653-0937/03 – Modern Techniques of Structure and Phase Analysis (MMSFA)
| Gurantor department | Department of Materials Engineering and Recycling | Credits | 10 |
| Subject guarantor | prof. Ing. Vlastimil Vodárek, CSc. | Subject version guarantor | prof. Ing. Vlastimil Vodárek, CSc. |
| Study level | postgraduate | Requirement | Choice-compulsory type B |
| Year | | Semester | winter + summer |
| | Study language | Czech |
| Year of introduction | 2022/2023 | Year of cancellation | |
| Intended for the faculties | FMT | Intended for study types | Doctoral |
Subject aims expressed by acquired skills and competences
PhD students will learn about principles of the most important techniques of structure, diffraction and spectral analyses, with possibilities and limitations of individual techniques of structure characterisation, with fundamentals of interpretation of structure analysis results. They will be able to define appropriate techniques of structure characterization needed to solve a problem and to prepare specimens for basic experimental techniques.
Teaching methods
Lectures
Individual consultations
Experimental work in labs
Summary
The aim of the course is to deepen the knowledge of PhD students in the field of structure and phase analyses of engineering materials. Lectures are mainly focused on qualitative and quantitative structure characterisation by using light microscopy, techniques based on the focused electron beam (electron microscopy) and X - ray diffraction. The attention is paid to applications of structure parameters in analysis structure - property relationships in engineering materials. Possibilities and limitations of individual experimental techniques are demonstrated on case studies.
Compulsory literature:
Recommended literature:
Way of continuous check of knowledge in the course of semester
Oral exam with the written preparation.
E-learning
Other requirements
There are no further special requirements.
Prerequisities
Subject has no prerequisities.
Co-requisities
Subject has no co-requisities.
Subject syllabus:
- Structural hierarchy. Reasons of structure characterization at a wide range of length scales (macrostructure, microstructure, nanostructure). Definition of the basic parameter for a comparison of different microscopic techniques: spatial resolution.
- Principle of the stereomicroscope. Development trends in light microscopes: direct, inverted (Le Chatellier), digital (without eyepiece). Confocal laser scanning microscopes. Spatial resolution and depth of focus. Preparation of specimens. Typical tasks of microstructure characterization by using light microscopy. Quantitative metallography, automated image analysis. Basics of stereology.
- Interaction of X-ray and electrons with a specimen: products of elastic and inelastic scattering. Application of the concept of reciprocal lattice for diffraction analysis. Geometric conditions of diffraction: Bragg´s law and Ewald´s reflection sphere. Structure factor.
- Application of X rays for structural and phase analysis of materials. X-ray diffraction analysis (XRD) of polycrystalline materials: instrumentation, qualitative and quantitative phase analyses. Study of residual stresses using X rays. Evaluation of residual stresses of the 1st (macro-stress) and 2nd (coherent size or defect density) order. Evaluation of preferred orientation of grains (texture). X ray diffraction analysis of single crystals. X- ray fluorescence (XRF) analysis of elemental composition.
- Instruments based on the focused electron beam. Principles of transmission and scanning electron microscopes. Analytical electron microscopy. Scanning electron microscopy at a low vacuum level (LVSEM, ESEM). Spatial resolution. Vacuum system, electron sources, electromagnetic lenses and their imaging defects, signal detectors.
- Contrast mechanisms in transmission electron microscopy (TEM): amplitude and phase contrasts. Bright field and dark field images. Basic principles of kinematic and dynamic theory of electron scattering, contrast on crystallographic defects. Preparation of specimens (extraction replicas and thin foils) for transmission electron microscopy.
- High resolution transmission electron microscopy (HRTEM). Dynamic theory of diffraction: two-beam approximation, multibeam approximation, method of multilayers. Lattice imaging. Structure imaging. Computer simulation of image contrast. Z-contrast method.
- Focused ion beam (FIB) microscopy. Interaction of ions with solid specimens. Ion sources. Injection of gas precursor. Manipulator. Double beam microscopes FIB/SEM. Basic applications of FIB/SEM. Negative phenomena associated with FIB technique. Tomography: 3D EBSD or EDX mapping.
- Electron diffraction techniques: selected area diffraction and convergent beam diffraction. Interpretation of diffraction patterns from single crystals and polycrystalline materials. Comparison of diffraction methods of electrons, X-rays and neutrons. Electron energy loss spectroscopy (EELS). Energy filtered transmission electron microscopy (EFTEM).
- Contrast mechanisms in scanning electron microscopy (SEM). Interaction volume. Detectors of secondary and back scattered electrons. Interpretation of images in secondary electrons and in backscattered electrons. X ray microanalysis: wave (WDX) and energy dispersive (EDX) analyses, possibilities and limitations, artefacts. Spectroscopy of Auger electrons.
- Electron back scattered diffraction (EBSD) in scanning electron microscope. Mechanisms of diffraction patterns formation. Indexing of diffraction patterns, their information content. Basic applications: phase identification and mapping of crystallographic orientation of grains. Presentation of results: pole figures (PF), orientation distribution function (ODF), IPF orientation maps, orientation and disorientation of grains, phase maps (PM). Preparation of specimens.
- Microscopy of surfaces using scanning probe techniques (SPM) – atom force microscopy (AFM), scanning tunneling microscopy (STM) magnetic force microscopy (MFM). Field ion microscopy. Atom probe (AP) tomography. Spatial resolution of individual techniques. Principle of correlative microscopy.
- Examples of structure characterization in the field of materials science and engineering.
Conditions for subject completion
Occurrence in study plans
Occurrence in special blocks
Assessment of instruction