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Course: Experimental Methods of Nanomaterials

Department/Abbreviation: KEF/EMNE

Year: 2021

Guarantee: 'Mgr. Jan Filip, Ph.D.'

Annotation: The main aim is to learn basic principles and applications of advanced methods for the characterization of (nano)materials.

Course review:
1. X-Ray powdered diffraction, electron and neutron diffraction. Generation and detection of X-ray. Fundamental principles (Bragg's law), instrumentation and sample preparation for X-ray powder diffraction, measurement of nanocrystalline materials, determination of particle size through small-angle X-ray scattering (SAXS), low- and high-temperature X-ray powder diffraction, measurement of thin films. Fundamentals of electron and neutron diffraction, their comparison with X-ray diffraction. 2. Methods based on emission/absorption of electrons/X-ray emitted by photon or particles. X-ray fluorescence spectroscopy (XRF): fundamentals (Moseley's law, Rayleigh's and Compton's scattering, saturation depth, secondary fluorescence), instrumentation and sample preparation, types of XRF spectrometers, electron microanalysis. Photoelectron spectroscopy (UPS, XPS/ESCA), Auger electron spectroscopy, X-ray absorption spectroscopy (XAS - EXAFS, XANES). 3. Mössbauer spectroscopy. Mössbauer effect, experimental observation of Mössbauer effect, hyperfine interactions, interpretation of Mössbauer spectra, Mössbauer spectroscopy with registration of conversion electrons (CEMS) and conversion X-ray (CXMS), low-temperature Mössbauer spectroscopy and spectroscopy in external magnetic field. 4. Magnetometry. Magnetometer based on superconducting quantum interference device (SQUID): fundamentals, instrumentation and sample preparation, parameters of hysteresis loop, magnetic properties of substances - specific in case of nanomaterials, interparticle interactions, AC susceptibility, thermal dependence of magnetization (FC-ZFC curves). Vibration magnetometer (VSM). 5. Nuclear magnetic resonance. Nuclear magnetic moment. Magnetic moment in magnetic field: classical approach, quantum approach. Resonance and relaxation of linear sets, Bloch's equations, stationary solution, determination of relaxation times T1 a T2, nonhomogeneous broadening of absorption line, nonstationary solution. Free precession. Experimental technique. CW and pulse spectrometry. NMR spectra. Chemical shift, double resonance, decoupling and INDOR techniques, dynamical effects, NMR of other nuclei, 2D-NMR, rotation by magnetic field, CIDNP, NMR tomography. Application of NMR to study of structure of solids. Magnetic resonance imaging (MRI): fundamentals, practical applications, contrast agents (SPIO). 6. Thermal analysis. Thermo gravimetric analysis, differential thermal analysis, differential scanning calorimetric; fundamentals, instrumentation and sample preparation, measured parameters. Analysis of gases (mass spectrometry, infrared spectroscopy). 7. Measurement of specific surface area by BET method. Fundamentals, instrumentation and sample preparation, Langmuir's isotherm, measurement of porous materials, physisorption, chemisorption, thermally controlled oxidation/reduction. 8. Dynamic light scattering. Fundamentals, instrumentation and sample preparation for particle size measurement, evaluation methods. Stokes' law. Zeta potential and its pH dependency, electrokinetical effects, isoelectric point, electric bilayer. 9. Vibration spectroscopy. Introduction, basic vibration. Instrumentation for IR spectroscopy. IR spectra. Raman spectroscopy - introduction and application to biomacromolecules. Resonant Raman's spectroscopy. UV-VIS absorption a luminescent spectroscopy. Surface enhanced Raman scattering (SARS). 10. Vacuum techniques. Vacuum preparation, types of pumps. Measurement of low pressures. Construction of vacuum apparatus. Ultrahigh vacuum systems.