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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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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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