS and XANES spectra
    • Atomic absorption background in XAS spectra.
    • Advanced analytical methods (parallel multiedge fitting of several EXAFS spectra, linear combination fits in XANES analysis
    • Typical examples of structure analysis: catalysts, nanomaterials, liquids, strongly disordered materials, environmental and biological samples, cultural heritage
    • Related x-ray absorption and XRF techniques with SR, 2D elemental mapping with sub-micron resolution.

Intended learning outcomes

Students learn the principles of different x-ray spectroscopic methods (EXAFS, XANES, micro-XAFS, …) and their use in practice as structural tools. Students gain know-how on the whole process from preparation and realisation of XAS experiments at synchrotron radiation laboratories, to the analysis and finally the interpretation of XAS spectra. With practical work on examples from research practice using up-to-date XAS software, they learn advanced techniques of the evaluation and interpretation of obtained XAS results. They obtain know-how necessary to prepare a good proposal for beamtime and to perform successful experiments at XAS beamlies at different synchrotron radiation facilities. Students learn which combination of spectroscopic methods is optimal for the analysis of specific material properties.

Readings

    • G. Bunker, Introduction to XAFS: A Practical Guide to X-ray Absorption Fine Structure Spectroscopy, Cambridge University Press, 2010
    • D.C. Konnigsberger and R. Prins (eds.), X-ray absorption spectroscopy, Wiley&Sons, 1988
    • J. J. Rehr, R. C. Albers, Theoretical approaches to x-ray absorption fine structure, Reviews of Modern Physics, Vol. 72, No. 3, July 2000, 621-654
    • J. Wong, F.W. Lytle, R. P. Messmer, D.H. Maylotte, K-edge spectra of slected vanadium compounds, Phys. Rev. B 30 (1984) 5596 – 5610
    • K. Vogel-Mikuš, P. Kump, M. Nečemer, P. Pelicon, I. Arčon, P. Pongrac, B. Povh, M. Regvar, Quantitative analyses of trace elements in environmental samples : options and (im)possibilities. Soil heavy metals, (Soil biology, 19). Heidelberg [etc.]: Springer, 2010, str. 113-138.
    • I. Arčon, Introduction to XANES and EXAFS analysis. Nova Gorica: [I. Arčon], 2008. 35 str., ilustr. [COBISS.SI-ID 933883]
    • I. Arčon, X-ray absorption spectroscopy : a practical guide to structural analysis of materials with EXAFS and XANES analysis. Nova Gorica: [I. Arčon], 2008 [COBISS.SI-ID 934139]
    • V. Kaučič, N. Zabukovec Logar, I. Arčon, Characterisation of microporous and mesoporous solids using complementary diffraction and X-ray absorption spectroscopic techniques, Characterization techniques for zeolites and related materials : state of the art and recent developments, 2nd FEZA school 2008, Universite Pierre et marie Curie, Paris, September 1-2, 2008 [COBISS.SI-ID 3992602]
    • I. Arčon, tutorials on the web: http://www.p-ng.si/~arcon/xas and http://www.ung.si/~arcon/xas-si and http://www.ung.si/~arcon/xas/students
    • IFEFFIT software and documentation for XAS analysis: http://cars.uchicago.edu/ifeffit/Ifeffit
    • DEMETER software and documentation (XAS software) http://bruceravel.github.com/demeter/
    • FEFF documentations: http://leonardo.phys.washington.edu/feff/

Assessment

During the course students prepare five individual projects of EXAFS and XANES analysis on real data from research practice. At the end of course they prepare a final project, i.e. experiment proposal for beamtime at a selected synchrotron X-ray absoprtion beamline. All projects are prepared in a written form and defend orally in an open discussion with professor and students. (50/50)

Lecturer's references

Prof. dr. Iztok Arčon is a full professor for the field of physics, employed at the University of Nova Gorica.

1.ARČON, Iztok, PICCOLO, Oreste, PAGANELLI, Stefano, BALDI, Franco. XAS analysis of a nanostructured iron polysaccharide produced anaerobically by a strain of Klebsiella oxytoca. Biometals, ISSN 0966-0844, 2012, vol. 25, no. 5, str. 875-881, doi: 10.1007/s10534-012-9554-6. [COBISS.SI-ID

2264827]

2.DOMINKO, Robert, ARČON, Iztok, KODRE, Alojz, HANŽEL, Darko, GABERŠČEK, Miran. In-situ XAS study on Li[sub]2MnSiO[sub]4 and Li[sub]2FeSiO[sub]4 cathode materials. V: Selected papers presented at the 14th international meeting on lithium batteries : Tianjin, China, 22 -28 June 2008 :

IMLB-2008, (Journal of power sources, ISSN 0378-7753, Vol. 189, Issue 1, 2009). Lausanne: Elsevier, 2009, vol. 189, no. 1, str. 51-58, doi: 10.1016/j.jpowsour.2008.11.077. [COBISS.SI-ID 1073915],

3. VALANT, Matjaž, KOLODIAZHNYI, Taras, ARČON, Iztok, AGUESSE, Frederic, AXELSSON, Anna-Karin, ALFORD, Neil McN. The origin of magnetism in Mn-doped SrTiO [sub] 3. Advanced functional materials, ISSN 1616-301X, maj 2012, vol. 22, no. 10, str. 2114-2122. [COBISS.SI-ID 2265083],

4. ARČON, Iztok, KOLAR, Jana, KODRE, Alojz, HANŽEL, Darko, STRLIČ, Matija. XANES analysis of Fe valence in iron gall inks. X-ray spectrometry, ISSN 0049-8246, 2007, vol. 36, str. 199-205. [COBISS.SI-ID 665339],

5. VOGEL-MIKUŠ, Katarina, ARČON, Iztok, KUMP, Peter, PELICON, Primož, NEČEMER, Marijan, VAVPETIČ, Primož, KOREN, Špela, REGVAR, Marjana. Analytical tools for exploring metal accumulation and tolerance in plants. V: ANJUM, Naser A. (ur.). Phytotechnologies : remediation of environmental contaminants. Boca Raton (FL): Taylor & Francis, cop. 2013, str. 443-495, ilustr. [COBISS.SI-ID 2671439]

University course code: 3FIi01

Year of study: 2

Lecturer:

ECTS: 9

Course type: elective

Languages: english

Learning and teaching methods:
lectures, exercises on state of the art software for the analysis of xas spectra under supervision of the the lecturer responsible for the course, individual project work under supervision of the lecturer responsible for the course, presentation and interpreation of project results to other students in open discussion under supervision of the lecturer responsible for the course, journal club – discussion of published research articles on the selected xas topic