66188 - Analysis of Surfaces and X-Ray Spectroscopies

Academic Year 2022/2023

Course contents

Prerequisites

To successfully attend this class, the student should know:

  • the basic of x-rays and x-ray diffraction (course: “X-Ray Diffraction” at the University of Lille)
  • the basic of the absorption and emission of electromagnetic radiation
  • the beer lambert law for absorption

Content

Introduction to the course.

X-rays: origin and generation. X-ray absorption coefficient and mass absorption coefficient. Calculations and examples on mass absorption coefficient. Decay of the core-hole: x-ray Fluorescence and Auger effect.

X-ray absorption spectroscopy and the acronyms XANES, EXAFS, SEXAFS, NEXAFS. Theory: The EXAFS equation and the key approximations: one electron, plane wave, and K-threshold. Muffin-Tin and many body effects. Debye-Waller EXAFS factor and disorder.

X-Ray Fluorescence spectroscopy. Resonant Inelastic X-ray Scattering.

X-Ray Microscopy.

Experimental methods for Absorption and Emission. Synchrotron radiation. XAS Spectroelectrochemistry and cells for in-situ measurements. Operando studies.

Data Analysis. XANES calculations ad EXAFS fittings. Primary data reduction: extraction of the (k) and Fourier Transformation. Data analysis using fitting approach. Chemometry for spectroscopy. Use of Multivariate Curve Resolution - Alternating Least Square (MCR-ALS) algorithm for the analysis of operando data collection.

Applications in the field of solution chemistry, surfaces, catalysis, batteries, inorganic and biological materials.

The course is completed by one laboratory (practical) using the X-Ray Fluorescence spectrometer.

Readings/Bibliography

G. Bunker, “Introduction to XAFS” Cambridge University Press, 2010. ISBN: 978-0-521-76775-0

Marco Giorgetti (2013). "A Review on the Structural Studies of Batteries and Host Materials by X-Ray Absorption Spectroscopy". Free download at: https://www.hindawi.com/journals/isrn/2013/938625/cta/

Marco Giorgetti and Lorenzo Stievano (2017). "X-Ray Absorption Spectroscopy Study of Battery Materials". Free download at: https://www.intechopen.com/chapter/pdf-download/53744

Dino Tonti, Mara Olivares-Marín, Andrea Sorrentino and Eva Pereiro (2017). "Studies of Lithium-Oxygen Battery Electrodes by Energy- Dependent Full-Field Transmission Soft X-Ray Microscopy". Free download at: https://www.intechopen.com/chapter/pdf-download/53739

Other specific material will be given by the teacher.

Teaching methods

The course describes the potentiality of both X-Ray Absorption and X-Ray Emission as an electronic and structural tools for the study of the condensed, crystalline, solution and amorphous phases, also including Operando experiments. Front lectures and exercitation will be the offered with several examples concerning basic data analysis and interpretation of spectra.

As concerns the practical experiences of this course, all students must attend Module 1, 2 [https://www.unibo.it/en/services-and-opportunities/health-and-assistance/health-and-safety/online-course-on-health-and-safety-in-study-and-internship-areas] online, while Module 3 on health and safety is to be attended in class. Information about Module 3 attendance schedule is available on the website of the degree programme.

Assessment methods

The exam (single session, about 30 minutes) is composed of two parts:

a) Oral presentation on a selected topic learned during the course using 10-15 slides (15 points)

b) Oral exam (15 points).

Teaching tools

Lecture slides and other material useful for exam preparation are made available to the student electronically on the IOL platform.

Students take notes during the lessons (the teachers will use the blackboard/whiteboard).

Access to students with disabilities is provided

Office hours

See the website of Marco Giorgetti

SDGs

Quality education Climate Action

This teaching activity contributes to the achievement of the Sustainable Development Goals of the UN 2030 Agenda.