Description and contextualization of the subject

In this subject the fundamentals of advanced characterization and characterization in large instruments (unique or exceptional scientific infrastructures with a relatively large investment and maintenance cost such as synchrotrons and neutron reactors) will be reviewed for the structural, microstructural, surface, interfacial and kinetic study of materials for electrochemical energy storage. Why, where and when large-scale facilities are used will be addressed, and an overview of available techniques and their suitability / limitations for in-situ studies will be offered. Examples of proposals will be analyzed to request beam time and examples of results will be given.



Advanced tools for the analysis and interpretation of data related to the following techniques will be provided:



i) X-ray powder diffraction (PXRD) and neutron powder diffraction (NPD) for the study of crystalline structures;

ii) Small-angle X-ray scattering (SAXS) for the microstructural and morphological study at nanometric scale of microporous materials;

iii) photoelectron spectroscopy for the study of compositional and chemical information of surface and subsurface regions and of chemical environment with lateral resolution (photoemission spectroscopy (XPS), high energy refinements (HAXPES) and ambient pressure (NAP-XPS), XPS imaging and Auger microscopy (SAM));

iv) X-ray absorption spectroscopy for chemical and structural analysis (near- edge structure (XANES) and extended fine structure (EXAFS));

v) ion scattering spectroscopy for the study of buried interfaces, depth-profiling and light elements probing;

vi) solid state NMR spectroscopy for structural, physicochemical and kinetic information.

Learning outcomes of the subject

- Basic knowledge about synchrotrons, how their radiation is generated and general features, difference from conventional X-ray sources in a laboratory.

- Know the basic theoretical concepts of the main techniques, their possibilities and limitations based on the different methods of detection, being able to select the most suitable one for each practical case; and to interpret their results

- Learn to use specific software tool for the analysis of the results of the main techniques

- Know the basics of in-situ electrochemical cell design and the specifics of in-situ and operando experiment setup

Ordinary call: orientations and renunciation

Written exam: 80%

Laboratory practices: 20%





A written test will be performed once the subject is finished. The test will be divided into four blocks:



• Large facilities

• Diffraction techniques

• Spectroscopic techniques

• Nuclear magnetic resonance



Each block will score over 20 points adding a maximum of 80. It is necessary to obtain 10 points in each block to take into account the written test score for the calculation of the final mark.



Laboratory practices will be divided into two blocks: (i) diffraction data analysis and (ii) analysis of spectroscopy data. Each block will score on 10 points adding a total of 20. The result of the practical test will be added to the written test note setting the final score on a maximum of 100 points.

Extraordinary call: orientations and renunciation

The procedure indicated in the ordinary call will be followed. Students who have not passed or have declined the activities to assess the learning outcomes throughout the course (laboratory practices, exercises, etc.) should be examined in the corresponding competences through an additional oral test in this extraordinary convocation.

Temary

1- Large facilities in the EU and around the world.

2- X-ray powder and neutron Powder Diffraction. Small Angle X-ray Scattering. Structural studies - in-situ.

3- X-ray, ion and electron spectroscopies.

4- Solid state NMR spectroscopy.

5- Proposals Preparation to request beam time.

Bibliography

Compulsory materials

Students should use the collections of issues and problems that teachers will publish at the beginning of the course, and for each topic, on the eGela platform.







The student will have on the eGela platform, of the subject matter and of the practical scripts in electronic format to favor the understanding of the subjects and the agile follow-up of the classes.

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.



- R.A. Young (1995) The Rietveld method, Oxford University Press.

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/