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The influence of mechanical alloying on contamination of powder mixtures and bulk materials
Kubíček, Antonín ; Hadraba, Hynek (referee) ; Moravčík, Igor (advisor)
This thesis deals with the influence of process parameters on the contamination level of powder materials produced by mechanical alloying (MA) technology. For this purpose austenitic stainless steel 316 L and equiatomic CoCrFeNi high-entropy alloy (HEA) were prepared by high-energy ball milling. Both materials were milled in argon and nitrogen atmospheres from 5 to 30 hours. Spark plasma sintering method (SPS) was then used for consolidation of chosen powder samples. Chemical analysis of contamination within MA was carried out using combustion analysers for determination of carbon, oxygen, and nitrogen contents after different lengths of milling. Also differences in chemical composition of powder and corresponding bulk samples were measured. The microstructure analysis using scanning electron microscopy (SEM) of both powder and bulk materials was executed with focus on oxide and carbide presence and dispersion. Increasing content of carbon with increasing milling time was observed across all measured samples. This contamination is attributed to using milling vial made of tool steel AISI D2 (containing 1,55 wt. % of carbon). Increase of carbon content within consolidation using SPS was also observed. Milling of specimens using N2 as milling atmosphere caused higher contamination level in both AISI 316 L and HEA compared to milling in argon.
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An investigation of novel electroceramic structures for new sensor applications
Nan, Bo ; Liedermann, Karel (referee) ; Milne, Steven (referee) ; Button, Timothy William (advisor)
Piezoelektrické keramické materiály jsou široce používány v mnoha aplikacích a průmyslových odvětvích, nicméně tradiční materiály obvykle obsahují olovo, které je toxické vůči životnímu prostředí. Většina zemí proto zavedla zákony a omezení, které postupně minimalizují spotřebu olova a podporují výzkum v oblasti bezolovnatých kompozic, které by nahradily olověné protějšky. Bezolovnatá piezoelektrická keramika se tak stala žhavým tématem v posledních letech. Nicméně výzkumy na praktické využití bezolovnatých piezoelektrických materiálů jsou jen zřídka publikovány. V této diplomové práci byl vybrán jeden z nadějných kandidátů na piezoelektrickou bezolovnatou keramiku (Ba0.85Ca0.15)(Zr0.1Ti0.9)O3 za účelem zkoumání metody snížení jeho vysoké teploty slinování pomocí dotování uhličitanem lithným, kde syntéza prášku byla připravená pomocí techniky sol-gel. Výsledky byly srovnány s konvenčním práškem syntetizovaným v pevné fázi. Vzorky vyrobené ze sol-gel prášku dopovaného 0.5% hmotn. uhličitanem lithným a slinované při 1300 °C po dobu 2 hodin vykazovaly d33 = 447 ± 9 pC N–1, teplotu Curie 98.7 °C a velikost zrn 7.0 ± 0.3 m. Další důležitou otázkou pro aplikace bezolovnatého piezoelektrického keramického materiálu je jeho výroba v různých konfiguracích. Použitím techniky odlévání pásky a aditivních výrobních postupů byla piezoelektrická keramika zpracována do tří různých konfigurací (2-2, 3-3 a 1-3), aby se překlenula mezera mezi materiálovými vědami a materiálovým inženýrstvím. Pro dolévání pásky byly použity suspenze na bázi oleje a vody. Pro přípravu neslinutých keramických fólií bez trhlin, byly pro odlévání na bázi oleje vyvinuty uhlíkové suspenze s obsahem pevných látek 25% hmotn. a BCZT suspenze s obsahem pevných látek 65% hmotn. Problém práškové hydrolýzy ve vodných suspenzích byl vyřešen povrchovou úpravou prášku Al(H2PO4)3, což umožnilo, aby byly tlusté vrstvy bez trhlin odlety v jednom kroku. Tlusté vrstvy slinované při 1500 °C vykazovaly relativní dielektrickou konstantu 1207, dielektrickou ztrátu 0.018 při 1 kHz, remanentní polarizaci 7.54 µC/cm2 a koercitivní síla intenzity pole (Ec) 0.23 kV/mm při 3 kV/mm. Pro tvarování BCZT v konfiguraci 3-3 a 1-3 byla použita přímá metoda tisknutí inkoustu. Pro správnou úpravu tiskového procesu byla použita inkoustová náplň s viskoelastickým chováním obsahující 41.6% obj. pevných látek BCZT a se zpracovatelskými přísadami (HPMC ~ 2.4% a PEI ~ 0.03%). Vzorky v konfiguraci 3-3, slinované při 1500 °C, vykazovaly nejvyšší dielektrické a piezoelektrické vlastnosti, kde Curieho teplota = 86 °C, tan = 0.021, remanentní polarizace = 4.56 µC/cm2 a d33 = 100 ± 4 pC/N. Vzorky v konfiguraci 1-3 slinované při 1500 °C, které byly smíchány s epoxidem, vykazovaly dielektrickou konstantu 144 a dielektrickou ztrátu 0.035 při 1 kHz. Tato práce popisuje tvarování bezolovnaté piezoelektrické keramiky s vynikajícími vlastnostmi v pokročilých strukturách jako krok k návrhu pro moderní senzorické a energy harvesting aplikace.
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Design of secondary electron detector for ultrahigh vacuum electron microscope
Skladaný, Roman ; Zigo, Juraj (referee) ; Bábor, Petr (advisor)
In this master’s thesis, a mechanical design of an in-column secondary electrons (SE) detector is presented. It is an ultravacuum compatible fibre-scintillation detector designed for use in an ultrahigh vacuum scanning electron microscope (UHV SEM). The designed in-column SE detector was manufactured and tested upon overcoming R&D challenges. The first section of this thesis deals with theoretical basis needed for understanding of functional principles of UHV SEM system and means of SE’s detection. In the second section, mechanical design of the in-column SE detector is described. The last section describes functionality of the designed detector. Effectiveness of light shielding of the detector was tested and the detective quantum efficiency was measured. Finally, images created by the designed in-column detector and an in-chamber SE detector were evaluated and compared.
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Influence of working conditions on the results of EDS in ESEM
Pospíchal, David ; Čech, Ondřej (referee) ; Čudek, Pavel (advisor)
The bachelor thesis deals with energy dispersion spectroscopy and detection of characteristic X-rays in the field of environmental scanning electron microscope. The aim of the semester work is to compare the results of elemental microanalysis of samples under optimal conditions and to monitor changes of results, when changing working conditions, resp. nitrogen and water vapor pressure in the sample chamber of the scanning electron microscope Vega3 XMU with LaB6 cathode. TESCAN, a.s equipped with Xflash 6 | 10 spectrophotometer. Bruker
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Analysis of active material for batteries by EDS
Vídeňský, Ondřej ; Jaššo, Kamil (referee) ; Čudek, Pavel (advisor)
This master thesis deals with analysis of battery mass using x-ray spectral microanalysis. For the measurement two scanning electron microscopes equipped with energy dispersive x-ray spectroscopes were used. Appropriate examples were prepaired by standard method. Then elemental analysis was performed with changing conditions of measurement. Two programs were used for spectrums evaluation and in the end the size of errors was observed for every conditions.
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Optimization of UHV SEM for nanostructure study in wide temperature range
Axman, Tomáš ; Zigo,, Juraj (referee) ; Bábor, Petr (advisor)
This diploma thesis deals with the optimization of ultra-high vacuum scanning electron microscope - UHV SEM, which is developed within the Amispec project in cooperation with BUT, Institute of Scientific Instruments of the Czech Academy of Science and Tescan Brno, s.r.o. The theoretical part deals with the description of the actual state of the developed equipment and the research of competing systems. The next part describes the optimization of the sample holder and the pallet receptor for studying nanostructures over a wide range of temperatures. Part of the optimization is the sapphire thermal diode development and experimental verification of the functionality of the designed components. This is followed by the verification of the functionality of the whole system for the transport of samples to the UHV area, deposition with effusion cell and in-situ observations.
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Optimization of scintillation detector for detection of low energy signal electrons in electron microscopy
Tihlaříková, Eva ; Kadlec, Jaromír (referee) ; Uruba, Václav (referee) ; Neděla, Vilém (advisor)
The dissertation thesis deals with optimization of the scintillation detector for efficient detection of low energy signal electrons in a specimen chamber of a scanning electron microscope. The solution was based on the study of signal electron energy loss mechanisms during their interaction with a conductive layer and a scintillator that can be studied using simulations based on the stochastics Monte Carlo methods. Based on test simulations and their comparison with experimental data, the ideal Monte Carlo software was chosen and used for the study of signal electron energy losses during their transport through the conductive layer as well as following interaction with scintillator, in dependency on the signal electron energy. Simulation results allowed to define criteria for the optimization of the conductive layer. According to these parameters, the optimized layers were deposited on the surface of different scintillators and experimentally tested in the scintillation detector of the scanning electron microscope. Experimental measurements allowed to verify accomplished simulations and provide new information about impact of materials and thicknesses of conductive layers in combination with materials of scintillators and light guides. The increase of the detection efficiency of the scintillation detector equipped with optimised conductive layers and its capability to detect low energy signal electrons were experimentally proved.
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Diagnostic of semiconductor materials by EBIC method
Davidová, Lenka ; Máca, Josef (referee) ; Čudek, Pavel (advisor)
Master´s thesis is focused on diagnostics of semiconductor materials by EBIC method (measuring of currents induced beam), determination of the lifetime of minority carriers, or their diffusion length. The theoretical part is aimed at the principle of scanning electron microscopy, the characteristic properties of the microscope and the signals generated by the interaction of the primary electron beam with the sample. The thesis describes a structure of semiconducting silicon, band models, types of lattice defects and doped of semiconductor structures. After that it is described the theory of calculation of the diffusion length of minority carriers in semiconductors of type N and P. The aim of the experiment part of the thesis is to measure the properties of the semiconductor structure by EBIC and determination of diffusion length and lifetime of minority charge carriers based on the measured data The aim of the experiment part of the thesis is to measure the properties of the semiconductor structure by EBIC and determination of diffusion length and lifetime of minority charge carriers on the basis of the measured data.
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