School of Science

Diffraction characterisation methods

This course is part of the programme:
Material Science

Objectives and competences

The primary goal of this course is to give students the theoretical and practical knowledge in crystallography and X-ray diffraction methods needed for the characterization of the structure of different crystalline materials.

Prerequisites

Knowledge and understanding:

Students learn the principles of symmetry in crystals, diffraction and diffraction methods, with emphasis on X-ray powder diffraction. They learn how to use X-ray diffraction methods, theoretically the preparation of the sample and performing the measurement, and practically about the analysis and interpretation of the results. In practical projects students gain knowledge how to use the specialized software for diffraction analysis. With practical work on examples from research practice they learn the evaluation and interpretation of XRD data.

Content (Syllabus outline)

The course deals with the basics of diffraction methods for the characterization of materials with emphasis on advanced X-ray diffraction methods.

The course includes the topics of:

  • Symmetry in crystals (crystal lattice, unit cell, symmetry elements and operations, point and space groups, crystal structure)
  • X-ray diffraction in crystals (crystal planes, Muller indices, interference of scattered waves, Bragg condition, reciprocal lattice, diffraction characteristics of the polycrystalline materials)
  • Determination and optimization of the crystal structure (structure factor, phase problem, Fourier transform (FT), optimization of the structural model, database)
  • X-ray powder diffraction (powder diffractometer, powder pattern, qualitative and quantitative analysis, Rietveld analysis)
  • Other diffraction methods (neutron diffraction, electron diffraction. synchrotron radiation and diffraction)
  • Structural characteristics of crystals (ionic, covalent and metallic crystals, errors in crystals, etc.)

Intended learning outcomes

Knowledge and understanding:

Students learn the principles of symmetry in crystals, diffraction and diffraction methods, with emphasis on X-ray powder diffraction. They learn how to use X-ray diffraction methods, theoretically the preparation of the sample and performing the measurement, and practically about the analysis and interpretation of the results. In practical projects students gain knowledge how to use the specialized software for diffraction analysis. With practical work on examples from research practice they learn the evaluation and interpretation of XRD data.

Readings

  • V.K. Pecharsky in P.Y. Zavalij: Fundamentals of Powder Diffraction and Structural Characterization of Materials, Springer, New York, 2005.
  • W. Clegg, Crystal Structure Determination, Oxford University Press, Oxford, 1998.
  • C. Hammond, The Basics of Crystallography and Diffraction, Third Edition, Oxford University Press, Oxford, 2009.
  • C. Giacovazzo, H. L. Monaco, G. Artioli, D. Viterbo, M. Milanesio, G. Ferraris, G. Gilli, P. Gilli, G. Zanotti and M. Catti, Fundamentals of Crystallography, Third Edition, Oxford University Press, Oxford, 2011.
  • N. Zabukovec Logar, tutorials in slovene language on the web: http://www.ki.si/index.php?id=1696
  • X’Pert HighScore Plus tutorial – PANalytical on the web: http://www.panalytical.com
  • TOPAS ACADEMIC tutorial on the web http://www.topas-academic.net/

Assessment

Written exam, Seminar presentation of selected topics for professors and students, Short individual project prepared in written form (qualitative and quantitative analysis of the X-ray powder pattern of unknown sample and crystal structure determination from single-crystal X-ray data)

Lecturer's references

Prof. dr. Nataša Zabukovec Logar:

Full Professor of Chemistry at the University of Nova Gorica.

Nataša Zabukovec Logar is a Head of Department for Inorganic Chemistry and Technology at the National Institute of Chemistry in Ljubljana. Her current research focusses are development of new metal-organic and inorganic porous materials for gas and heat storage and studies of sorption mechanisms of metals on natural and synthetic zeolites for water treatment.

Selected publications:

1. KRAJNC, Andraž, KOS, Tomaž, ZABUKOVEC LOGAR, Nataša, MALI, Gregor. A simple NMR-based method for studying the spatial distribution of linkers within mixed-linker metal-organic frameworks. Angewandte Chemie, ISSN 1433-7851. [Print ed.], Sep. 2015, vol. 54, iss. 36, str. 10535-10538. doi: 10.1002/anie.201504426. [COBISS.SI-ID 5735962]

4. BIRSA ČELIČ, Tadeja, RANGUS, Mojca, LAZAR, Karoly, KAUČIČ, Venčeslav, ZABUKOVEC LOGAR, Nataša. Spectroscopic evidence for the structure directing role of the solvent in the synthesis of two iron carboxylates. Angew. Chem. (Int. ed., Print). [Print ed.], 2012, vol. 51, iss. 50, str. 12490-12494, ilustr., doi: 10.1002/anie.201204573. [COBISS.SI-ID 36300805]

6. MAZAJ, Matjaž, BIRSA ČELIČ, Tadeja, MALI, Gregor, RANGUS, Mojca, KAUČIČ, Venčeslav, ZABUKOVEC LOGAR, Nataša. Control of the crystallization process and structure dimensionality of Mg-benzene-1,3,5-tricarboxylates by tuning solvent composition. Cryst. growth des., 2013, vol. 13, iss. 8, str. 3825-3834. doi: 10.1021/cg400929z. [COBISS.SI-ID 5290522]

7. MAZAJ, Matjaž, MALI, Gregor, RANGUS, Mojca, ŽUNKOVIČ, Emanuela, KAUČIČ, Venčeslav, ZABUKOVEC LOGAR, Nataša. Spectroscopic studies of structural dynamics induced by heating and hydration : a case of calcium-terephthalate metal-organic framework. The journal of physical chemistry. C, 2013, vol. 117, issue 15, str. 7552-7564, doi: 10.1021/jp311529e. [COBISS.SI-ID 36628485]

8. RISTIĆ, Alenka, ZABUKOVEC LOGAR, Nataša, HENNINGER, Stefan K., KAUČIČ, Venčeslav. The performance of small-pore microporous aluminophosphates in low-temperature solar energy storage : the structure-property relationship. Adv. funct. mater. 2012, vol. 22, iss. 9, str. 1952-1957. [COBISS.SI-ID 4910618]

University course code: 2ZMA06

Year of study: 1

Semester: 2

Course principal:

Lecturer:

ECTS: 6

Workload:

  • Lectures: 20 hours
  • Exercises: 20 hours
  • Seminar: 5 hours
  • Field exercises: 15 hours
  • Individual work: 120 hours

Course type: mandatory

Languages: slovenian / english

Learning and teaching methods:
lectures, exercises on state of the art software for xrd data analysis under supervision of the the lecturer responsible for the course, individual qualitative and quantitative analysis of difraction data, presentation of the seminar to other students in open discussion.