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Wednesday 29th August


Opening Lecture: Powder Diffraction: State of the Art and Perspectives
Lecturer: Gilberto Artioli (University of Padova, Italy)

Current powder diffraction instruments, methods and acquired protocols will be briefly reviewed. Their role as standardized tools for the investigation of solid matter will be discussed, with a view on recent instrumental and methodological developments. It is argued that (1) presently powder diffraction is often used well below its potential for providing key information on materials, (2) the combination or the simultaneous use of powder diffraction with spectroscopic and/or imaging techniques are assuming an increasingly important experimental role in the investigation of matter. Examples will be discussed, drawn from different fields of research such as cultural heritage materials, industrial applications, and advanced characterization techniques.



Fundamental Aspects of Powder Diffraction I
Lecturer: Ernesto Mesto (University of Bari, Italy)

X-ray powder diffraction (XRPD) is a powerful non-destructive technique for characterizing crystalline materials. It provides qualitative and quantitative phases analysis, and information on crystal structure, texture, grain size, crystallinity, strain, and crystal defects. The students will be introduced to the basic theoretical aspects (interaction of X-rays with crystalline solids, principles of diffraction, scattering of periodic arrays, etc.) and to the experimental details of the powder X-ray diffraction (Debye-Scherrer and Bragg-Brentano geometry). The aim is to provide a basic knowledge of diffraction methods for the polycrystalline materials analysis.



Fundamental Aspects of Powder Diffraction II: Preliminary data treatment
Lecturer: Gennaro Ventruti (University of Bari, Italy)

Powder diffraction data consist of a raw file of scattered intensity as a function of scan angle. This raw diffraction file contains abundant information for various applications. To accurately interpret and analyse patterns some data treatment processes are required. For example, when applications involve the identification of phases in a specimen it is necessary to extract a reduced pattern which lists integrated intensities and positions of distinguishable reflections to be used in searching and matching routine. The obtained reduced pattern may be also used in indexing, lattice parameters refinement and ab initio structure solution. This lecture aims to drive the user through the different steps employed in the treatment of raw powder diffraction data (background subtraction, data smoothing, Kα2 stripping, peak searching, data extraction) and obtain preliminary information.



Modern Powder Diffraction Instruments
Lecturer: Andy Fitch (ESRF, Grenoble, France)

Powder diffraction measurements can be carried out using a laboratory X-ray source, or at a central facility exploiting synchrotron radiation or neutrons. Whereas laboratory sources are the most accessible, and are the basis for most powder diffraction measurements made in the academic, industrial and analytical domains, synchrotron radiation and neutrons allow the design of specialised instruments, with very high d-spacing resolution, high time resolution, and allowing measurements using hard X-ray energies. The talk will give an overview of the current possibilities.



Qualitative analysis: the PDF 4+ database
Lecturer: Matteo Leoni (University of Trento, Italy)

Working with real data: let's avoid to reinvent the wheel! Why you need a database? What can you find in PDF4+? What's the idea behind a search match.



Tutorial Session: QUALX2.0
Lecturer: Aurelia Falcicchio (Institute of Crystallography-CNR, Italy)

QUALX2.0 is a computing program freely distributed for qualitative phase analysis by X-ray powder diffraction data. The software is based on the traditional search–match method, it is able to manage the commercial database PDF-2 maintained by ICDD, and a freely available database POW_COD generated by the structure information contained in the Crystallography Open Database. QUALX2.0 demonstration will be devoted to present examples of applications by using standard and non-standard computational and graphic options of the program.



Thursday 30th August


Powder Diffraction for Solving Crystal Structures
Lecturer: Elena Kabova (University of Reading, UK)

Powder X-ray diffraction (PXRD) is widely used in industry for solid form screening but can we routinely and confidently employ it for crystal structure solution? This talk aims to answer the above question by giving a broad overview of the last 20 years of successfully employing powder X-ray diffraction as a crystal structure determination tool. In particular, I will aim to cover the wide range of strategies used to overcome the limitations of PXRD data and highlight the challenges in solving increasingly complex molecular crystal structures from PXRD alone.



Indexing and Space Group Determination
Lecturer: Anna Moliterni (Institute of Crystallography-CNR, Italy)

The correct determination of the unit cell parameters and the space group is a fundamental task for the success of the structure solution process. Both indexing and space group identification are usually trivial in case of single crystal data; in case of powder diffraction data, they can be challenging steps due to typical and often concomitant problems (i.e., overlap of reflections, wrong background description, preferred orientation effects, ...).
The main approaches aimed at finding unit cell parameters and space group will be described, with particular attention to the methods implemented in the EXPO program. Some examples of applications of EXPO to experimental data will be given.



Structure Solution in Reciprocal Space
Lecturer: Rosanna Rizzi (Institute of Crystallography-CNR, Italy)

The reciprocal space (RS) methods for crystal structure solution from powder diffraction data work in the reciprocal space applying the following scheme: first, the structure factor moduli |Fh| of each h reflection are extracted from the experimental diffraction pattern; then the phases phih of structure factors Fh=|Fh|exp(iphih) are estimated; finally the electron density map is calculated by inverse Fourier transform of the structure factors, determined in moduli and phases. The RS methods have numerous advantages: they are fast, reliable, easy to use and able to solve any type of compound. This is particularly true for single crystal data. In case of powders, the solution process via RS methods is not straightforward because the inaccuracy on integrated intensities estimates principally due to the unavoidable diffraction peaks overlap. Different strategies have been adopted to improve the extraction process but the errors on the calculated structure factor moduli remain. Consequently, the phasing process by RS methods may be not always successful. The theoretical background and the practical tools for solving powder structures by RS methods will be given.



Structure Solution in Direct Space
Lecturer: Radovan Černý (Université de Genčve, Switzerland)

When no reliable integrated intensities can be extracted from a powder pattern, then the only choice of structure solution is modelling the pattern as a whole, i.e. searching for a correct structural model in direct space. Such situation is typical for real conditions of crystallization as found in many applied materials, in-situ studies of reactions, phase transitions. Any additional information about the atomic coordination and connectivity creating bigger building units and leading so to lower number of structural parameters to be determined is easily used.
The basic ideas, historical development and available software of crystal structure solution from powder diffraction data in direct space (aka global optimization method or pattern modelling) will be discussed. The highlights and pitfalls of direct space method with examples will be shown.



Tutorial Session: EXPO
Lecturer: Corrado Cuocci (Institute of Crystallography-CNR, Italy)

This tutorial session focuses on the main stages of the crystal structure determination from powder diffraction data by using the computer program EXPO2014: indexing and space group determination, crystal structure solution by reciprocal and direct space methods, Rietveld refinement. Selected representative practical examples will be shown and the students will be encouraged to work alone on topics discussed in the lectures and on examples provided by teachers or on their own data.



Tutorial Session: FOX
Lecturer: Radovan Černý (Université de Genčve, Switzerland)

When no reliable integrated intensities can be extracted from a powder pattern, then the only choice of structure solution is modelling the pattern as a whole, i.e. searching for a correct structural model in direct space. Such situation is typical for real conditions of crystallization as found in many applied materials, in-situ studies of reactions, phase transitions. Any additional information about the atomic coordination and connectivity creating bigger building units and leading so to lower number of structural parameters to be determined is easily used.
The basic ideas, historical development and available software of crystal structure solution from powder diffraction data in direct space (aka global optimization method or pattern modelling) will be discussed. The highlights and pitfalls of direct space method with examples will be shown.



Tutorial Session: DASH
Lecturer: Elena Kabova (University of Reading, UK)

Powder X-ray diffraction (PXRD) is widely used in industry for solid form screening but can we routinely and confidently employ it for crystal structure solution? This talk aims to answer the above question by giving a broad overview of the last 20 years of successfully employing powder X-ray diffraction as a crystal structure determination tool. In particular, I will aim to cover the wide range of strategies used to overcome the limitations of PXRD data and highlight the challenges in solving increasingly complex molecular crystal structures from PXRD alone.



Friday 31st August


The Rietveld method for refining crystal and magnetic structures
Lecturer: Juan Rodriguez-Carvajal (Institut Laue-Langevin, Grenoble, France)

In this talk the fundamental principles of the Rietveld method and recent extensions to treat complex powder diffraction patterns will be presented. Topics that will be treated in the talk, illustrated with relatively simple cases, include: i) The use of X-ray and/or neutron diffraction, advantages and drawbacks of each technique, ii) Simplified microstructural analysis (double Voigt approach), iii) Crystal and magnetic structure determination and refinement, iv) The usefulness of multi-pattern refinements (including single crystals) and v) Symmetry modes approach using refinable amplitudes of irreducible representations of the high symmetry space group with the help of program like ISODISTORT or AMPLIMODES.



Quantitative Analysis
Lecturer: Giuseppe Cruciani (University of Ferrara, Italy)

Abstract will be provided soon



Tutorial Session: FULLPROF
Lecturer: Juan Rodriguez-Carvajal (Institut Laue-Langevin, Grenoble, France)

In this talk the fundamental principles of the Rietveld method and recent extensions to treat complex powder diffraction patterns will be presented. Topics that will be treated in the talk, illustrated with relatively simple cases, include: i) The use of X-ray and/or neutron diffraction, advantages and drawbacks of each technique, ii) Simplified microstructural analysis (double Voigt approach), iii) Crystal and magnetic structure determination and refinement, iv) The usefulness of multi-pattern refinements (including single crystals) and v) Symmetry modes approach using refinable amplitudes of irreducible representations of the high symmetry space group with the help of program like ISODISTORT or AMPLIMODES.



Tutorial Session: OCHEMDB
Lecturer: Nicola Corriero (Institute of Crystallography-CNR, Italy)

The Open Chemistry Database (OChemDb) is a free on-line portal which, using an appropriately designed database of already solved crystal structures, has been very recently developed for searching and analysing crystal-chemical information of organic, metal-organic and inorganic structures, and providing statistics on desired bond distances, bond angles, torsion angles, space groups, and atom types. It can result of great utility for structural chemistry, in particular in the process of determination of a new crystal structure (also by powder diffraction data), and for any discipline involving crystalline structure knowledge. The easy use of OChemDb will be shown by representative examples of application.



Tutorial Session:GSAS
Lecturer: Giuseppe Cruciani (University of Ferrara, Italy)

Abstract will be provided soon



Saturday 1st September


Modelling Interstratified and Defective Structures
Lecturer: Bruno Lanson (ISTerre, Université Grenoble Alpes, Grenoble, France)

The nature, content, and possibly distribution of structure defects controls to a large extent mineral/ material reactivity and properties. More especially, the high density of structure defects of layered minerals and materials is key to their reactivity. These defects range from local defects such as isomorphous substitutions, layer vacancies, or atomic displacements, to random or well defined stacking faults induced by non-periodic layer rotations, translations or twinning, and to mixed layering resulting from the coexistence within a given crystal of layers having different structure, thickness, or interlayer displacement. The occurrence of stacking faults in lamellar structures is favoured by the energetic similarity of the different stacking modes, owing to the weak interactions between adjacent layers. To determine, control, or predict mineral / material reactivity a detailed structural characterization of layered structures, including structure defects, is thus essential, and X-ray diffraction (XRD) has been the preferred method of investigation for this purpose. However, as a result of their non-periodicity or their reduced periodicity, the diffraction maxima recorded from these compounds do not strictly obey Bragg’s law, thus hampering the use of conventional diffraction approaches, such as the Rietveld method. Profiles and intensities of diffraction maxima are affected by the nature, content, and distribution of structure defects, however, thus allowing the determination of these parameters with diffraction techniques. The present talk will report on approaches allowing reliable interpretation of diffraction data, and thus determination of average structural information, from crystals deprived of 3D periodicity. Applications to various layered structures will be reported.



Line profile analysis
Lecturer. Matteo Leoni (University of Trento, Italy)

Ideal and real diffraction patterns. Traditional size analysis using Scherrer equation. Adding microstrain: Williamson-Hall plot. Fourier methods: Warren-Averbach analysis. Full pattern methods: Whole Powder Pattern Modelling (WPPM). Extending the WPPM beyond 3D periodicity



Tutorial Session: DEFECTS MATTER
Lecturer: Bruno Lanson (ISTerre, Université Grenoble Alpes, Grenoble, France)

The nature, content, and possibly distribution of structure defects controls to a large extent mineral/ material reactivity and properties. More especially, the high density of structure defects of layered minerals and materials is key to their reactivity. These defects range from local defects such as isomorphous substitutions, layer vacancies, or atomic displacements, to random or well defined stacking faults induced by non-periodic layer rotations, translations or twinning, and to mixed layering resulting from the coexistence within a given crystal of layers having different structure, thickness, or interlayer displacement. The occurrence of stacking faults in lamellar structures is favoured by the energetic similarity of the different stacking modes, owing to the weak interactions between adjacent layers. To determine, control, or predict mineral / material reactivity a detailed structural characterization of layered structures, including structure defects, is thus essential, and X-ray diffraction (XRD) has been the preferred method of investigation for this purpose. However, as a result of their non-periodicity or their reduced periodicity, the diffraction maxima recorded from these compounds do not strictly obey Bragg’s law, thus hampering the use of conventional diffraction approaches, such as the Rietveld method. Profiles and intensities of diffraction maxima are affected by the nature, content, and distribution of structure defects, however, thus allowing the determination of these parameters with diffraction techniques. The present talk will report on approaches allowing reliable interpretation of diffraction data, and thus determination of average structural information, from crystals deprived of 3D periodicity. Applications to various layered structures will be reported.



Tutorial Session: PM2K
Lecturer: Matteo Leoni (University of Trento, Italy)

Hands-in session on the analysis on nanocrystalline materials using the WPPM method: bring your own data!



Sunday 2nd September


Powder Diffraction in Industry
Lecturer: Giuseppe Cruciani (University of Ferrara, Italy)

Abstract will be provided soon



Powder Diffraction and Patents
Lecturer: Paolo P. Mazzeo (University of Parma, Italy)

Two of the requirements for a patent are novelty and non-obviousness. By definition a new crystal form is novel and, since crystal forms cannot be predicted a priori, they are also not obvious. Hence, many new crystal forms are patentable and have been patented, especially in the pharmaceutical field. Since about 60% of the new molecular entities approved by the FDA in the last 25 years claims to have polymorphs, we have also consequently assisted to an authentic explosion of patent litigations filed between pharma companies for a turnover of about 60 bln $. Market protection plays therefore a major role in the growth of the pharmaceutical industry and X-ray powder diffraction represents the ultimate tool to unequivocally characterize the solid state of a drug products. By way of example, a couple of important case studies will be described.



Powder Diffraction for Difficult Organic Materials
Lecturer: Dubravka Šišak Jung (DECTRIS LTd, Baden-Daettwil, Switzerland))

In comparison to inorganic materials, structure determination of organic compounds may challenging due to their relatively low scattering capability, radiation sensitivity and limited crystallinity. Although both reciprocal and direct space methods are almost routinely used to determine crystal structures of a variety of organic structures, there are cases where both reach their limits. The success of the reciprocal methods depends on how the overlap method is treated, while the direct-space methods are limited by the correctness of the chemical model. This talk presents a series of organic molecules whose structures could be solved only by using a specific data collection and structure determination approaches. The data collection approach is based on a very short data acquisition time, while the structure determination approach relies on the combination of two complementary methods.



Non-Ambient Powder Diffraction
Lecturer: Željko Skoko (University of Zagreb, Croatia)

Non-ambient powder diffraction implies diffraction experiments that require special conditions – high/low temperature, high/low pressure, reactive environment, electrical potential or solutions. These special “outside” conditions have strong effect on the synthesis processes, stability of compounds, stress and texture properties, microstructure and they cause phase transitions and structural distortion. In non-ambient experiments, data is collected as a function of controlled variables, such as temperature, pressure and time. Main advantage of non-ambient diffraction experiments lies in the controlled “outside” conditions which usually cannot be obtained ex-situ. X-ray diffraction proves to be an indispensable technique to fathom the influence of non-ambient conditions on materials’ properties. Results of non-ambient conditions on material will be demonstrated in the case of the alluring thermosalient (“jumping”) crystals.



Powder Diffraction for Materials Science
Lecturer: Jasminka Popović (Rudjer Bošković Institute, Zagreb, Croatia)

Governments and industries invest billions of euros every year into the research and development of advanced materials – from solid state electrolytes to solar cells, from microelectronics to advanced optical devices. X-ray powder diffraction (XRPD) has the pivotal role in all of those research topics since it allows identification and quantification of phases, determination of the degree of crystallinity, determination of crystal structure of novel materials, crystal orientation and texture, residual stress analysis and many more. This talk will illustrate the importance of structural analysis in material science on several different research topics: from novel pathways for the preparation of nanomaterials to utilization of mixed-metal oxides for li-ion batteries.




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