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Prvoprincipiální analýza stability krystalů pevných látek
Řehák, Petr ; Buršík, Jiří (oponent) ; Šob, Mojmír (oponent) ; Černý, Miroslav (vedoucí práce)
Cílem vědeckovýzkumné činnosti v průběhu autorova doktorského studia byla analýza mechanické stability kubických krystalů při vnějším zatížení. V této práci je ukázáno, jakým způsobem byla posuzována mechanická stabilita fcc krystalů (C, Al, Ir, Pt, Au) za podmínek izotropního (hydrostatického) tahového zatížení. K tomuto účelu bylo použito ab initio metod. Studované krystaly byly podrobeny simulované izotropní tahové deformaci a byla posouzena jejich elastická stabilita. Výsledky této analýzy ukazují, že elastické porušení Al, Pt a Au souvisí s vymizením trigonálního smykového modulu, přičemž diamant a Ir zůstávají stabilní až do dosažení maxima napětí. Podle vypočtené pásové struktury si krystal diamantu zachovává svůj charakter izolantu až do tohoto porušení. Následně byla určena fononová spektra metodou lineární odezvy a bylo provedeno studium dynamické stability. Získané výsledky odhalují měkké módy u Al, Pt a Ir dříve než by došlo k jejich elastickému porušení. Vybrané krátkovlnné nestability jsou potvrzeny vytvořenými modely mikroskopické deformace i disperzními závislostmi stanovenými pomocí metody nadmříží. Vlivem nalezených nestabilit je kritická deformace příslušná maximu napětí snížena až o 40 %, přičemž kritické napětí je redukováno maximálně o 20 %.
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Quantitative Imaging in Scanning Electron Microscope
Skoupý, Radim ; Buršík, Jiří (oponent) ; Shimoni, Eyal (oponent) ; Krzyžánek, Vladislav (vedoucí práce)
This thesis deals with the possibilities of quantitative imaging in scanning (transmission) electron microscope (S|T|EM) together with its correlative applications. It starts with quantitative STEM (qSTEM) method description, where estimated local sample thickness can be related to irradiated dose and create a mass-loss study, which was applied on samples of ultrathin epoxy resin sections at variate conditions (age, temperature, staining, plasma cleaning, carbon covering, probe current). The possibilities of the detector calibration process, the necessary background of the Monte Carlo simulations of electron scattering and achievable accuracy of the method are discussed and demonstrated. The method is then extrapolated for the use of back-scattered electron (BSE) detector, where new detector calibration technique, based on primary beam deflection on electron mirror, was postulated, developed and tested on various thin coating layers with thicknesses in range from 1 to 25 nm. The use of BSE detector brings the opportunity to measure the thickness of not only the electron transparent samples as in case of qSTEM, but also thin layers on substrates – qBSE. Both above-mentioned methods (qSTEM and qBSE) are intensity-based. This brings complication in the need of proper calibration, where just a slight drift of base-signal level causes a significant change of the results. This insufficiency was overcome in case of qSTEM by using the most probable scattering angle (captured by pixelated STEM detector) instead of an integral image intensity captured by an annular segment of STEM detector. The advantage of this method is its applicability post-acquisition, where no special previous actions are needed before each imaging session. The disadvantage is the limited range of detectable thicknesses given by the peak creation in signal/scattering-angle dependency. In general, low thickness region is immeasurable as well as those too thick (usable thickness range for latex is 185 - 1,000 nm; given by detection geometry and pixel size). Moreover, multiple applications of conventional and commercially available quantitative techniques of cathodoluminescence (CL) and energy-dispersive X-ray spectroscopy (EDX) are presented in correlation with high-resolution images taken in secondary and transmitted electrons.
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NANOCERIA PREPARED BY ELECTRON BEAM EVAPORATION
Pizúrová, Naděžda ; Hlaváček, A. ; Kavčiaková, Zuzana ; Roupcová, Pavla ; Kuběna, Ivo ; Buršík, Jiří ; Sokovnin, S. Y.
Cerium oxide nanoparticles (nanoceria) are currently one of the most investigated nanomaterials because of their attractive properties used in biomedical applications, catalysis, fuel cells, and many others. These attractive properties are connected with the Ce3+ and Ce4+ valency state ratio. In the nanoparticle form, cerium oxides contain a mixture of Ce3+ and Ce4+ on the nanoparticle surfaces. Switching between these two states requires oxygen vacancies. Therefore, nanoceria's inherent ability to act as an antioxidant in an environmentally-dependent manner and a “redox switch” to confer auto-regenerating capabilities by automatically shifting between Ce4+ and Ce3+ oxidation states is significantly affected by surface morphology. Regarding this demanded behavior, we aimed to characterize synthesized nanoparticle surface quality and its influence on the cerium oxidation states. The received results were used to evaluate the synthesis method's suitability for suggested utilization. We used nanoparticles prepared by electron beam evaporation. This unique physical method includes nanoparticle creation through the fast cooling process followed by breaking radiation damaging nanoparticle surfaces to create surface off-stoichiometry. We prepared a sample containing clusters of a mixture of ultra-small nanoparticles and approximately 100 nm particles. X-ray diffraction confirmed the CeO2 phase in both components. To extract the finest component, we used centrifugal size fractionation. We received 200 nm clusters of 2-10 nm nanoparticles. Nanoparticle shapes and facet types were analyzed using transmission electron microscopy methods. We found out most nanoparticles were formed with truncated octahedrons containing {1,1,1} and {1,0,0} facet types and truncated cuboctahedrons containing {1,1,1}, {1,0,0}, and additional {1,1,0} facets. No octahedron (without truncation) containing only {1,1,1} facets was observed. Nanoparticle shapes containing {1,1,0} and {1,0,0} are suitable for redox activity. Some amount of irregular shapes, beneficial for redox activity, was also observed. Spectroscopy methods confirmed Ce3+ content.
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Thermal stability of Ti/Ni multilayer thin films
Václavík, R. ; Zábranský, L. ; Souček, P. ; Sťahel, P. ; Buršík, Jiří ; Fořt, Tomáš ; Buršíková, V.
In this work, thermal stability and mechanical properties of Ti/Ni multilayer thin films were studied. The multilayer thin films were synthesised by alternately depositing Ti and Ni layers using magnetron sputtering. The thickness of constituent layers of Ti and Ni varied from 1.7 nm to 10 nm, and one coating was deposited by simultaneous sputtering of both targets. Single crystalline silicon was used as a substrate. The effects of thermal treatment on the mechanical properties were studied using nanoindentation and discussed in relation to microstructure evaluated by X-ray diffraction. Annealing was carried out under low-pressure conditions for 2 hours in the range of 100-800 degrees C.
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Quantitative Imaging in Scanning Electron Microscope
Skoupý, Radim ; Buršík, Jiří (oponent) ; Shimoni, Eyal (oponent) ; Krzyžánek, Vladislav (vedoucí práce)
This thesis deals with the possibilities of quantitative imaging in scanning (transmission) electron microscope (S|T|EM) together with its correlative applications. It starts with quantitative STEM (qSTEM) method description, where estimated local sample thickness can be related to irradiated dose and create a mass-loss study, which was applied on samples of ultrathin epoxy resin sections at variate conditions (age, temperature, staining, plasma cleaning, carbon covering, probe current). The possibilities of the detector calibration process, the necessary background of the Monte Carlo simulations of electron scattering and achievable accuracy of the method are discussed and demonstrated. The method is then extrapolated for the use of back-scattered electron (BSE) detector, where new detector calibration technique, based on primary beam deflection on electron mirror, was postulated, developed and tested on various thin coating layers with thicknesses in range from 1 to 25 nm. The use of BSE detector brings the opportunity to measure the thickness of not only the electron transparent samples as in case of qSTEM, but also thin layers on substrates – qBSE. Both above-mentioned methods (qSTEM and qBSE) are intensity-based. This brings complication in the need of proper calibration, where just a slight drift of base-signal level causes a significant change of the results. This insufficiency was overcome in case of qSTEM by using the most probable scattering angle (captured by pixelated STEM detector) instead of an integral image intensity captured by an annular segment of STEM detector. The advantage of this method is its applicability post-acquisition, where no special previous actions are needed before each imaging session. The disadvantage is the limited range of detectable thicknesses given by the peak creation in signal/scattering-angle dependency. In general, low thickness region is immeasurable as well as those too thick (usable thickness range for latex is 185 - 1,000 nm; given by detection geometry and pixel size). Moreover, multiple applications of conventional and commercially available quantitative techniques of cathodoluminescence (CL) and energy-dispersive X-ray spectroscopy (EDX) are presented in correlation with high-resolution images taken in secondary and transmitted electrons.
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ANALYTICAL ELECTRON MICROSCOPY OF DILUTED CU-CO ALLOYS
Buršík, Jiří ; Svoboda, Milan
The work is focused on characterization of diluted model Cu-Co alloys with Co content from 2 to 4 wt.% after various thermal treatment. After initial annealing at 1273 K followed by water cooling, further annealing of the oversaturated solid solution in the range 773 to 1073 K generated a fine distribution of Co-rich precipitates. Parameters of microstructure were characterized by means of transmission electron microscopy with energy dispersive X-ray analysis.
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Study of mechanical properties of nanolayered Ti/Ni coatings
Zábranský, L. ; Václavík, R. ; Přibyl, R. ; Ženíšek, J. ; Souček, P. ; Buršík, Jiří ; Fořt, Tomáš ; Buršíková, V.
The aim of the present work was to study the dependence of mechanical properties of Ti/Ni multilayer thin films on the thicknesses of constituent Ti and Ni layers. The multilayer thin films were synthesized by deposition of Ti and Ni layers alternately on single crystalline silicon substrates using direct current magnetron sputtering method. Thicknesses of Ti and Ni layers varied from 1.7 nm to 100 nm. The micro-structure of the multilayer films was studied using X-ray diffraction technique, scanning electron microscopy with focused ion beam technique and transmission electron microscopy. Mechanical properties obtained from nanoindentation experiments were discussed in relation to microstructural observations.
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Characterization of Ta-B-C nanostructured hard coatings
Buršík, Jiří ; Buršíková, V. ; Souček, P. ; Zábranský, L. ; Vašina, P.
Microstructure and mechanical properties of Ta-B-C nanocrystalline layers prepared by magnetron sputtering were studied. DC magnetron sputtering was used to prepare thin layers on rotated substrates. Various deposition parameters were tested. Microstructure of layers was studied by means of scanning and transmission electron microscopy on thin lamellar cross sections prepared using a focussed ion beam. Both undisturbed layers and the volume under relatively large indentation prints (load of 1 N) were observed. The microstructure observations were correlated with mechanical properties characterized by means of nanoindentation experiments in both the static and the dynamic loading regime. Elastic modulus, indentation hardness and fracture resistance of prepared nanostructured coatings were evaluated and discussed.
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