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Získání 3D informací o struktuře vyvíjeného materiálu Si3N4 pro válcovávání legovaných drátů
Lövy, Vít ; Salamon, David (oponent) ; Chlup, Zdeněk (vedoucí práce)
Diplomová práce se věnuje využití metody 3D EBSD rekonstrukce pro analýzu keramického materiálu nitridu křemíku, určeného na válcovací stolice pro tažení drátů. Díky aplikaci této metody je možné zrekonstruovat zrnovou strukturu v daném objemu a stanovit základní mikrostrukturní parametry. V této práci je kladen důraz na vývoj vhodného postupu pro 3D rekonstrukci struktury tohoto materiálu. Zevrubně jsou popsány jednotlivé kroky od přípravy vzorku ze zkoumaného materiálu, přes nastavení parametrů analýzy až po vyhodnocení a vizualizaci zrnové struktury. Byl navržen zatím nepoužívaný tvar vzorku, který vede ke kvalitnějšímu a rychlejšímu pozorování a tím usnadňuje výslednou mikrostrukturní analýzu keramických materiálů. V této práci jsou také popsány parametry rekonstrukce, jakými jsou geometrie sestavy použité v mikroskopu bez nutnosti mechanického natáčení vzorku, či vliv zvodivění povrchu pomocí in-situ naprašování kovové vrstvy, nebo nastavení elektronového a iontového svazku. Dále jsou popsány dvě možnosti použití softwaru použitých pro výslednou generaci 3D informací o struktuře a posouzení jejich výhod a nevýhod. U zpracování dat 3D struktury materiálu je také posuzován vliv nastavení filtrace a dalších parametrů a jejich vliv na výsledné strukturní parametry.
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Design of nuclear ceramic materials with enhanced thermal conductivity
Roleček, Jakub ; Katovský, Karel (oponent) ; Salamon, David (vedoucí práce)
Uranium dioxide (UO2) is the most common fuel material used in commercial nuclear reactors. The main disadvantage of UO2 is its low thermal conductivity, and large amount of heat generated during the fission in nuclear reactor creates a large temperature gradient in the UO2 fuel pellet. This temperature gradient induces large thermal stress, which leads to fuel pellet cracking. These cracks help to the release of fission product gases after high burnup. The formation of cracks and increase fission gas generation leads to a considerable reduction of fuel pellet durability. This thesis deals with the issue of increasing the thermal conductivity of the UO2 nuclear fuel on model material (CeO2). In this work are studied similarities of the CeO2 and UO2 behavior during conventional sintering and spark plasma sintering. The concept of thermal conductivity enhancement deal with incorporation of high thermal conductivity material – silicon carbide (SiC) into the CeO2 pellets. Silicon carbide is expected to increase the heat flow out of the fuel pellet, and thus increasing the CeO2 thermal conductivity. Similarities of SiC behavior in the CeO2 matrix and SiC behavior in the UO2 matrix reported in literature are also discussed in this work.
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Extremely fast sintering of advanced ceramic materials
Tan, Hua ; Chlup,, Zdeněk (oponent) ; Sedláček,, Jaroslav (oponent) ; Salamon, David (vedoucí práce)
Rapid sintering techniques, such as Spark Plasma Sintering (SPS), Flash Sintering (FS), Selective Laser Sintering (SLS), Induction Sintering (IS), and Microwave Sintering (MS), are designed to effectively and predictably control ceramic microstructure during the sintering process. Spark Plasma Sintering as one of the most novel rapid sintering technique has been studied for decades. There are three main features in SPS: direct Joule heating, pulsed direct current, and mechanical pressure. However, the mechanisms of these features are not clearly and fully addressed. This thesis was inspired by the increasing attention towards rapid sintering techniques and open scientific questions. The present study has four parts, investigation of ‘Field effect’, pulse pattern effect, pressure effect, and direct Joule heating. The results showed the negligible impact of the electromagnetic field during SPS according to the simulation as well as no ‘field effect’ was found during the experiments. While the effect of pulse pattern was significant, the TiO2 powder was sintered by pulse patterns 12:2 and 10:9 with the constant power input. Titania grain size increased one order of magnitude and 8% in density after application of the pulse pattern 10:9, while the amount of consumed energy remained constant. The variation of the effective power and contact resistance induced by the mechanical pulse are two main reasons accounting for the varying energy efficiency heating with different pulse patterns. The pressure timing effect also significantly influenced the SPS. The results showed that applying the pressure at 900 brought high density and small grain size of the sintered alumina nanopowder, leading to the best Vickers hardness. The interaction between pressure and vapor, leading to the different vapor transfer rate of the first sintering stage, was considered as a reason for the differences in microstructure (micropores, grain size, etc.). The timing of the mechanical pressure can also promote the densifying diffusion mechanisms during the second sintering stage, such as grain boundary diffusion and lattice diffusion. The direct Joule heating of the electrically conductive samples by direct electrical current passing through the sample leads to high internal and low measured temperature when sintering boron carbide (B4C) and its composites. Adding titanium alloy and silicon in B4C significantly increased the densification, which was the main reason for the change of mechanical properties. The sample doped by 1 vol. % of Ti alloy (B4C+1.0Ti) reached the hardness 3628.5 ± 452.6 HV1 (16.2% higher than pure boron carbide) with a fracture toughness 2.11 ± 0.25 MPam0.5. The sample doped by 0.5 vol. % of Si (B4C+0.5Si) achieved the hardness 3524.6 ± 207.8 HV1 (13.0% higher than pure boron carbide), the sample B4C+1.0Si achieved the highest fracture toughness 2.97 ± 0.03 MPam0.5 (15.6% higher than pure boron carbide). The grains of titanium doped composites became a bit larger and inhomogeneous compared with the pure boron carbide. In contrast, the grain size of silicon doped samples did not change compared with that of pure boron carbide. The secondary phase silicon carbide was well connected with the boron carbide matrix and showed a great strengthen effect on both the hardness and fracture toughness. This work examined various features of the SPS technique and their effect on ceramic materials, leading to a better understanding of this novel technique.
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Measurement of surface tension for surface characterization of advanced ceramic materials
Mišáková, Liliana ; Kachlík, Martin (oponent) ; Salamon, David (vedoucí práce)
The presented thesis theoretically describes methods applied for the characterization of organic substances presented on the surfaces of advanced ceramic materials. Measurement of contact angles experimentally verifies the changes on surfaces of advanced ceramics. These changes are caused by the contamination of the surface. Adsorption of organic compounds on inorganic surfaces is rather unfavorable, therefore obtained results may provide useful information about the mechanisms of removal of the contaminants from surface. In the experimental part, water contact angle measurements were used to monitor and describe the changes of surface characteristics of ceramic oxides ZnO, TiO2, hydroxyapatite, Al2O3 and ZrO2. WCAs for untreated surfaces along with the WCA values for thermally or chemically treated surfaces of studied materials were assessed and compared in order to describe changes in surface energy, hydrophilicity and adhesivity caused by adsorbed organic adlayer. The decrease of contact angle values was achieved by cleaning of the surface with subsequent deprivation of adsorbed molecules.
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Nanášení kovové vrstvy na keramické substráty pro úpravu povrchových vlastností
Dvorský, Vojtěch ; Kachlík,, Martin (oponent) ; Salamon, David (vedoucí práce)
Práce se soustředí na přípravu povlaku niklu na keramický (Al2O3) substrát. Depozice niklu byla provedena technikou bezproudého pokovování v lázni za různých kinetických podmínek. Rovněž byl zkoumán vliv rozměrů, tvarů a drsností povrchu keramických substrátů. Cílem bylo optimalizovat experimentální podmínky lázně pro přípravu tenkých homogenních kovových vrstev. Připravené povlaky niklu byly charakterizovány pomocí rastrovací elektronové mikroskopie, EDX analýzy, mechanické profilometrie a pokovovací lázeň byla analyzována metodou UV-VIS spektrofotometrie. Modifikací procesu depozice bylo dosaženo souvislých povlaků niklu na keramickém substrátu a byl popsán kinetický mechanismus sledovaného experimentálního systému lázně.
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Syntéza feroelektrických a dielektrických keramických kompozitních materiálů
Čípová, Eva ; Salamon, David (oponent) ; Částková, Klára (vedoucí práce)
Tématem diplomové práce je příprava feroelektrických a dielektrických kompozitních materiálů, konkrétně se práce zabývá přípravou barium stroncium titanitu (BST). V teoretické části jsou popsány možnosti syntéz BST prášků a jejich další zpracování. Experimentální část se věnuje precipitační syntéze barium stroncium titanitu, připravené prášky byly charakterizovány z hlediska morfologie a fázového složení. Dále bylo pro přípravu hutné keramiky využito beztlakého slinování a izostatického lisování za horka (HIP). Sol-gel precipitační syntézou byly připraveny čisté BST prášky, které byly tvarovány a slinovány. Nejvyšší hustoty byly dosaženy při slinování zpomaleným cyklem (pomalé nárůsty teplot a prodleva během slinování) a doslinováním pomocí HIP.
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Tailoring of phase composition and microstructure of calcium phosphate scaffolds applied in regenerative medicine.
Pejchalová, Lucie ; Novotná, Lenka (oponent) ; Salamon, David (vedoucí práce)
Calcium phosphates are the most used ceramic materials for bone regeneration. Calcium phosphates are biocompatible, bioactive and differ in solubility and related degradation in organism. Therefore, calcium phosphate materials are used to regenerate bone defects of small size and as coatings for metallic implants. The solubility of the used materials in body environment after implantation is determined by the ratio of individual calcium phosphates and related degradation rates. This thesis deals with the impact of shaping methods on microstructure and phase composition of calcium phosphates. Commercial hydroxyapatite powder was used as a starting ceramic powder and was treated by calcination at 800 °C for one hour. The biphasic mixture of hydroxyapatite and -tricalcium phosphate was formed during the calcination and this mixture was used for ceramic suspension preparation, with solid loading of 15 vol%, as well as for green bodies preparation. Samples were prepared using several shaping methods: freeze casting, cold isostatic pressing, uniaxial pressing, and slip-casting. Characterization of both, green bodies and sintered samples was performed and the impact of used shaping methods on microstructure and phase composition, was confirmed. It was also observed that the hydroxyapatite content is increasing with increasing porosity, and pore size. This trend applies for samples with unimodal pore size distribution as well as for samples with bimodal pore size distribution.
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Zviditelnění a analýza mikrostruktury částečně slinutých oxidových keramických materiálů
Jemelka, Marek ; Salamon, David (oponent) ; Spusta, Tomáš (vedoucí práce)
Bakalářská práce má za úlohu experimentálně stanovit vhodné parametry leptacích procedur pro leptání částečně zhutnělých keramických materiálů (Al2O3, ZrO2 + 3mol. % Y2O3, ZrO2 + 8mol. % Y2O3) s důrazem na minimální ovlivnění výsledné mikrostruktury. Z výsledků vyplývá, že optimální leptací procedurou pro zvolené materiály je termální leptání za podmínek: Al2O3 (rel. 95,7 ± 0,9 %)- Tlept. = 1015 C (Ts – 350 C), tetragon. ZrO2 (rel. 94,5 ± 0,6 %)- Tlept. = 1005 C (Ts – 350 C), kubic. ZrO2 (rel. 94 ± 0,5 %)- Tlept. = 1105 C (Ts – 350 C). Užitím chemického leptání v prostředí H3PO4 s výdrží 60s je u Al2O3 a kubického ZrO2 možné dosáhnout naleptaného stavu povrchu v kratších časech, nicméně náročnost provedení a volby vhodných parametrů řadí tuto proceduru až za leptání termální. Zviditelnění mikrostruktury vybraných materiálů pomocí iontového svazku bylo experimentálně stanoveno jako nevhodné z důvodu časové a personální náročnosti metody.
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Impact of macro channels on mechanical stability of bone scaffolds during indirect 3D printing
Vojníková, Michaela ; Novotná, Lenka (oponent) ; Salamon, David (vedoucí práce)
Porous materials are currently subject to the great interest of tissue engineering. They provide unique properties such as bioactivity, biodegradability, osteoconductivity, and vascularization. Particularly, ceramic porous systems show appreciable potential in medical applications. However, there is a crucial problem with the porous scaffold on account of their bad mechanic properties and therefore they are presently used only at low-load locations. This thesis focuses on the preparation of the scaffolds made of hydroxyapatite by using the freeze-casting method where the indirect 3D printing was applied to get open channels with the size over 200 µm. It also compares the mechanical properties of the scaffolds with different internal structures and monitors how the implementation of different types of grids affects the resulting stability. The scaffolds were prepared with a different arrangement of macro-channel in the internal structure, but they had equal dimensions as common property. The 3D grid was implemented before freezing into the mold and afterward the grid was eliminated by sintering, leaving only a channel system with the size 540-600 µm in the final scaffold. The influence of the type of the 3D grid on the resulting mechanical stability of the scaffold was determined. Rotation of this grid does not have a significant effect on the result, while it only helps with cracking in the direction of the helix. The combination of these methods reports very good controllability with directed macro-channels in the resulting scaffold and therefore it is suitable for the preparation of the bone-implants with different structures.
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Growth of 3D Structures Induced by Electron Beam on Ceramic Substrates
Bukvišová, Kristýna ; Čechal, Jan (oponent) ; Salamon, David (vedoucí práce)
Irradiation of a sample surface by the electron beam is known to cause structural changes. One type of these changes is vertical growth of 3D structures on surface of ceramic materials. In the thesis, the conditions necessary for such processes are analysed. A calculation of heating effect of the electron beam is conducted, since a temperature rise can trigger several surface changes. Impact of various e-beam parameters on the growth of 3D structures is investigated. Changes of volume and dimensions of the structures related to the beam parameters are studied using the AFM. The estimated temperature increase is in range of units or maximally tens of K. Significant volumetric growth rate is observed at low voltages and currents. Height of the grown structures can reach 100 nm per minute and depends inversely on beam current.
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