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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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Electrical properties of nanoscale heterojunctions formed between GaN and ZnO nanorods
Tiagulskyi, Stanislav ; Yatskiv, Roman ; Grym, Jan ; Schenk, Antonín ; Roesel, David ; Vaniš, Jan ; Hamplová, Marie
Vertical periodic arrays of ZnO nanorods are prepared by hydrothermal growth on GaN templates patterned by focused ion beam. Electro-physical properties of a single vertically-oriented ZnO nanorod are investigated by measuring the current-voltage characteristics using a nanoprobe in a scanning electron microscope. This technique enables to observe the surface morphology of ZnO nanorods simultaneously with their electrical characterization in vacuum. The vacuum chamber rejects the impact of gas adsorption and light irradiation, which both affect the properties of ZnO nanorods. Moreover, mechanical damage and strain induced during the nanorod transfer are eliminated. Nonlinear current-voltage characteristics under the forward bias are explained by the tunneling-recombination process and by the space charge limited current. The high reverse bias current in the p-n heterojunction is attributed to direct tunneling via a narrow tunnel barrier
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Temperature drift compensation for nanostructure analysis
Hakira, Stanli ; Páleníček, Michal (referee) ; Bábor, Petr (advisor)
An ultra high vacuum apparatus for nanostructure experiments is being developed by the Tescan company in cooperation with the Institute of Physical Engineering of the Faculty of Mechanical Engineering. The apparatus is designed for preparation, modification, and analysis of nano-scale structures. A sample holder which allows heating and cooling has been developed for the apparatus. A scanning electron microscope is attached to the chamber to provide analytical and manufacturing capabilities. During experiments with heating enabled, the sample moves relative to the SEM column, causing drift of the image. This bachelor thesis proposes a solution to the problem of temperature drift by the means of motion tracking based on image registration using Fourier transform. An application complementary to the SEM control software which implements the algorithm was designed and tested at the instrument.
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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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Utilization of sampling filters from the Kresin atmospheric station for further analysis
Vítková, Gabriela ; Kahoun, D. ; Strnadová, G. ; Hanuš, Vlastimil ; Petrov, M. ; Tříska, Jan ; Holoubek, Ivan
The Kresin At Pacov Atmospheric Station serves as a monitoring point for the occurrence and remote transmission of greenhouse gases, selected atmospheric pollutants and basic meteorological characteristics. The determination of the GHG concentration (CO2, CH4, N2O, CO) is carried out in air continuously sampled at 10, 50, 125 and 250 m heights. The analysis itself takes place at the foot of a high mast where the air is drawn through the tubes of Synflex 1300. lines and individual analyzers are protected from mechanical pollution by input filters that are changed at regular intervals as part of the routine maintenance of the device or earlier when unexpected clogging occurs. Analyzing these filters can provide additional information about the surrounding area. These are stainless filters (Swagelog „T“ filter) with a porosity of 40 μm. A sampling head is provided in front of them to protect them from rough dirt and water drops. The volume flow of the scrubbed air is about 15 l / min, the exchange interval is usually 3 months. The need to replace these filters has increased in recent months as the flow rate on the sampling lines has fallen. The question arises as to how long the filters remain fully passable and how well they serve their purpose without burdening the sampling system and lowering the measurement quality. The results of analyzes of polycyclic aromatic hydrocarbons (PAHs) carried out on filters at the Institute of Chemistry and Biochemistry of the Faculty of Science of South Bohemian University as well as images from the Scanning Electron Microscope (SEM) could be helpful in answering this question. On the basis of the preliminary results, we propose a more extensive study for the use of this waste material for the analysis of solid particles from the atmosphere in the surroundings of AS Křešín near Pacov and the optimization of the QA / QC sampling systems of greenhouse gas analyzers.
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Preparing of the Chameleon coating by the Ion Jet Deposition method
Skocdopole, J. ; Aversa, L. ; Golan, Martin ; Schenk, A. ; Baldi, G. ; Kratochvílová, Irena ; Kalvoda, L. ; Nozar, P.
Preparation of chameleon coatings using an Ionized Jet Deposition (IJD) technique is reported in the present paper. IJD is a new flexible method for thin film deposition developed by Noivion, Srl. The chameleon coatings are thin films characterised by a distinct change of their tribological properties according to the external conditions. The deposited films of SiC and TiN materials were examined by the Raman spectroscopy, SEM and XPS. The results of the Raman spectroscopy have proved an amorphous structure of SiC films. The data from XPS on TiN films have shown that the\nfilms are heavily oxidized, but also prove that the films are composed of TiN and pure Ti. The SEM provided information about the size of grains and particles constituting the deposited films, which is important for tribological properties of the films. Deposition of the chameleon coating is very complex problem and IJD could be ideal method for preparation of this coating.\n
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