617-3014/01 – Textural and structural analysis (TSA)
| Gurantor department | Department of Chemistry | Credits | 5 |
| Subject guarantor | doc. Ing. Vlastimil Matějka, Ph.D. | Subject version guarantor | doc. Ing. Vlastimil Matějka, Ph.D. |
| Study level | undergraduate or graduate | Requirement | Compulsory |
| Year | 1 | Semester | summer |
| | Study language | Czech |
| Year of introduction | 2019/2020 | Year of cancellation | |
| Intended for the faculties | FMT | Intended for study types | Follow-up Master |
Subject aims expressed by acquired skills and competences
The aim of the lectures and laboratory practice is to introduce the issues related to the structure and texture of the materials and methods of the structure and texture analysis.
Teaching methods
Lectures
Tutorials
Experimental work in labs
Other activities
Summary
The subject is focused on explanation of theoretical as well as practical issues related to structural and textural analyses of materials.
Compulsory literature:
Recommended literature:
Way of continuous check of knowledge in the course of semester
Oral exam.
E-learning
Other requirements
There are not additional requirements.
Prerequisities
Subject has no prerequisities.
Co-requisities
Subject has no co-requisities.
Subject syllabus:
1. Introduction – texture and structure of the materials. Why to study the texture and structure? Amorphous, mesomorphous and crystal materials. Crystal materials and their structure – macroscopic symmetry of the crystals, point groups and crystallographic systems. Classification of the structures based on the character of the bonds.
2. Basics of the diffraction theory. RTG irradiation and the sources of X-ray. Interaction of X-ray with a matter. Dispersion of X-rays, diffraction of X-rays on crystal grid, effect of the atoms distribution on diffraction pattern. Principle of the methods of the structural analysis.
3. Overview of the X-ray diffraction techniques, monocrystal methods, studies of the powder and polycrystalline materials. Concept of the X-ray diffractometers, modifications of the diffractometers set-up.
4. X-ray diffraction pattern, measurement of the diffraction lines positions, qualitative evaluation of the diffraction patterns. Intensity of the diffraction patterns, integral intensity of the diffraction patterns, fitting of the diffraction peaks.
5. Application of the diffraction methods. Qualitative and quantitative diffraction analysis, determination of the lattice parameters of the polycrystalline materials, calculation of crystallite size, measurement of microscopic tension. X-ray diffraction methods for texture evaluation. X-ray diffraction method at high temperatures and pressures.
6. Neutron diffraction analysis – sources of the neutrons, monochromatization. Diffraction experiment, examples of the utilization of neutron diffraction analysis. Defects of the crystalline structure and the methods of their studies. X-ray tomography, principle of the methods, practical utilization.
7. Scanning electron microscopy, interaction of the sample with electrons, sources of the electrons, utilization of secondary and back scattered electrons for the images creation, construction of scanning electron microscopes. Energy and wave dispersive microanalysis, preparation of the samples for SEM.
8. Transmission electron microscopy. Origination of the image in TEM, scattering and diffraction contrast, samples observation in bright and dark field, construction of microscopes, preparation of the samples for TEM. Diffraction analysis in TEM.
9. Texture of the surfaces. Parameters for evaluation of the surface roughness. Surface profiling techniques – stylus, confocal microscopy, holographic microscopy.
10. Scanning probe microscopy techniques. Scanning tunneling microscopy and atomic force microscopy. Principle of the methods, construction of the microscopes, probes, positioning parts, detection. Topography measurement with AFM.
11. Derived AFM techniques. Lateral force microscopy, magnetic force microscopy, Kelvin probe force microscopy, force modulation microscopy, electric force microscopy, AFM spectroscopy. Basiscs of the image analysis.
12. Textural analysis of powdered materials. Physical sorption of gases, desorption, chemisorption. Types of adsorption isotherms, BET isotherm, capillary condensation, distribution of micro and mezo pores. Mercury porosimetry, principle, construction of the porosimeters, data evaluation. Dynamic vapor sorption, principle of the measurement, device construction, data evaluation.
Laboratory practice:
1. Introduction, seminary work.
2. Excursion in the laboratory of X-ray diffraction. Determination of lattice parameters of crystalline material.
3. Excursion in the laboratory of X-ray diffraction. Determination of the crystallite size, effect of the amorphous character on the X-ray diffraction pattern.
4. Excursion in the laboratory of X-ray diffraction. Effect of the texture of drawn wire on the shape of X-ray diffraction pattern.
5. Excursion in the laboratory of scanning electron microscopy. Observation of the surface of the polished and acid attacked sample of the metal alloy.
6. Image analysis using software Gwyddion.
7. Excursion in the laboratory of confocal microscopy. Determination of the roughness parameters of the surface of metal sample polished with different sand papers.
8. Excursion to the laboratory of atomic force microscopy. Observation of the periodically repeated motives on the surface of the samples.
9. Excursion to the laboratory of atomic force microscopy. Study of the electric conductivity of the composites using spreading resistance microscopy.
10. Excursion to the laboratory of textural parameters. Measurement of specific surface area and pores of the powder samples.
11. Excursion to the laboratory of textural parameters. Measurement of pore distribution using mercury porosimetry.
12. Excursion to the laboratory of textural parameters. Measurement of sorption of water vapor using dynamic vapor sorption instrument.
13. Excursion to the laboratory of tomography. Study of macroscopic defects.
14. Presentation of the tasks solution defined within seminary works. Credits.
Conditions for subject completion
Occurrence in study plans
Occurrence in special blocks
Assessment of instruction