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Mechanical properties of doped piezoceramics based on BaTiO3
Zeman, Dominik ; Chlup, Zdeněk (referee) ; Drdlík, Daniel (advisor)
This master‘s thesis deals with study of basic physical, microstructural and mechanical properties of doped piezoceramic materials based on BaTiO3 prepared by electrophoretic deposition. The dopants used were rare earth oxides, i.e. Eu2O3, Er2O3, CeO2, Dy2O3 and Tb4O7 in amounts 1, 3 and 5 wt. %. The influence of dopants and their amount on density, phase composition, mean grain size, hardness, elastic modulus, fracture toughness, and flexural strength was examined. Suitable dopant choice enabled decrease in mean grain size and increase in relative density, hardness, elastic modulus, fracture toughness and flexural strength of sintered specimens. Relative densities up to 99 %, mean grain size below 1 m, hardness up to 13,1 GPa, elastic modulus up to 199 GPa, fracture toughness above 1 MPa·m1/2 and flexural strength above 115 MPa were achieved.
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Fabrication and properties of doped piezoceramics based on BaTiO3
Mařák, Vojtěch ; Chlup, Zdeněk (referee) ; Drdlík, Daniel (advisor)
This diploma thesis deals with the preparation of doped piezoceramic materials based on BaTiO3 using electrophoretic deposition. Five rare earth oxides, i.e. Er2O3, Dy2O3, Eu2O3, Tb407 and CeO2, were used as dopants in amounts of 1, 3, and 5 wt. %. The prepared deposits were evaluated in terms of preparation methodology, high temperature dilatometry, X-ray diffraction analysis, relative density, mean grain size, hardness and fractographic analysis. The study of dilatometric curves described the sintering behavior and its changes at different material compositions. X-ray diffraction analysis revealed a tetragonal phase in all samples; the tetragonality of the BaTiO3 crystalline cell decreased with dopant content. By a suitable choice of dopant, it was possible to significantly increase the relative density of sintered samples, their hardness and at the same time prevent the samples from coarsening of the microstructure during heat treatment. A relative density up to 98 %, a mean grain size below 1 m and a hardness of over 10 GPa were achieved. Analysis of the fracture surfaces revealed that the fracture mode was transcrystalline for the most of studied materials; only the samples doped with cerium dioxide had fracture surfaces with both transcrystalline and intercrystalline fracture modes. Based on the obtained results, a suitable composition of the material for the intended use in a layered piezoceramic harvester was identified, which, in addition to the BaTiO3 layers, consists of functionally-protective Al2O3 and ZrO2 layers.
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Piezoceramic materials prepared by electrophoretic deposition
Zeman, Dominik ; Chlup, Zdeněk (referee) ; Drdlík, Daniel (advisor)
This bachelor thesis deals with the preparation of piezoceramic materials based on Ba0.85Ca0.15Ti0.9Zr0.1O3 using electrophoretic deposition, which was used for this type of material for the first time. The influence of preparation method, milling time and sintering temperature on mean grain size, relative density, mechanical and piezoelectric properties of samples were investigated. The high energy milling lasting 30-240 min increased electrical conductivity of the suspensions which led to reduction of deposition rate and the density of deposits was increased up to 47.4%. The reduced particle size in green body allowed using of relative low sintering temperature (1350°C) while the deposits with high density of 95.9% and piezoelectric coefficient of d33* = 1027 pm/V were obtained. The hardness of piezoceramic materials prepared was in range of 2.6-3.1 GPa.
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The Role of Bi/Material Interface in Integrity of Layered Metal/Ceramic
Masini, Alessia ; Černý, Martin (referee) ; Bermejo, Raul (referee) ; Chlup, Zdeněk (advisor)
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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PREDICTION OF FRACTURE TOUGHNESS TRANSITION FROM TENSILE TEST DATA APPLYING NEURAL NETWORKS
Dlouhý, I. ; Hadraba, Hynek ; Chlup, Zdeněk ; Válka, Libor ; Žák, L.
Reference temperature localizing the fracture toughness temperature diagram on temperature axis was predicted based on tensile test data. Regularization artificial neural network (ANN) was adjusted to solve the interrelation of these properties. For analyses, 29 data sets from low-alloy steels were applied. The fracture toughness transition dependence was quantified by means of master curve concept enabling to represent it using one parameter - reference temperature. Different strength and deformation characteristics from standard tensile specimens and notched specimens, instrumented ball indentation test etc. have been applied. A very promising correlation of predicted and experimentally determined values of reference temperature was found.
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Prediction of the Traction Separation Law of Ceramics Using Iterative Finite Element Modelling
Kozák, Vladislav ; Chlup, Zdeněk ; Padělek, P. ; Dlouhý, Ivo
Specific silicon nitride ceramics, the influence of the grain size and orientation on the bridging mechanisms was found. In ceramic matrix composites, crack-bridging mechanisms can provide substantial toughness enhancement coupled with the same and/or increased strength. The prediction of the crack propagation through interface elements based on the fracture mechanics approach and cohesive zone model is investigated. From a number of damage concepts the cohesive models seem to be especially attractive for the practical applications. Within the standard finite element package Abaqus a new finite element has been developed; it is written via the UEL (user’s element) procedure. Its shape can be modified according to the experimental data for the set of ceramics and composites. The element seems to be very stable from the numerical point a view. The shape of the traction separation law for four experimental materials is estimated via the iterative procedure based on the FEM modeling and experimentally determined displacement in indentation experiments, J-R curve is predicted and stability of the bridging law is tested.
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Fracture-mechanics behaviour of ceramic foam with macroscopic stress concentrator upon the tensile test
Ševeček, O. ; Majer, Z. ; Bertolla, Luca ; Chlup, Zdeněk ; Kotoul, M.
The work investigates an influence of the macroscopic stress concentrator inside the ceramic open cell foam structure on the fracture-mechanics response of the foam upon the tensile test. As the concentrator, the central crack/rectangular notch was taken into account. The influence of the crack/notch length and width on the stress concentration ahead the concentrator tip was assessed using the simplified FE beam element based model with irregular cells simulating the real ceramic foam structure. Average principal stresses calculated on set of struts ahead the crack/notch tip were compared with average stresses in the intact structure. It was found that the ratio of these stresses increases linearly with the crack length. The stress concentration ratio is slightly lower in case of thick rectangular notch than in case of a thin crack. Furthermore, the failure load leading to complete fracture of the studied specimens, subjected to the tensile loading, were calculated using the same model. It is shown that the difference factor between the critical fracture force in case of structure without concentrator and with concentrator is very close to the concentration factor calculated from the average stresses on particular struts in the region in front of the concentrator tip.\n
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MICROSTRUCTURE EVOLUTION DURING FATIGUE LOADING OF BULK NANOSTRUCTURED ALLOY AL(93)FE(3)CR(2)TI(2)
Chlupová, Alice ; Chlup, Zdeněk ; Kuběna, Ivo
The results of observation of the microstructure evolution during fatigue loading of the bulk nanostructured quasicrystalline Al alloy are presented. Feedstock powder with nominal composition of Al93Fe3Cr2Ti1 produced by gas atomization was hot extruded for powder compaction. The enhanced strengthening of the quasicrystalline nanostructured Al alloy is attributed to the microstructure refinement, formation of supersaturated solid solution, presence of reinforcing icosahedral quasicrystalline phase and work hardening caused by the deformation during extrusion. Good thermal stability is supported by presence of spherical quasicrystalline particles with different interior structure and sizes of up to 250 nm in the diameter. Low cycle fatigue stress-strain characteristics and microstructural evolution of the material were studied. For the microstructure observation the samples of material before and after fatigue loading the TEM and SEM microscopy was employed. The microstructure evolution caused by cyclic loading with positive mean stress was evaluated.
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Behaviour of the Interface of Low Toughness Materials
Halasová, Martina ; Pabst, Willi (referee) ; Tatarko, Peter (referee) ; Fintová, Stanislava (referee) ; Chlup, Zdeněk (advisor)
The work is focused on evaluation of factors influencing behaviour of interface in low toughness ceramic materials reinforced with fibres. The main aim was to characterise processing effects influencing the quality of fibre-matrix interface, with respect to final behaviour of composites at various loading type. The partial goal was to map the possibility of influencing the composite material by choice of matrix material, eventually by change of its processing, leading to change of interfacial properties without need of modification of reinforcement surface. The materials used in studied composites as a matrix were based on thermal transformation of polymer precursors, thus, the resulting materials were characterised in partially as well as in fully pyrolyzed state. Behaviour of interface in cpomposite materials was first evaluated from the global behaviour (i.e., change of mechanical properties) and in chosen representative composites also from the point of local changes in close surrounding of the interface (i.e., microstructure, chemical processes, fracture-mechanic processes, etc.) due to thermal exposition. In experiment were used particularly composite materials prepared by pyrolysis of polysiloxane resins reinforced by basalt fibres or Nextel™720 fibres. With respect to thermal resistance of the reinforcement, the basalt reinforced composites contained only partially pyrolyzed matrix (i.e., to temperature of 800°C), and in composites with Nextel™720 reinforcement was the matrix in form of fully pyrolyzed polymer into ceramic (SiOC). At partial pyrolysis of polysiloxane resin occurs rapid change of behaviour at temperature of 600°C. It was demonstrated, that around this temperature the formed interface with basalt fibre exhibits optimum adhesion/strength, allowing to reach sufficient level of composite strength at acceptable fracture toughness. Above temperature of 750°C occur significant difusion processes in the area of the interface and formation of new crystalline phases in the fibre, what deteriorates the fibre strength, and on the contrary, strengthen the interface cohesion, what leads to degradation of properties of the whole composite. At composite materials determined for high temperatures, reinforced by Nextel™720 fibres, was detected significant resistivity against oxidation caused especially by fully pyrolyzed matrix. As similarly important factor was observed the formation of mullite interphase in surface area of the fibre. Volume changes caused by formation of the interphase, difusional transport of the matter and thermal exposition led to formation of thermally and stress-induced micro-cracks, weakening interfacial surrounding in matrix as well as in fibre. This mechanism in contrast to amplifying chemical bond between fibre and matrix led to preserving of the composite properties also at high temperatures up to 1500°C. The work also dealed with effects of loading rate, where in contrast to static loading were observed different failure mechanisms. Realized research led to description and explanation of the influence of the fibre-matrix interface by change of matrix material processing parameters, which allow processing of economically advantageous and thermally stable composite.
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Behaviour of the Interface of Low Toughness Materials
Halasová, Martina ; Chlup, Zdeněk (advisor)
The work is focused on evaluation of factors influencing behaviour of interface in low toughness ceramic materials reinforced with fibres. The main aim was to characterise processing effects influencing the quality of fibre-matrix interface, with respect to final behaviour of composites at various loading type. The partial goal was to map the possibility of influencing the composite material by choice of matrix material, eventually by change of its processing, leading to change of interfacial properties without need of modification of reinforcement surface. The materials used in studied composites as a matrix were based on thermal transformation of polymer precursors, thus, the resulting materials were characterised in partially as well as in fully pyrolyzed state. Behaviour of interface in cpomposite materials was first evaluated from the global behaviour (i.e., change of mechanical properties) and in chosen representative composites also from the point of local changes in close surrounding of the interface (i.e., microstructure, chemical processes, fracture-mechanic processes, etc.) due to thermal exposition. In experiment were used particularly composite materials prepared by pyrolysis of polysiloxane resins reinforced by basalt fibres or Nextel™720 fibres. With respect to thermal resistance of the reinforcement, the basalt reinforced composites contained only partially pyrolyzed matrix (i.e., to temperature of 800°C), and in composites with Nextel™720 reinforcement was the matrix in form of fully pyrolyzed polymer into ceramic (SiOC). At partial pyrolysis of polysiloxane resin occurs rapid change of behaviour at temperature of 600°C. It was demonstrated, that around this temperature the formed interface with basalt fibre exhibits optimum adhesion/strength, allowing to reach sufficient level of composite strength at acceptable fracture toughness. Above temperature of 750°C occur significant difusion processes in the area of the interface and formation of new crystalline phases in the fibre, what deteriorates the fibre strength, and on the contrary, strengthen the interface cohesion, what leads to degradation of properties of the whole composite. At composite materials determined for high temperatures, reinforced by Nextel™720 fibres, was detected significant resistivity against oxidation caused especially by fully pyrolyzed matrix. As similarly important factor was observed the formation of mullite interphase in surface area of the fibre. Volume changes caused by formation of the interphase, difusional transport of the matter and thermal exposition led to formation of thermally and stress-induced micro-cracks, weakening interfacial surrounding in matrix as well as in fibre. This mechanism in contrast to amplifying chemical bond between fibre and matrix led to preserving of the composite properties also at high temperatures up to 1500°C. The work also dealed with effects of loading rate, where in contrast to static loading were observed different failure mechanisms. Realized research led to description and explanation of the influence of the fibre-matrix interface by change of matrix material processing parameters, which allow processing of economically advantageous and thermally stable composite.
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