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Experimental manufacturing of multiphase Ni-Si based layers
Rončák, Ján ; Moravčík, Igor (referee) ; Jan, Vít (advisor)
The diploma thesis deals with the preparation of the composite material based on the NiSi system using powder metallurgy supplemented by the sintering with the usage of SPS method (spark plasma sintering). Theoretical part contains general information about the mechanical-chemical process and sintering, while materials and methods used for experimental observation are explained in a separate chapter. Experimental part explains the procedure of the experiment and selected parameters of individual processes. In the experiment, two powder mixtures were created in order to form the NiSi phase in the maximum possible amount of powder material. After successfully reaching presence of the NiSi phase in the range of 87 to 89 wt. %, both mixtures were used to produce sintered samples at temperatures from 700 to 900 °C. Experiments showed the best results for sample number 2, which was sintered at 900 °C for 4 minutes. Resulting porosity was 0.9 % and hardness reached a maximum value of 718 HV 1. However, all sintered samples show cracks at room temperature associated with increased brittleness of the material.
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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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High-entropy alloys – bulk alloys and surface treatments
Pišek, David ; Šiška, Filip (referee) ; Hadraba, Hynek (advisor)
Master‘s thesis deals with the preparation and evaluation single-phase high-entropy alloy based on cobalt, chromium, iron, nickel and manganese and its variants strengthened by dispersion of oxidic particles. High-entropy alloy was prepared in powder form by mechanical alloying from the equiatomic proportions of atomic powders. Obtained powder was subsequently compacted by spark plasma sintering. By the method of mechanical alloying were successfully prepared single-phase high-entropy alloy and its variant strengthened by dispersion of nanometric yttria oxides. It has been found that the oxide particles present in the microstructure of high-entropy alloy significantly block mobility of grain boundary and dislocation at elevated temperatures. As a result of this behavior were observed doubling of alloy strength and decreasing of creep rate at 800 °C.
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High-speed sintering of ceramic materials
Chvíla, Martin ; Spusta, Tomáš (referee) ; Pouchlý, Václav (advisor)
Modern ceramic materials are of a key function in a number of applications in all industrial sectors. The process of preparation of the modern ceramic materials includes an important technological step – sintering. Recently methods operating also with sintering by an electric field have been used. These methods are called non-conventional sintering methods (Spark Plasma Sintering, Flash Sintering etc.) and they represent a promising progress in the manufacturing of advanced ceramic materials. These methods provides time and energy saving, and materials produced by these technologies can achieve better specific properties. The sintering in Spark Plasma Sintering have been in the past few years subject of intensive research. Nevertheless, all the sintering conditions (for example the sintering mechanism) in Spark Plasma Sintering are not completely clarified. The aim of this thesis is to summarize the findings about the preparation of advanced ceramic materials using the non-conventional methods of sintering. During experimental work, the effect of the heating rate while sintering by the Spark Plasma Sintering method on the amount of activation energy of sintering that is needed for sintering of the material ZrO2 + 3 mol. % Y2O3 with regard to the microstructure has been investigated. During the thesis was proved that the time and energetic efficiency is increased using the Spark Plasma Sintering method with higher rating rate (50 °C/min compared to 750 °C/min). The relative densities of samples manufactured by using different heating rate with constant pressure stayed almost unchanged. By using higher heating rates, it was possible to achieve a high relative density and shrinkage already at lower temperature. The method of Master Sintering Curve proved that the activation energy of sintering decreases when higher heating rates of sintering were used.
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Advanced ceramic layered materials with heterogeneous microstructure for ballistic applications
Mařák, Vojtěch ; Kachlík, Martin (referee) ; Drdlík, Daniel (advisor)
This bachelor thesis deals with a preparation technology of layered ceramic materials (laminates) with heterogeneous microstructure containing Al2O3 as a matrix with addition of SiC. For the preparation of these materials, dry and wet shaping of ceramic powder with subsequent SPS (Spark Plasma Sintering) was chosen. Due to the goals of the bachelor thesis, the dry shaping proved to be less suitable due to the difficult preparation of the layered structure and the significant wear of the graphitic dies used in the SPS technology. However, the information obtained about mechanical and physical properties has led to the design of the ceramic suspension used in wet shaping (slip-casting). As optimal design 5 vol % of SiC in Al2O3 was chosen. Via this way, ceramic laminates with a sharp layer interface were prepared and the graphitic die wear was minimized. Prepared ceramic samples reached relative density up to 99 % and hardness up to 20.7 GPa. The obtained knowledge has shown the need to optimize the technology of suspension preparation to create ceramic material suitable for ballistic applications.
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Tailoring of microstructure of advanced ceramic materials by conventional and non-conventional sintering approaches
Prajzler, Vladimír ; Bermejo, Raúl (referee) ; Bača,, Ľuboš (referee) ; Maca, Karel (advisor)
Tato doktorská práce se zabývala mikrostrukturálním vývojem vybraných oxidových keramických materiálů během konvenčního slinování (CS), rychlého slinování (RRS), flash slinování (FS) a slinování pomocí plazmatu (SPS). S ohledem na keramiku pro strukturální aplikace byly pomocí RRS připraveny relativně velké (1 cm3), bez defektní a téměř hutné pelety oxidu hlinitého a yttriem stabilizovaného oxidu zirkoničitého (YSZ) s homogenní mikrostrukturou. RRS bylo také shledáno jako optimální metoda pro přípravu vysoce hutné bezolovnaté piezoelektrické keramiky s podobnými vlastnostmi, jako byly získány po časově a energeticky náročnějším CS. Metoda SPS dále zlepšila vlastnosti bezolovnaté piezoelektrické keramiky a produkovala plně hutné vzorky, což je dobrým předpokladem pro translucenci a z níž vyplývajícím optoelektrickým vlastnostem. Nejoptimálnějších výsledků – plné hustoty a vysokých piezoelektrických vlastností – bylo dosaženo kombinací SPS a RRS. Analýzy provedené v této studii také poukázaly na důležitost eliminace těkavých nečistot před rychlým ohřevem. Jinak totiž dochází k zachycení těchto látek ve slinuté keramice, což ve výsledku limituje její konečnou hustotu. Ukázalo se, že nízké konečné hustoty RRS YSZ jsou spojeny se zachycením zbytkového chloru pocházejícího ze syntézy prášku. Pokud byl zbytkový chlor odstraněn vysokoteplotním žíháním keramických kompaktů před zahájením RRS, byly touto metodou získány téměř plně hutné YZS vzorky. Negativní vliv zbytkového chloru na zhutnění byl viditelný také u flash slinovaných YSZ vzorků. Navíc FS YSZ často vede ke zrychlení růstu zrn v jádře vzorku, v důsledku vyšší teploty a elektrochemické redukce. Ve spektru procesních parametrů použitých v rámci této práce dokonce došlo k abnormálnímu růstu zrna (AGG). Silně bimodální distribuce velikosti zrn ukázaná v této práci nebyla dříve nalezena u flash slinutého YSZ. AGG byl vysvětlen dvěma přispívajícími faktory – relativně velkou velikostí vzorku, která vedla k lokalizaci elektrického proudu a vzniku horkých míst (z angl. hot-spots), a celkově akcelerovanou kinetikou růstu zrn v jádře vzorku způsobenou elektrochemickou redukcí.
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Preparation of the lead-free piezoceramic by non-conventional sintering methods
Sršeň, Maroš ; Prajzler, Vladimír (referee) ; Pouchlý, Václav (advisor)
Ceramic materials that exhibit piezoelectric properties currently have a variety of uses in various industries, such as the automotive industry or information technology. Leading materials are currently the best ceramic piezoelectrics, but these materials show considerable toxicity. This has led to the need to find health-safe and environmentally friendly materials based on lead-free piezoelectric materials. Among these materials, KNN-based materials prove to be good candidates. However, their preparation has its own specifications, and therefore the use of conventional sintering methods may not lead to the desired results. It is for this reason that research into the preparation of these materials using unconventional sintering methods that use electric current for sintering has come to the fore in recent years. One of these methods is the Spark Plasma Sintering method, which has therefore been intensively researched in recent years. Within the experimental part of the work, ceramic bodies based on KNN were prepared. Sintering was performed by a conventional method using a laboratory oven, as well as by an unconventional Spark Plasma Sintering method, and the results were compared. Compacting ceramic bodies with high relative density were obtained by sintering by both methods. It has been shown that the Spark Plasma Sintering method can be used to prepare lead-free piezoelectric materials with a high relative density in a relatively short time. It has also been confirmed that the Spark Plasma sintering method has several advantages over conventional sintering methods, and that the ceramic bodies obtained have a higher relative density when sintered by this method.
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