Master degree in Materials Science

Advanced Diffraction Methods for Applications

Advanced Diffraction Methods for Applications

Academic year 2023/2024

Sommario del corso

• Course objectives
• Results of learning outcomes
• Program
• Course delivery
• Learning assessment methods
• Suggested readings and bibliography
• Notes
• Class schedule
• Teaching tools
• Course card

Course objectives

Course (theoretical lessons and laboratory sessions with practical activities) goals:

1. Describe the main applications of X-ray diffraction.
2. Describe the main instrumental configurations (laboratory instruments) with particular attention to the optics, related aberrations, and their effect on the experimental data.
3. Recognize the main effects of the instrumental configuration on the quality of the diffraction pattern and, consequently, propose solutions to artifacts and improvements in the experimental setup.
4. Apply the knowledge acquired to Material Science issues.

Results of learning outcomes

Knowledge and understanding:

Comprehension of the relationships between theoretical concepts of crystallography and diffraction and their experimental evidence. 

Applying knowledge and understanding:

The ability to apply the knowledge of diffraction theory to diffractometric experimental methods for the determination of lattice parameters and the identification of a crystalline phase and the ability to identify artifacts and instrumental effects are required.

A learning path is proposed, that goes from understanding to applying the concepts discussed to:

1. Diffractometric analysis techniques from powders with particular reference to the theoretical basis and their evidence in the lab.
2. Quali-quantitative analysis of a powder diffraction pattern.
3. Crystal structure refinement (Rietveld method) on synthetic and natural materials using X-ray powder diffraction as a reference technique both in R&D and quality analysis laboratories.
4. Quantitative analysis of mixtures of inorganic crystalline phases (including amorphous fraction quantification).
5. Texture analysis
6. Line broadening analysis (grain size and microstrain)

Making judgements

• Acquisition of aware judgment autonomy concerning evaluation and interpretation of experimental data, from diffractometric techniques.

Communication skills 

• Acquisition of oral and written English communication skills and expertise in the field.

Learning skills

• Acquisition of autonomous learning capacity and self-assessment of its preparation, in order to undertake subsequent studies with a high degree of autonomy.

Program

Recap of crystallography: Diffraction principles. Laue classes. Space groups. 

Diffraction from powders: Conventional sources, optics, and detectors. Parafocusing and transmission geometries. Notes on non-conventional sources.

Quali-quantitative analysis: Databases. Identification of crystalline phases in polycrystalline mixtures. Use of the free QUALX program for phase identification in crystalline mixtures. Quantitative analysis using RIR.

The Rietveld method: Quantitative, structural, and textural analysis. Use of structural refinement programs: an overview of the main structural refinement programs with particular reference to the free GSASII program. Notes on the indexing of crystalline phases.

The line broadening analysis: Scherrer grain size and microstrain analysis with particular reference to the Williamson-Hall (W-H) method.

Laboratory: Hands-on software: Identification of crystalline phases in polycrystalline mixtures. Exercises on structural and quantitative analysis: structural refinement of crystalline phases, multiphase mixtures, mixtures containing amorphous. Texture, grain size, and microstrain analysis. Indexing of diffraction patterns. Pattern deconvolution and its crystallographic meaning (Pawley vs Le Bail vs deconvolution).

Sample preparation. Acquisition of data on laboratory instruments for research and routine analysis, with particular attention to the optics configurations and their effects on the experimental data. 

Single-crystal diffraction.

Course delivery

Lectures (3CFU-24hours) and Laboratory (1CFU-16hours) in presence.

The laboratory is mandatory for at least 70% of the hours (3 lab days).

The program addressed during classes will be thoroughly revisited during the laboratory sessions.

Learning assessment methods

The oral exam will address all the topics considered during the lessons and laboratories, starting from the verification of the knowledge of basic concepts up to the discussion of more detailed topics.

Hammond - The Basics of Crystallography and Diffraction. IUCr-Oxford Science Publications

R.A. Young -; The Rietveld method. Oxford Science Publication

V.K. Pecharsky, P.Y. Zavalij - Fundamentals of powder diffraction and structural characterization of materials. Springer

Notes

The teacher is available by appointment to discuss, repeat, and clarify the concepts explained in class and the laboratory activities.

Class schedule

• Teaching material
• Exams and finals
• Class schedule
• Go to Moodle
• Register for the course
• Enrolled students
• Invia email agli studenti registrati
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