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Correlation of electron backscatter diffraction for elastic stress mapping
Ondračka, Václav ; Kuběna, Ivo (referee) ; Spousta, Jiří (advisor)
Electron backscatter diffraction is a method that is well described and commonly used for orientation image mapping, including grain size estimation. The use of this method for measuring elastic deformation and rotations caused by plastic deformations is not so well decribed. This diploma thesis first describes the typical EBSD system. The information regarding the standard coordinate systems, grain orientation notation and system calibration is then used to create an open-source software for mapping elastic deformations and rotations inside a single grain or a monocrystal. This software uses data acquired during standard EBSD mapping on a commercial system.
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Fracture toughness testing at high temperature range using miniaturized CT specimens
Holas, Jiří ; Kuběna, Ivo (referee) ; Šiška, Filip (advisor)
This master´s thesis deals with the evaluation of fracture behavior of ODS steel MA956 at high temperature range. This behavior was tested by using miniaturized CT specimens, on which were performed experiments to measure of ductile crack growth resistance curves (J-R curves). The value of the fracture toughness was determined from these J-R curves. Fracture properties were consequently evaluated by using fractographic analysis of the fracture surfaces. Structural properties of material was identified by hardness measurement and analyzed by metallographic methods. Results of the measurements show drop of the fracture toughness with respect to the increasing temperature.
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New compositions of advanced oxide dispersion steels based on rare earth elements
Pech, Filip ; Kuběna, Ivo (referee) ; Hadraba, Hynek (advisor)
The main objective of present diploma thesis is to prepare three different classes of steels, differing by their content of chromium: 9Cr, 14Cr, 17Cr steels and their oxide dispersion strengthened variants. Steels were prepared from atomic and pre-alloyed powders by the mechanical alloying and compacted by the spark plasma sintering method. Used strengthening elements were yttrium, which is most commonly used, and aluminium. Preparation of oxide dispersion was done in two ways: direct adding of yttria and alumina and inner oxidation of aluminium and yttrium. In the experimental part has been found, that it is possible to make oxide dispersion by both ways, but aluminium strengthened steel has to be prepared by inner oxidation to ensure fine oxide dispersion.
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Development of Nanofabrication Methodology for Study of Mechanical Properties of Thin Films using Focused Ion Beams
Kuběna, Ivo ; Švejcar, Jiří (referee) ; Kruml, Tomáš (advisor)
The main goal of this work is to find a methodology of the fabrication of microcompressive specimens (pillars) from thin metallic film prepared by means of PVD. The studied film was prepared by the ON Semiconductor company, Roznov pod Radhostem. Its chemical composition was Al-1.5 wt.% Cu; such films are used for electric connections on integrated circuits. At first, a thin intermediate layer of W-10 wt.% Ti was deposited on the Si single crystalline substrate with the purpose of improving adhesion properties of the studied film. The geometry of the microcompressive specimen should be as close to the cylindrical shape as possible. The height of the cylinder is given by the film thickness, its diameter is approximately 1 m. Such specimens were prepared in Quanta 3D FEG Dual BeamTM facility using focused ion beams technology. Experiments were done at FEI Company in Brno. In total, 39 microcompressive specimens were prepared at various ion milling conditions. The required geometry was finally attained by the optimization of processing parameters, in particular the parallelism of lateral faces was improved, the bottom of the removed zone in the vicinity of the pillar was almost flat and the transition pillar – flat bottom was regular. The prepared pillars are suitable for the microcompression tests; the first of them have been already performed within the cooperation with the Institut of Physics, Academy of Sciences of the Czech Republic, Praha.
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Early Stages of Fatigue Damage of Steels for Fusion Energetics
Kuběna, Ivo ; Spätig, Philippe (referee) ; Lukáš, Petr (referee) ; Kruml, Tomáš (advisor)
Hlavním cílem této práce bylo vysvětlit únavové chování ocelí ODS Eurofer, 14Cr ODS feritické oceli vyráběné v CEA (Commissariat a l’énergie atomique, Saclay, France) a 14Cr ODS feritické oceli vyráběné v EPFL (École Polytechnique Fédérale de Laussane, Switzerland). Pokud to bylo možné byly získané výsledky porovnány s ocelí Eurofer 97. Tato práce je součástí široké spolupráce, která je zaměřena na vývoj konstrukčních materiálů pro fuzní reaktory. V průběhu práce byly provedeny následující experimenty: • Standardní únavové zkoušky za pokojové teploty, při 650 a při 750 , byly získány křivky cyklického zpevnění/změkčení, cyklické deformační křivky, Coffinovy–Mansonovy a Wöhlerovi křivky. Hysterezní smyčky byly detailně analyzovány. • Pozorování mikrostruktury výchozího stavu pomocí TEM a porovnání s mikrostrukturou po cyklickém zatížení. • Pozorování povrchového reliéfu, který vznik díky lokalizaci cyklické plastické deformace - byla odhalena místa iniciace únavových trhlin a byl analyzován mechanismus jejich vzniku. • Měření kinetiky únavových trhlin. Oxidická disperse značně zpevňuje materiály, redukuje cyklické změkčení a stabilizuje mikrostrukturu v celém rozsahu teplot. Byly nalezeny velké rozdíly v životnosti jednotlivých ocelí. Ty byly vysvětleny pomocí rozdílných mechanismů iniciace trhlin a jejich různou rychlostí.
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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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Correlation of electron backscatter diffraction for elastic stress mapping
Ondračka, Václav ; Kuběna, Ivo (referee) ; Spousta, Jiří (advisor)
Electron backscatter diffraction is a method that is well described and commonly used for orientation image mapping, including grain size estimation. The use of this method for measuring elastic deformation and rotations caused by plastic deformations is not so well decribed. This diploma thesis first describes the typical EBSD system. The information regarding the standard coordinate systems, grain orientation notation and system calibration is then used to create an open-source software for mapping elastic deformations and rotations inside a single grain or a monocrystal. This software uses data acquired during standard EBSD mapping on a commercial system.
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LCF behaviour of 301LN steel: coarse-grained vs. UFG-bimodal structure
Man, Jiří ; Chlupová, Alice ; Kuběna, Ivo ; Kruml, Tomáš ; Man, O. ; Järvenpää, A. ; Karjalainen, L. P. ; Polák, Jaroslav
Low-cycle fatigue (LCF) behaviour of metastable austenitic 301LN steel with different grain sizes – coarse-grained (14 µm) and UFG (1.4 µm) with a grain bimodality – produced by reversion annealing (RA) was investigated. Symmetrical push-pull LCF tests were conducted on flat sheet specimens at room temperature with constant strain rate of 2×10–3 s–1 and constant total strain amplitude ranging from 0.4% to 0.8%. After completion of fatigue tests a ferritescope was adopted for quantitative assessment of volume fraction of deformation induced martensite (DIM). Microstructural changes, distribution and morphology of DIM in the volume of material were characterized at different scales by colour etching, TEM and EBSD techniques. Experimental data on microstructural changes are confronted with the stress-strain response and with the chemical heterogeneity present in the material.
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MICROSTRUCTURE EVOLUTION DURING FATIGUE LOADING OF BULK NANOSTRUCTURED ALLOY AL(93)FE(3)CR(2)TI(2)
Chlupová, Alice ; Chlup, Zdeněk ; Kuběna, Ivo
The results of observation of the microstructure evolution during fatigue loading of the bulk nanostructured quasicrystalline Al alloy are presented. Feedstock powder with nominal composition of Al93Fe3Cr2Ti1 produced by gas atomization was hot extruded for powder compaction. The enhanced strengthening of the quasicrystalline nanostructured Al alloy is attributed to the microstructure refinement, formation of supersaturated solid solution, presence of reinforcing icosahedral quasicrystalline phase and work hardening caused by the deformation during extrusion. Good thermal stability is supported by presence of spherical quasicrystalline particles with different interior structure and sizes of up to 250 nm in the diameter. Low cycle fatigue stress-strain characteristics and microstructural evolution of the material were studied. For the microstructure observation the samples of material before and after fatigue loading the TEM and SEM microscopy was employed. The microstructure evolution caused by cyclic loading with positive mean stress was evaluated.
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