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Design of nuclear ceramic materials with enhanced thermal conductivity
Roleček, Jakub ; Katovský, Karel (referee) ; Salamon, David (advisor)
Oxid uraničitý (UO2) je v současnosti nejčastěji používaným materiálem jakožto palivo v komerčních jaderných reaktorech. Největší nevýhodou UO2 je jeho velmi nízká tepelná vodivost, a protože se při štěpení UO2 v jaderném reaktoru vytváří velké množství tepla, vzniká v UO2 peletě velký teplotní gradient. Tento teplotní gradient způsobuje vznik velkého tepelného napětí uvnitř pelety, což následně vede k tvorbě trhlin. Tyto trhliny napomáhají k šíření štěpných plynů při vysoké míře vyhoření paliva. Tvorba trhlin a zvýšený vývin štěpného plynu posléze vede ke značnému snížení odolnosti jaderného paliva. Tato práce se zabývá problematikou zvyšování tepelné vodivosti jaderného paliva na modelu materiálu (CeO2). V této práci jsou studovány podobnosti chování CeO2 a UO2 při konvenčním slinováním a při „spark plasma sintering.“ Způsob jak zvýšit tepelnou vodivost použitý v této práci je včlenění vysoce tepelně vodivého materiálu, karbidu křemíku (SiC), do struktury CeO2 pelet. Od karbidu křemíku je očekáváno, že zvýší tok tepla z jádra pelety, a tím zvýší tepelnou vodivost CeO2. V této práci je také porovnávána podobnost chování SiC v CeO2 matrici s chováním SiC v UO2, které bylo popsáno v literatuře.
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Extremely fast sintering of advanced ceramic materials
Tan, Hua ; Chlup,, Zdeněk (referee) ; Sedláček,, Jaroslav (referee) ; Salamon, David (advisor)
Techniky rychlého slinování jako „Spark Plasma Sintering (SPS)“, „Flash Sintering“ (FS), „Selective Laser Sintering“ (SLS), „Induction Sintering“ (IS) a „Microwave Sintering“ (MS) jsou navrženy tak, aby účinně a předvídatelně kontrolovaly mikrostrukturu během slinovací proces. Spark Plasma Sintering jako jedna z nejmodernějších technik rychlého slinování a byla studována po celá desetiletí. V SPS má tři hlavní rysy: přímý ohřev elektrickým proudem, pulzní stejnosměrný elektrický proud a mechanický tlak. Mechanismy působení faktorů během SPS procesu však nejsou zatím jasně objasněny. Tato práce byla inspirována zvýšeným zájmem o techniky rychlého slinování a snahou o objasnění působení hlavních faktorů. Tato studie je rozdělena do čtyř částí: efekt elektromagnetického pole, efekt pulzního vzoru, tlakový efekt a přímý Joulův ohřev. Výsledky ukázaly, že elektromagnetické pole v SPS může být ignorováno, jak ukázaly simulace, a rovněž během experimentů nebyl nalezen žádný „efekt pole“. Na druhou stranu účinek pulzního vzoru byl významný, prášek TiO2 byl slinován pulzními vzory 12:2 a 10:9 s konstantním příkonem. Po aplikaci pulzního vzoru 10:9 došlo ke zvýšení velikosti zrna o jeden řád a ke zvýšení hustoty o 8%, zatímco množství spotřebované energie zůstalo konstantní. Při zahřátí s různými vzory pulzů se mění účinný výkon a kontaktní odpor indukovaný mechanickým pulsem, což jsou dva hlavní důvody, které vysvětlují měnící se energetickou účinnost. Vliv tlaku byl také významný, výsledky ukázaly, že použití tlaku při 900 ° C přineslo vysokou hustotu a malou velikost zrn, což vedlo k nejvyšší tvrdosti měřenou podle Vickerse. Interakce mezi tlakem a parami, vedoucí k rozdílné rychlosti přenosu páry v prvním slinovacím stupni, je považována za důvod pro rozdíly v mikrostruktuře, jako jsou mikropóry. Načasování mechanického tlaku může také podporovat difúzní mechanismy zhutňování během druhého slinovacího stupně, jako je difúze na hranicích zrn a mřížková difúze. Přímý ohřev, kdy se vede elektrický proud přímo skrz vzorek, vede k nízké měřené teplotě při slinování karbidu boru a jeho kompozitů, avšak teplota uvnitř vzorku je podstatně vyšší. Přidání slitiny titanu a křemíku do B4C významně zvýšilo finální hustotu, což byl hlavní důvod ovlivnění mechanických vlastností. Vzorek B4C + 1.0Ti (1 obj. % Ti slitiny) dosáhl nejvyšší tvrdosti 3628.5 ± 452.6 HV1 (16.2% vyšší než čistý B4C) s lomovou houževnatostí 2.11 ± 0.25 MPa m0.5. Zatímco při dopování křemíkem dosáhl vzorek B4C + 0.5Si (0.5 obj. % křemíku) nejvyšší tvrdosti 3524.6 ± 207.8 HV1 (o 13.0% vyšší než čistý B4C), vzorek B4C + 1.0Si dosáhl nejvyšší lomové houževnatosti 2.97 ± 0.03 MPa m0.5 (o 15.6% vyšší než čistý B4C). Velikost zrn kompozitů dotovaných titanem se oproti čistému karbidu boru byla o něco větší a mikrostruktura více nehomogenní. Naproti tomu se velikost zrn vzorků dotovaných křemíkem příliš nezměnila ve srovnání s velikostí zrn čistého karbidu boru. Sekundární fáze karbid křemíku byla dobře spojena s matricí karbidu boru a vykazovala pozitivní účinek jak na tvrdost, tak na lomovou houževnatost. Tato práce zkoumala vliv různých kontroverzních a nepopsaných aspektů na slinování keramických materiálů metodou Spark Plasma Sintering, což vedlo k lepšímu pochopení této techniky slinování.
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Preparation of Mg-Ti based bulk materials via powder metallurgy
Žilinský, Martin ; Wasserbauer, Jaromír (referee) ; Březina, Matěj (advisor)
The aim of this thesis is preparation and characterization of bulk Mg–Ti based materials. In the first theoretical part properties of base materials and the complexity of preparation alloy from these metals is discussed. Second part is focused on powder metallurgy and its applicability on Mg–Ti system. In another part particle composites are described. In chapter current research another possible methods of alloy preparation from magnesium and titanium are mentioned. The experimental part of this thesis was the preparation of bulk Mg–Ti materials from metal powders. For sample preparation conventional methods of powder metallurgy and spark plasma sintering was employed. Furthermore a characterisation of these materials was done. Microstructure was observed. Present phases were found using X-ray diffraction analysis. Amounts of these phases were determined using a scanning electron microscope with energy–dispersive spectrometry and using X-ray fluorescence. Furthermore hardness was measured and bending test with evaluation was done. Significant difference in results of sample preparation using conventional methods of powder metallurgy and spark plasma sintering was observed.
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Structure and mechanical properties of magnesium materials prepared by SPS
Pleskalová, Kateřina ; Hutařová, Simona (referee) ; Doležal, Pavel (advisor)
This diploma thesis deals with the processing of the magnesium-based powder materials with the addition of zinc by the spark plasma sintering. The aim of this thesis is to evaluate influence of sintering parameters and zinc content on the microstructure and mechanical properties of the material. First part of the thesis is literary research which is divided into two main chapters. The first chapter describes magnesium-based materials and mentions their use as biomaterials. The second chapter discusses powder metallurgy, specifically magnesium powders and spark plasma sintering. In the experimental part the powders were sintered at temperatures 300 °C and 400 °C and an analysis was performed using optical microscope, scanning electron microscope, then also EDS analysis and hardness, microhardness and three-point bending tests were performed. An increase in hardness was observed with increasing zinc content and with increasing sintering temperature. The flexural strength was higher for materials sintered at a temperature of 400 ° C.
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Modification of SPS quasicrystalline compacts via electron beam treatment
Poczklán, Ladislav ; Lukáč,, František (referee) ; Čížek, Jan (advisor)
The quasicrystals are characterized by unusual rotational symmetries that are not observed in the crystalline materials, which is the cause of their interesting material properties. Because of that a particular attention was paid to quasicrystalline structures in the literature research. The research also contains a description of electron beam technology, spark plasma sintering method and introduction to the problematics of wear. As the default materials for the experimental part were selected Titanium Grade 2 powder and Cristome A5 powder which was partially composed of quasicrystalline phase. The first series of samples was sintered only from powder Cristome A5. The second series was sintered from the mixture of 80 % Titanium Grade 2 powder and 20 % Cristome A5 powder. For the compaction of samples spark plasma sintering technology was selected. Samples were then systematically modified by electron beam and subjected to pin on disc tests. Samples modified at 750 °C had the best wear resistance. Samples modified at 1150 °C contained increased amount of quasicrystalline phase.
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High entropy alloys fabricated via SPS compaction of high energy milled feedstock powders
Gubán, Ivan ; Hadraba, Hynek (referee) ; Čížek, Jan (advisor)
The subject of this thesis is preparation of CoCrFeMnNiNx high entropy mixtures via the methods of mechanical alloying and spark plasma sintering (SPS). Three series of specimens were fabricated in this thesis: samples milled in argon (benchmark materials), samples milled in nitrogen atmosphere (to observe their ability of nitrogen absorption) and samples microalloyed with CrN, FeN nitrides (to observe their dissociation into the solid solution potential). The fabricated powders and SPS compacts were subsequently observed by electron microscopy and their phase content by X-Ray diffraction (XRD) and elemental composition by EDS analysis were carried out. A method of reduction melting in inert atmosphere was used to determine the exact oxygen and nitrogen content in powders, while the respective particle size distribution measured by laser diffraction method. The influence of nitrogen content on the hardness of the samples was studied via the microhardness measured. After completing the process of mechanical alloying under the Nitrogen atmosphere was the maximal concentration of nitrogen in the structure 0,208% after 24 hours of milling (dependency on time was linear), which means, the method of milling under the Nitrogen atmosphere was successful. XRD of milled samples showed the existence of the only FCC single solid solution phase, while samples milled under the Nitrogen atmosphere showed the trend of the growth of the lattice parameter with the increasing nitrogen content. There was observed the presence of the chromium nitrides precipitates on the grain boundaries of the FCC phase in microalloyed samples. All specimen were contaminated by a mixture of metallic oxides and manganeese sulphides, which were present in the default manganeese powder. The greatest value of microhardness showed the duplex sample. The increase in values of microhardness (344 HV 0,3) in comparison with the standard sample (262,9 HV 0,3) was recorded on the samples milled under the nitrogen atmosphere, which conforms the positive influence of the nitrogen content on strength characteristics of this alloy.
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Properties of quasicrystal-reinforced high entropy alloys
Adami, Martin ; Tesař,, Tomáš (referee) ; Čížek, Jan (advisor)
This diploma thesis deals with the processing of the high-entropy alloys with the addition of quasicrystals by the spark plasma sintering method. The aim of this thesis is to evaluate the influence of quasicrystals content on the microstructure and wear resistance. The literature review part is divided into several section. The first part is an overview of high-entropy alloys and quasicrystals, including their properties and production methods. The next part pertains to spark plasma sintering and the wear phenomenon. In the experimental part, spark plasma sintering compacts were produced at 1100 °C and an analysis was performed using scanning electron microscope as well as X-ray diffraction and their tribological properties were measured by the pin-on-disc method. It was found that increasing the content of quasicrystals triggered an improvement in the compacts’ wear resistance.
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The influence of heating rate on two step sintering of advanced ceramic materials
Klevetová, Tereza ; Maca, Karel (referee) ; Pouchlý, Václav (advisor)
Recently, there has been growing interest in new technologies and procedures to improve the microstructure of advanced ceramic materials. One of the most commonly used sintering methods is Two step sintering (TSS), Rapid rate sintering (RRS) and Spark plasma sintering (SPS). Within the framework of this bachelor thesis number of experiments were carried out for the research of the microstructure interconnecting the Two step sintering with the Rapid rate sintering and non-preassure Spark plasma sintering. The aim of this work was to determine the influence of the heating rate on the size of final relative density and the average grain size for ceramic materials based on ZrO2. The results of the study show that occurrence of the „core-shell“ structure on the ZrO2 doped by 3 mol.% Y2O3 (TZ-3Y) tend to production of non-homogenous microstructure with a fully compacted surface and a porous center. In the case of ZrO2 doped by 8 mol.% Y2O3 (TZ-8Y) this structure was detected only in several cases at higher heating rates. An the same time it was found that the final relative density decreases with increasing heating rate. Using cubic ZrO2 with larger grain size (TZ-8YSB), the „core-shell“ structure did not appear, however a lower relative densities of about 98 % t.d. was always achieved, regardless of the applied temperature profile. The best results were obtained with TZ-8Y using Spark plasma sintering and Rapid rate sintering. Smaller grain size was obtained as compared with conventional methods of other authors. The difference in grain size was just within the framework of the standart deviation. This work doesn’t show any positive influence of Rapid rate sintering on the resulting grain size.
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Preparation of transparent advanced ceramic base on Al2O3.MgO
Chvíla, Martin ; Maca, Karel (referee) ; Pouchlý, Václav (advisor)
Ceramic materials are in general characterized by high hardness, high modulus of elasticity, excellent abrasion resistance, etc. These properties make ceramics among others useful in optically transparent applications. An ideal form of optically transparent ceramic material is monocrystalline. However, the monocrystalline fabrication is expensive and/or time consuming. From this point of view polycrystalline ceramics is preferred. But the polycrystalline transparent ceramics fabrication is fraught with complications such as porosity, inappropriate grain size and insufficient purity. These circumstances could be solved by using sintering additives. This master’s thesis compiles literature research summarizing modern technologies of advanced ceramics sintering and ceramic polycrystalline microstructure dependence on its optical properties. The experimental part of this thesis focuses on the fabrication parameters of polycrystalline advanced ceramics based on Al2O3MgO and evaluation of their optical properties. Polycrystalline magnesium-aluminate spinel with sintering additive contents 0; 0.3 and 0.6 weight % LiOH was fabricated by optimalisation of Spark Plasma Sintering cycle. Fully dense ceramic samples of polycrystalline magnesium-aluminate spinel with favourable optical properties in visible spectrum radiation were achieved. Real In-line Transmission RIT and Total Forward Transmittance TFT were analysed. RIT exceeded 84 % at wavelength of 633 nm and TFT exceeded 83 % at wavelength above 860 nm. The decisive factors in terms of the optical properties of ceramics sintered with sintering additives were the amount of time-spending at high temperatures and the purity of ceramic powders.
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