Národní úložiště šedé literatury Nalezeno 2 záznamů.  Hledání trvalo 0.00 vteřin. 
Tailoring of microstructure of advanced ceramic materials by conventional and non-conventional sintering approaches
Prajzler, Vladimír ; Bermejo, Raúl (oponent) ; Bača,, Ľuboš (oponent) ; Maca, Karel (vedoucí práce)
This doctoral study investigated microstructural evolution of selected oxide ceramic materials during conventional sintering (CS), rapid rate sintering (RRS), flash sintering (FS), and spark plasma sintering (SPS). Considering ceramics for structural applications, the relatively large (1cm3), defect-free, and nearly dense alumina and yttria-stabilized zirconia (YSZ) pellets with uniform microstructure were prepared by RRS. The RRS was also found as an optimal method for preparation of highly dense lead-free piezoelectric ceramics with the similar performance as obtained by more time- and energy-consuming CS. The SPS methods further improved the properties of lead-free piezoelectric ceramics, producing fully dense samples which is a good prerequisite for translucency, and thus, additional optoelectrical properties. The most optimal results – a full density and high piezoelectric performance – were attained by combining SPS and RRS approaches. The analyses performed in this study also pointed out the importance of elimination of volatile impurities prior to the rapid heating. Otherwise, these substances are trapped in the sintered ceramic, which in turn limits its final density. It was shown that the low final densities of RRS YSZ are connected to the entrapment of residual chlorine originating from powder synthesis. If residual chlorine was removed by high-temperature annealing of the green bodies before the onset of RRS, almost fully dense YSZ samples were obtained by following RRS. The negative effect of residual chlorine on densification was also visible in flash sintered YSZ samples. Moreover, the FS of YSZ often results in an accelerated grain growth in the sample core due to a higher temperature and electrochemical reduction. In the spectrum of our process parameters, it even led to abnormal grain growth (AGG). The strongly bimodal grain size distribution showed in this work was not reported in flash sintered YSZ before. The AGG was explained by two contributing factors – large sample size, which resulted in localization of electric current and formation of hot-spots, and overall accelerated grain growth kinetics in the specimen core caused by electrochemical reduction.
The Role of Bi/Material Interface in Integrity of Layered Metal/Ceramic
Masini, Alessia ; Černý, Martin (oponent) ; Bermejo, Raul (oponent) ; Chlup, Zdeněk (vedoucí práce)
The present doctoral thesis summarises results of investigation focused on the characterisation of materials involved in Solid Oxide Cell technology. The main topic of investigation was the ceramic cell, also known as MEA. Particular attention was given to the role that bi-material interfaces, co-sintering effects and residual stresses play in the resulting mechanical response. The first main goal was to investigate the effects of the manufacturing process (i.e. layer by layer deposition) on the mechanical response; to enable this investigation, electrode layers were screen-printed one by one on the electrolyte support and experimental tests were performed after every layer deposition. The experimental activity started with the measurement of the elastic characteristics. Both elastic and shear moduli were measured via three different techniques at room and high temperature. Then, uniaxial and biaxial flexural strengths were determined via two loading configurations. The analysis of the elastic and fracture behaviours of the MEA revealed that the addition of layers to the electrolyte has a detrimental effect on the final mechanical response. Elastic characteristics and flexural strength of the electrolyte on the MEA level are sensibly reduced. The reasons behind the weakening effect can be ascribed to the presence and redistribution of residual stresses, changes in the crack initiation site, porosity of layers and pre-cracks formation in the electrode layers. Finally, the coefficients of thermal expansion were evaluated via dilatometry on bulk materials serving as inputs for finite elements analyses supporting experiments and results interpretation. The second most important goal was to assess the influence of operating conditions on the integrity of the MEA. Here interactions of ceramic–metal interfaces within the repetition unit operating at high temperatures and as well at both oxidative and reductive atmospheres were investigated. The elastic and fracture responses of MEA extracted from SOC stacks after several hours of service were analysed. Layer delamination and loss of mechanical strength were observed with increasing operational time. Moreover, SEM observations helped to detect significant microstructural changes of the electrodes (e.g. demixing, coarsening, elemental migration and depletion), which might be responsible for decreased electrochemical performances. All the materials presented in this work are part of SOC stacks produced and commercialised by Sunfire GmbH, which is one of the world leading companies in the field.

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