Description and contextualization of the subject

This course will review the fundamentals of advanced characterization techniques using large-scale facilities (unique or exceptional scientific infrastructures with relatively high investment and maintenance costs, such as synchrotrons and neutron facilities) for the chemical, structural, microstructural, surface, interfacial, and kinetic study of materials for electrochemical energy storage. The course will address why, where, and when large-scale facilities are used, providing an overview of available techniques and their suitability/limitations for in-situ/operando studies. Additionally, proposal examples for beam time applications and results will be analyzed.

Advanced tools will be provided for the analysis and interpretation of data related to the main physical-chemical characterization techniques:

Learning outcomes of the subject

Knowledge or content:

RCO6: Knowledge of the fundamentals of in-situ electrochemical cell design and the details of in-situ and operando experimental set-up.

RCO7: Knowledge of available large-scale facilities and their applications to the study of electrochemical energy storage materials.



Abilities or skills:

RHT2: Skills in choosing the appropriate characterisation technique to obtain, with the aid of specific software, the information required to understand certain properties of a material, or to solve a given problem.

Ordinary call: orientations and renunciation

The final grade for the course will be calculated as follows:

-Practical Work: 20%

-Final Written Exam: 80%

Conditions/Restrictions: A minimum of 5 out of 10 points is required in both blocks to pass.

Extraordinary call: orientations and renunciation

Students who do not pass the ordinary session will be evaluated solely through a final exam in the extraordinary session.

Conditions/Restrictions: A minimum of 5 out of 10 points is required to pass.

Temary

1- Large scale facilities in EU and worldwide

Why, where and when using large scale facilities, overview of available techniques

2- Electrochemical in-situ/operando measurements

In-situ electrochemical cell designs, overview of most commonly used techniques, specificities of time resolved experiments: in-situ vs operando

3- Structural studies ¿ in-situ/operando X-ray and neutron diffraction

Neutron vs synchrotron radiation, sequential diffraction pattern analysis, investigation of charge-discharge mechanisms

4- Spectroscopic studies ¿ in-situ/operando X-ray, ion and electron spectroscopies

X-ray absorption spectroscopy: near edge structure (XANES) and extended fine structure (EXAFS). Spectra simulation and fitting.

Ion scattering spectroscopy: buried interfaces and depth profiling. Probing light elements.

X-ray photoemission spectroscopy: compositional and chemical information of surface and subsurface regions. Peak fitting and principal component analysis. Application to solid electrolyte interphase study.

5- Proposal preparation

Procedures for accessing beam time, planning an experiment, guidelines for proposal preparation, examples of proposals.

Bibliography

Compulsory materials

Students will have access to the course content, lab guides, and supplementary readings on the eGela platform.

Basic bibliography

- Gordon J. Kearley & Vanessa K. Peterson (2015), Neutron Applications in Materials for Energy, Wiley, ISBN: 978-3-319-06655-4

- Philip Willmott (2011), An Introduction to Synchrotron Radiation: Techniques and Applications, Wiley, ISBN: 978-1-119-97286-0

- Jeroen A. van Bokhoven & Carlo Lamberti (2016), X-Ray Absorption and X-Ray Emission Spectroscopy: Theory and Applications, ISBN: 978-1-118-84423-6

- J. Wayne Rabalais (2002), Principles and Applications of Ion Scattering Spectrometry: Surface Chemical and Structural Analysis, Wiley, ISBN: 978-0-471-20277-6.

- Stefan Hüfner (2003), Photoelectron Spectroscopy: Principles and Applications, Springer, ISBN-13: 978-3540418023.

In-depth bibliography

- Gordon J. Kearley & Vanessa K. Peterson (2015), Neutron Applications in Materials for Energy, Wiley, ISBN: 978-3-319-06655-4



- Margaritondo, G. (1988). Introduction to Synchrotron Radiation. New York: Oxford University Press.



- Saldin, E., Schneidmiller, E. & Yurkov, M. (2000). The Physics of the Free Electron Laser. Berlin: Springer.



- J. Als-Nielsen and D. McMorrow (2009), Elements of Modern X-ray Physics, Wiley, New York.



- J.D. Jackson, Classical Electrodynamics (1999), Wiley, New York.



- D. C. Koningsberger and R. Prins (1988), X-ray Absorption: Principles, Applications, Techniques of EXAFS, SEXAFS, and XANES, John Wiley & Sons.

Journals

El alumnado dispondrá en la plataforma eGela de diversos artículos científicos relacionados con el contenido de la asignatura.

Links

http://www.pascal-man.com/



https://www.ill.eu/sites/fullprof/



https://www.ill.eu/



http://xdb.lbl.gov/



http://henke.lbl.gov/optical_constants/



https://srdata.nist.gov/xps/



https://www.albasynchrotron.es



https://als.lbl.gov/



https://www.aps.anl.gov/



https://www.diamond.ac.uk/Home.html



http://www.elettra.eu/lightsources/elettra.html



http://www.esrf.eu/



https://www.maxiv.lu.se/



http://photon-science.desy.de/



https://www.psi.ch/fr/sls



https://www.xfel.eu/