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Ceramic dental restoration milling from stock based on ZrO2
Ščasnovič, Erik ; Spusta, Tomáš (referee) ; Kaštyl, Jaroslav (advisor)
In this bachelor thesis, the theoretical overview about the milling of the dental zirconia blanks was performed. The tests of biaxial flexural strength were evaluated in the experimental part, as well as the roughness and the grain size in sintered state and the linear shrinkage was determined. These tests were done for gel cast blanks from zirconia dioxide prepared in laboratories and also for two types of commercially available zirconia oxide blanks fabricated by cold isostatic pressing. The relationship between strength and grain size was shown. The samples prepared from gel cast blanks had statistically significantly higher strength than samples from commercial blanks. At the end of the thesis, the milling of dental crown was carried out based on real tooth model from gel cast zirconia blank studied in this thesis.
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Microstructure revealing and analysis of partially sintered oxide ceramic materials
Jemelka, Marek ; Salamon, David (referee) ; Spusta, Tomáš (advisor)
The goal of this bachelor’s thesis is to experimentally determine appropriate etching conditions for etching of partially sintered advanced ceramic materials (Al2O3, ZrO2 + 3mol % Y2O3, ZrO2 + 8mol % Y2O3) with emphasis on minimal influence on the final surface microstructure. The obtained results show, that the optimal etching way of selected materials is thermal etching under conditions: Al2O3 (rel. 95,7 ± 0,9 %)- Te = 1015 C (Ts – 350 C), tetragon. ZrO2 (rel. 94,5 ± 0,6 %)- Te = 1005 C (Ts – 350 C), cubic. ZrO2 (rel. 94 ± 0,5 %)- Te = 1105 C (Ts – 350 C). The applying of chemical etching in H3PO4 for 60s led to revealing of the microstructure of Al2O3 and cubic ZrO2 in shorter times, but the procedure carries its difficulties of etching conditions determination and execution itself, which put it in the second place. Microstructure revealing via using focused ion beam was experimentally determined as inappropriate due to time and personnel demands.
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Evolution of pores during sintering of advanced oxide ceramic materials
Spusta, Tomáš ; Kaštyl, Jaroslav (referee) ; Maca, Karel (advisor)
The goal of this bachelor’s thesis is to experimentally specify behaviour of pores in oxide ceramic materials (Al2O3, t-ZrO2, c-ZrO2), particularly to describe the transition from open to close porosity. Ceramics powders made by different producers and with different initial particle size (Al2O3 – AKP30, REYNOLDS, TAIMICRON; ZrO2 + 3 mol.% Y2O3 – TZ3Y, TZ3YSB; ZrO2 + 8 mol.% Y2O3 – TZ8Y, TZ8YSB) were used. Samples were pressed by cold isostatic pressing CIP at pressures of 100MPa and 300MPa, and pressureless sintered up to relative densities up to 88-96%. The obtained results show, that evolution is mainly affected by material, independently of size of initial particles neither by initial shaping pressure. Elimination of open pores occurs in cubic ZrO2 at 91-92 % of relative density, in tetragonal ZrO2 at 92-93 % of relative density and in Al2O3 at 94 % of relative density.
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The effect of modification of cermic surface on the sintering of advanced ceramic materials
Vykydal, Adam ; Spusta, Tomáš (referee) ; Pouchlý, Václav (advisor)
This thesis is focused on the effect of modification of ceramic surface on the sintering of the advanced ceramic materials. To modify the surface of ceramic materiál was used method atomic layer deposition. For the research we used materiál TiO2 and materiál TiO2, which was modified using gas in an ALD chamber. To determine the appropriate sintering temperature we used high-temperature dilatometry, where we found that the sintering temperature is about 800 °C. Moreover, the coefficient of thermal expansion (CTE) was determined using subsequent calculation with the data of shrinkage from sintering densification curve. The samples were placed in a kiln where they were sintered on the mentioned temperature on four different dwell times to find effective dwell time for the best value of density of material. Using a scanning electron microscope, the surface-modified material was found to have a uniform structure when sintered to 800 ° C. At a sintering temperature of 1500 ° C, it can be observed that the ZrO2 did not remain only at the grain boundaries, but is more or less evenly distributed. The core-shell structure was not preserved in the structure, however ZrO2 was agglomerated into particles and in the vicinity of these particles titanium dioxide and zirconia react according to the phase diagram. Based on the diagram, it can be stated that this is the ZrTiO4 phase. The occurrence and size of this pase can be verified by RTG analysis.
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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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Fabrication of ceramic materials for piezoelectric applications
Karkuszová, Karina ; Spusta, Tomáš (referee) ; Částková, Klára (advisor)
The content of this thesis is about preparation and processing of lead-free piezoceramic materials with perovskite structure. Potassium sodium niobate (KNN) powder was prepared by solid state reaction (SSR) and liquid phase reaction (sol-gel reaction). The powders were formed by uniaxial and isostatic pressing and further sintered. The density, grain size and morphology were determined on the sintered samples. The powder, synthesised by SSR and sintered in a conventional furnace, was chosen as a standard. The maximum density achieved on samples after optimization of sintering cycle was 93 %TD. The sintering optimization involved a homogenization step at 950 °C, which promotes the correct development of the phase composition and microstructure, followed by sintering at 1120 °C. The same approach and sintering cycle were used for sintering the samples, prepared by sol-gel synthesis. The maximum density of the samples prepared by sol-gel reaction and sintered in a conventional way, was 92 %TD. For further comparison, both of the synthesised powders were sintered using SPS (spark plasma sintering), which increased their final density up to 97 %TD. The approximate value of the piezoelectric coefficient d33 (pC/N) has been measured on selected SSR samples with pure phase composition ((K0,5Na0,5)NbO3). The best measured value of d33 was around 100 pC/N.
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Utilization of theoretical and experimental approaches to sintering for tailoring the microstructure and properties of advanced ceramic materials
Spusta, Tomáš ; Pánek,, Zdeněk (referee) ; Michálková,, Monika (referee) ; Maca, Karel (advisor)
Táto práca sa zaoberá prispôsobením (tailoring) mikroštruktúry vybraných pokročilých keramických materiálov (oxid hlinitý, kubický a tetragonálny oxid zirkoničitý) metódou izostatického lisovania za tepla (post-HIPing) s cieľom pripraviť vzorky s teoretickou hustotou and minimálnou veľkosťou zŕn. Vzhľadom na to, že izostatické lisovanie je vo väčšine prípadov používané ako dokončovacia metóda, pred-slinovanie (príprava vzoriek v štádiu uzavretej pórovitosti) bolo tiež dopodrobna študované. Extenzívny teoretický a experimentálny výskum pred-sintrovania pokročilých keramických materiálov ukázal niekoľko výsledkov. Bolo zistené, že uzatváranie pórov je materiálová charakteristika riadená medzi-povrchovými energiami (uzatváranie pórov nastáva pri 92-96 % t.d. pre skúmané materiály), je nezávislé na technológii prípravy keramického polotovaru a je nezávislé na histórii sintrovacieho procesu. Pre analýzu mikroštruktúry skenovacím elektrónovým mikroskopom a výrazné zvýšenie efektivity mikroštruktúrnej analýzy, bola vyvinutá nízkoteplotná metóda termálneho leptania. Táto metóda umožňuje zviditeľnenie leštenej mikroštruktúry pri leptacej teplote 900 °C a výdrži 1 hodina čiastočne sintrovaných a plne hutných vzoriek bez teplotnej kontaminácie (zvýšenie hustoty a veľkosti zŕn). Pred-sintrované vzorky boli post-HIPované nadizajnovaným kombináciami teploty (1200-1400 °C), aplikovaného tlaku (50 a 200 MPa) a času výdrže (0,5 až 9 hodín) s cieľom štúdia vplyvu týchto post-HIPovacích parametrov na mikroštruktúru vzoriek. Najdôležitejší výsledok experimentov je, že aplikovaný tlak vykazuje iba minimálny vplyv na rast zŕn v priebehu post-HIPovania, pričom výrazne posilňuje zhutňovanie. Sintrovacia teplota a čas výdrže tiež vykazovali zhutňovací potenciál, avšak s negatívnym efektom na veľkosť zŕn počas post-HIPovania rešpektujúc kinetickú rovnicu rastu zŕn – exponenciálny rast pre teplotu a parabolický rast pre čas. Tieto výsledky boli použité pre optimalizáciu post-HIPovacích cyklov pre študované materiály. Výsledné vzorky boli zhutnené nad 99,7 % t.d. a s minimálnym (pod 10 %) nárastom veľkosti zŕn v porovnaní s pred-sintrovanou veľkosťou zŕn. Aplikáciou získaných znalostí bola pripravená transparentná korundová keramika dopovaná erbiom s fotoluminiscenčnými vlastnosťami. Pripravená vzorka s tvrdosťou HV 10 26,9 GPa a so skutočnou inline priepustnosťou RIT 56 % vykazuje najlepšie hodnoty tvrdosti a priepustnosti v doposiaľ publikovaných korundových keramických materiáloch dopovaných prvkami vzácnych zemín.
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Study of transition from open to closed porosity stage during sintering of advanced ceramic materials
Spusta, Tomáš ; Pouchlý, Václav (referee) ; Maca, Karel (advisor)
Lisovanie za tepla (HIP) je pokročilá technológia pre výrobu plne hutných keramických materiálov, ktoré majú množstvo štruktúrnych (napr. rezné nástroje), biologických (napr. implantáty hutných kostí a kĺbov) alebo funkčných (napr. transparentné štíty a okná) aplikácií. Pre úspešné použitie tejto technológie je potrebné, aby predspekané vzorky boli plynotesné, teda bez otvorených pórov. Výskum zaoberajúci sa premenou otvorených pórov na uzatvorené je preto veľmi dôležitý, avšak iba málo publikovaný v odbornej literatúre. Preto bolo experimentálne a teoretické štúdium tohto javu hlavným cieľom diplomovej práce. Analýzy teoretických modelov ukazujú, že transformácia z otvorenej na uzatvorenú pórovitosť je materiálová charakteristika, ktoré sa mení iba s dihedrálnym uhlom, nezávisle na veľkosti častíc prášku alebo na spôsobe tvarovania a nastáva od 92.6% t.d. do 93.7% t.d pre daný materiál (oxid hlinitý, oxid zirkoničitý a horečnato-hlinitý spinel). Tieto teoretické výpočty boli porovnané s experimentálnymi dátami z literatúry a dátami z experimentálnej časti diplomovej práce s úspešnou zhodou pre kubické systémy (spinel a kubický oxid zirkoničitý). Výsledky experimentov s oxidom hlinitým boli v dobrej zhode s experimentálnymi dátami publikovanými v literatúre, ale boli vyššie ako teoretické hodnoty. Na objasnenie týchto odlišností bolo vytvorených niekoľko hypotéz a tiež boli navrhnuté spôsoby riešenia tejto témy.
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Highly porous ceramic materials prepared by Spark Plasma Sintering
Barančíková, Miriama ; Spusta, Tomáš (referee) ; Salamon, David (advisor)
Porous ceramic materials are an interesting group of materials due to a wide range of physical properties, low density, and good permeability. Production of a monolith with a shape stability that would also have a high specific surface area and high porosity is a common problem with porous ceramics. The goal of this work was to maintain the high specific surface area and to produce a monolith with a shape stability. Two forms of porous silica nanofibers (as prepared and milled) were used and partially sintered using the Spark Plasma Sintering method (SPS). Different sintering times and temperatures for SPS were tested. The findings revealed that the best SPS conditions were as follows: temperature: 600 °C, sintering time: 5 minutes, pressure: 3 MPa, and the heating rate: 144 °C/min. These sintering conditions resulted in a stable silica based machinable monolith made from fibers or milled fibers. The monoliths have the specific surface area of up to 470 m^2/g and porosity of 72 %, or the specific surface area of up to 422 m^2/g and porosity of 69 % for as prepared fibers and milled fibers, respectively.
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The printing of the complex shapes by DLP technology from the ceramic materials
Popek, Tomáš ; Roleček, Jakub (referee) ; Spusta, Tomáš (advisor)
This work is focused on the characteristics of advanced ceramics, the basic principles of the 3D printing, and the division of methods for the 3D printing of ceramic materials. It also discusses the removal of the binder from the printed samples, subsequent sintering, and associated TGA analysis and high-temperature dilatometry. Al2O3 ceramic powder was used to print ceramic components, from which two suspensions with a weight fill of 60 and 65 % were prepared. These components have been progressively subjected to TGA analysis and high-temperature dilatometry. The results of the two measurements were used to determine the debinding and sintering cycle. Debinding took place in a vacuum at 410 . As a result, the weights decreased to 63.91 ± 0.45% and 68.62 ± 1.08% of the original weights. The parts were sintered for 120 minutes at 1550 and then the relative densities were measured, which were 87.89 ± 1.05 % and 88.36 ± 0.81 %. The complex components were a turbine with a height of h = 4.4 mm and a diameter of d = 27 mm, a hexagon head screw with a length of 20 mm and an M8 thread, and a nut with a height of 6.5 mm and a width of 13 mm with an M8 thread.
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