Four silicon nitride powder blends vary in starting powder characteristics, glass chemistry, and phase composition. This work focuses on how these properties influence densification behavior, microstructural development, and the resulting mechanical performance of dense ceramics. Previous work completed on alpha-rich, low oxide containing (8 wt%), and fine silicon nitride powder (GS-44) showed high hardness equiaxed with grained ceramic. GS-44 served as an excellent precursor for the matrix phase material in graphene reinforced composites, which resulted in 235% increase in toughness and high hardness retention [1] with the addition of 1.5 vol% graphene. As the GS-44 powder is no longer in production, investigative work into other commercial powders and customization of powder blends was initiated. Commercial blends were selected based on availability, high alpha content, fine particle size, and additive chemistry (Al2O3, MgO, and Y2O3). The objective was to understand which powder characteristics led to a ceramic design that contained high hardness, strength, and toughness properties in order to increase the use of silicon nitride in extreme temperature environments. One such example is aerospace and structural applications that require a high-performance material that is lightweight and good thermal stability. Strong covalent bonding in silicon nitride make densification of powders extremely difficult; thereby, sintering additives are necessary to promote liquid phase sintering processes. Compaction of ceramic powders was carried out using a spark plasma sintering (SPS) furnace by utilizing a pulsed direct current through a conductive graphite die that encapsulates the sample powder. SPS was preferred over other conventional sintering methods owing to its high heating rate and short dwell times at the sintering target temperature. Thus, SPS provides superior control for tailoring the final silicon nitride properties by producing a hard alpha-phase and tough beta-phase microstructures. The custom blend developed had an appreciable amount of media wear included during the milling process that increased the additive content. Development of the custom blend was used to understand the effect of a larger additive content. Commercial GS-44 blend was used as the control to track the effect of adjusting specific surface area and oxide content in silicon nitride powder systems (HCS-M, C-R3, and UA-SN). The mechanical results for the four matrix systems, showed that toughness increased with grain coarsening and minimization of alumina content in beta silicon nitride. Based on these findings it is important to determine tradeoffs (i.e. balance of high hardness, toughness, and strength) to engineer an optimal ceramic that can be used for structural and aerospace applications.

The diploma thesis deals with phase composition measurement of the TRIP steel, using EBSD method. The steel was delivered as thermo-mechanically treated via two different routes. The phase composition of the steel was examined during gradual plastic deformation in the range 0 to10.99%. One route of thermo-mechanical treatment exhibited good agreement with the literature in terms of measured fraction of the retained austenite (15.6%) as well as its decrease during the deformation (to 8.9% at the maximum imposed strain). The samples of the second route did not show any agreement in either of the parameters spoken.

The dissertation thesis is devoted to the study of belite clinkers and to the possibilities of the increase in their hydraulic activity. The mechanism and the kinetics of belite clinker formation were studied together with the relation of the velocity of these processes and the hydraulic activity of clinker. The influence of various parameters (degree of lime saturation, duration and temperature of burning) of the belite clinker preparation on the belite clinker development in time, on belite polymorphism, on the chemical composition of belite crystals and on the belite cement hydraulic activity was studied, too. The research methods used for the investigation involved electron microscopy, optical microscopy, X-ray diffraction analysis, high-temperature microphotometry and calorimetry. The resulting clinkers were hydraulically activated by addition of calcium sulfate. The experiments have proven that the higher rate of belite formation does not lead to the increase of its hydraulic activity, as opposed to that of alite. On the other hand, the chemical activation by sulfate anions enables to prepare clinker with relatively higher degree of lime saturation with minor admixture of alite and anhydrite, which is hydraulically activated. The work was concluded by experimental burning of belite clinker doped with sulfate anions in a model rotary kiln and by the preparation of cements blended with common industrial alite clinker. The results indicate the possibility of separate industrial production of special belite clinker alongside with common alite clinker and the production of economically and environmentally beneficial blended Portland cements with suitable technological parameters, or targeted production of special cements with properties corresponding to their required utilization.

Commercially important hydrogenation reactions make use of precious noble metal catalysts which are becoming increasingly scarce, and the search for capable alternative catalysts prevails. Transition metal carbides of group IV-VI metals show similar catalytic behavior to platinum and are $103/kg lower in price than the precious metal catalysts. Tungsten carbide, studied in this work, can form in different stoichiometries and phase compositions depending upon synthesis methods. Synthesis of high surface area tungsten carbide with control over its phase composition remains a challenge currently. In this work, the novel isothermal synthesis method of tungsten carbide (WC, W2C) in a CH4/H2 carburization atmosphere with synthesis temperature and presence or absence of a silica support in the catalyst precursor (WO3) as process variables was investigated. The amounts of CO and H2O formed during synthesis corresponded to the amount of oxygen in the WO3 precursor. The catalysts were further characterized by X-ray diffraction to determine phase composition and crystallite size, by scanning electron microscopy to determine morphology, and by CO chemisorption to determine metallic surface area. X-ray diffraction analysis indicated the carbide catalysts to contain W2C, WC, and metallic W phases. The use of a silica-supported precursor favored the formation of a nearly phase pure, high surface area W2C rich catalyst whereas high synthesis temperature and absence of silica precursor favored formation of a low surface area WC rich catalyst. Further, the catalysts were tested for steady state activity at a W/F (weight catalyst/toluene feed rate) of 0.20-0.30 h-1, addition of H2 to a total pressure of 21 bar absolute and 250 °C, and the effect of phase composition and surface area on the activity was studied. This work resulted in the successful synthesis of 4 tungsten carbide catalysts with varying phase compositions and surface areas and correlation of their compositions and surface areas with their corresponding toluene hydrogenation activities.

OBJECTIVES: This study aims to fill these voids in the literature regarding the microstructure, mechanical and optical properties of multilayered zirconia subjected to repeated firing. It will aim to increase knowledge and understanding of this type of novel material, whether multilayered by chroma or composition. MATERIALS AND METHODOLOGY: The three materials examined are ZirCAD Prime by Ivoclar Vivadent, Origin Beyond+ Hybrid by B and D Dental Technologies, and Katana HTML by Kuraray Noritake. Beam-shaped specimens were sectioned to the correct size from discs of the three zirconia materials and subsequently cleaned, polished, and annealed. Ten specimens taken from each group were subjected to one, three, and five repeated firings, which were then used for the destructive flexural strength test using a universal testing machine. Another set of smaller specimens were produced and used for the non-destructive tests, prepared in the same manner as the other specimens, with 2 samples present in each group. These small specimens were examined for the following properties: contrast ratio and CIELAB measurements on a white and black background using a spectrophotometer, crystallographic phase changes using x-ray diffraction (XRD), and elemental analysis using energy dispersive spectroscopy (EDS). RESULTS: Repeated firings did not have any significant effects across all brands of materials for all tests conducted. However, significant differences existed between the different materials, and within their different layers for all tests conducted unrelated to repeated firing. Significant differences only existed in flexural strength depending on annealing, polishing status, type of polishing, and size independent of repeated firing. Annealing yielded weaker specimens than non-annealed, polished specimens were stronger than non-polished ones, automated polishing resulted in stronger specimens than manually polished ones, and smaller specimens were stronger than larger ones in terms of flexural strength. CONCLUSIONS: Within the limitations of this study, repeated firing has no significant effects on the various multilayered zirconia tested in this study. There is a significant difference in flexural strength between the materials studied. Significant differences in flexural strength also existed between specimens that were annealed versus ones that were not; and between specimens that were polished versus ones that were not. This study has increased knowledge regarding this novel material.

Electrospininig se osvědčil jako jeden z nejpopulárnějších a nejrozšířenějších způsobů výroby vysoce kvalitních vláken s požadovanými parametry. Kvalita a morfologie vyráběných vláken závisí na mnoha parametrů, jako je vlhkost, dávka materiálu, aplikované napětí atd. Omezení keramických piezomateriálů (křehkost, toxicita vzorků obsahujících olovo, obtížnost přípravy složitých tvarů atd.) vynutila výzkum v oblasti piezoelektrických polymerů. Jedním z nich je polyvinylidenfluorid (PVDF). polyvinylidenfluorid může by být připraven v různých formách: tenké filmy, objemové vzorky, vlákna. PVDF vlákna přitahují největší pozornost díky vysoké flexibilitě, nízké hmotnosti, mechanické stabilitě a chemické inertnosti. Vlastnosti PVDF vláken lze zlepšit pomocí doplňujících materiálů: keramické částice, kovové nanočástice, Graphicitové materiály jako jsou oxid Graphicenu nebo uhlíkové nanotrubičky (CNT).

DIPLOMA THESIS IS DEVOTED TO THE STUDY OF PREPARATION OF PURE BELITE CLINKER FOR THE POTENTIAL INCREASE OF KINETICS OF THE HYDRATION PROCESS BY CHEMICAL ACTIVATION. THE THESIS OF THIS WORK IS BASED ON RESEARCH FINDINGS CONCERNING BELITE CLINKER AND RESEARCH AT THE INSTITUTE OF THD. THE THESIS AIMS TO DESIGN COMPOSITION OF THE RAW MEAL BURNING BELITE, FOLLOWING MODIFICATION BY SULPHATE AND POTASSIUM CARBONATE IN ORDER TO POTENTIALLY INCREASE THE REACTIVITY OF THE BURNT BELITE CLINKER AND THE LABORATORY FIRING OF PREPARED SAMPLES. THE LAST STEP WAS TO ASSESS THE MINERALOGICAL COMPOSITION OF BURNED SAMPLES XRD ANALYSIS AND FOLLOWING COMPARISON CELL PARAMETER OF BELITE WITH AND WITHOUT ADDED MODIFYING ADDITIVES.

In the study the influence of different dental technical tools on the surface temperature and phase composition of fixed dental prostheses (FDPs) made of yttria-partially stabilized zirconia polycrystals (3Y-/4Y-/5Y-PSZ) was investigated. FDPs were fabricated by using computer-aided manufacturing (CAM). The FDPs were treated with a contra-angle handpiece equipped with different burs and polishers. The resulting surface temperatures were measured with a thermographic camera, and the resulting phase transformations were investigated by X-ray diffraction and quantified by Rietveld refinement. Processing with burs resulted in no phase transformation, but a preferred orientation shift. Using coarse polisher induced a phase transformation to the rhombohedral phase, while fine polishers produced no relevant phase transformations and no preferred orientation shift. Compared to the monoclinic phase (ca. 9% theoretical volume increase), which is associated with low-temperature degradation (LTD), the rhombohedral phase is much more voluminous (ca. 15% theoretical volume increase) and distorted and, therefore, has a greater degradation potential.

No / The kinetics of the dissociation is fundamental to the formation and the in vivo performance of cyclodextrin supramolecules. The individual determination of the apparent dissociation rate constant (kd,app) using high performance affinity chromatography (HPAC) is a tedious process requiring numerous separate studies and massive data fitting. In this study, the multianalyte approach was employed to simultaneously measure the kd,app values of three drugs through one injection based on the investigation of the dependence of drug-cyclodextrin interaction kinetics on the mobile phase composition. As a result, the kd,app values increased when decreasing the ion strength, increasing the ionization of drugs and adding extra organic solvents. The values of kd,app for acetaminophen, phenacetin and S-flurbiprofen estimated by the multianalyte approach were 8.54+/-1.81, 5.36+/-0.94 and 0.17+/-0.02s(-1), respectively, which were in good agreement with those determined separately (8.31+/-0.58, 5.01+/-0.42 and 0.15+/-0.01s(-1)). For both of the single and multiple flow rate peak profiling methods, the results of the multianalyte approach were statistically equivalent with that of the single compound analysis for all of the three drugs (p>0.05). The multianalyte approach can be employed for the efficient evaluation of the drug-cyclodextrin kinetics with less variance caused by cyclodextrin column bleeding.

Alloying aluminum offers the possibility of creating low-density high-entropy alloys (HEAs). Several studies that focus on the system AlCoCrFeNiTi differ in their phase determination. The effect of aluminum on the phase composition and microstructure of the compositionally complex alloy (CCA) system AlxCoCrFeNiTi was studied with variation in aluminum content (molar ratios x = 0.2, 0.8, and 1.5). The chemical composition and elemental segregation was measured for the different domains in the microstructure. The crystal structure was determined using X-ray diffraction (XRD) analysis. To identify the spatial distribution of the phases found with XRD, phase mapping with associated orientation distribution was performed using electron backscatter diffraction. This made it possible to correlate the chemical and structural conditions of the phases. The phase formation strongly depends on the aluminum content. Two different body-centered cubic (bcc) phases were found. Texture analysis proved the presence of a face-centered cubic (fcc) phase for all aluminum amounts. The hard η-(Ni, Co)3Ti phase in the x = 0.2 alloy was detected via metallographic investigation and confirmed via electron backscatter diffraction. Additionally, a centered cluster (cc) with the A12 structure type was detected in the x = 0.2 and 0.8 alloys. The correlation of structural and chemical properties as well as microstructure formation contribute to a better understanding of the alloying effects concerning the aluminum content in CCAs. Especially in the context of current developments in lightweight high-entropy alloys (HEAs), the presented results provide an approach to the development of new alloy systems.