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Advanced high-temperature resistant metal-ceramic composites based on TiB2 for cutting tools
Halmazňa, Jiří ; Drdlík, Daniel (referee) ; Chlup, Zdeněk (advisor)
This diploma thesis deals with the preparation of new high-temperature resistant cermets based on TiB2. The hard ceramic phase is bonded by NiW metallic alloy, which was prepared by mechanical alloying using a planetary ball mill. The first part of the thesis is targeted to the optimization of mixing of both powders in the planetary ball mill. The procedure of preparation of powders mixture with homogenous particles distribution of the NiW alloy was designed and verified with simultaneous particle size refinement. The second part is focused on the microstructure characterisation and mechanical properties evaluation of sintered materials. In this case both powders, TiB2 and NiW, were mixed in a tubular mill and consequently compacted by a rapid hot pressing method at four different sintering temperatures. The influence of the sintering temperature on the microstructure development characterized by the density, porosity and grain size was monitored. The elastic modulus, fracture toughness, flexural strength and hardness were measured on prepared test specimens. The results of conducted experiments show a significant dependence of the microstructure and mechanical properties on applied sintering temperatures. The higher sintering temperatures are used the better mechanical properties are observed. However, the sintering temperature of 1375°C seems to be an optimal one. The sintering temperature of 1400°C leads to the significant losses of the metal phase due to sublimation of nickel resulting in increased porosity in the metal phase regions.
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3D microstructure evaluation of developed Si3N4 material for alloyed wire rolling applications
Lövy, Vít ; Salamon, David (referee) ; Chlup, Zdeněk (advisor)
This diploma thesis is devoted to the use of 3D reconstruction using EBSD method for microstructural analysis of silicon nitride ceramic material predetermined for the rolling-mill used in the wire production. Application of this method can be used for the grain structure reconstruction and basic microstructural parameters can be than extracted. The development of a suitable method for 3D reconstruction of the structure of the materials the main aim of this work. There are described the different steps begun by sample preparation from the investigated material trough the optimisation of analysis parameters up to the visualization of the grain structure. New type of sample geometry has been designed which leads to the better and faster observation of the microstructure of ceramic materials. This thesis also describes optimal reconstruction parameters such as the geometry of the assembly used in the microscope without mechanical movement of the sample or the influence of conductive coating prepared via in-situ sputtering of suitable metal, or adjustment of the electron and ion beams. Further are described two options of software which can be used for the final generation of 3D structure information and are assessed their advantages and disadvantages. The effect of the filter setting and other parameters and their influence on the resulting structural parameters are also evaluated.
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Low temperature tests and fracture toughness of selected ceramic materials
Beck, Branislav ; Drdlík, Daniel (referee) ; Chlup, Zdeněk (advisor)
Diploma thesis deals with the determination of fracture toughness values of sintered silicon carbide and casted basalt using both the Single Edge V-Notch Beam (SEVNB) and the Chevron Notched Beam (CNB) methods at room and cryogenic temperatures. The first part of this thesis offers general overview and categorization of ceramic materials. Fracture mechanics of the ceramic materials and available fracture toughness testing methods are discussed in following chapters. The last section in the theoretical part is aimed to the microstructure and properties of the silicon carbide. Experimental part of the work summarizes methods used for characterization of selected materials from the microstructural and fracture point of view. Preparation of samples for microstructural observation and samples for fracture toughness determination are described in details. The results of the fracture toughness data for sintered silicon carbide and cast-basalt obtained at room temperature and at -100 °C are displayed. Consideration of possible measurements errors and application of various fracture toughness testing methods are discussed in the next chapter of this work. The difference in the fracture toughness values with the decrease of testing temperature was found. The difference depends on both, the used method of fracture toughness determination and the material used for the tests. The most important results gained during the experimental work are summarized in the chapter “Conclusions”.
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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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Optimisation of fibre-matrix interface in ceramic matrix composite
Halasová, Martina ; Černý,, Martin (referee) ; Chlup, Zdeněk (advisor)
This thesis is concerned to the study of behaviour of fibre composites with ceramics matrix. The composite consists of pyrolysed polysiloxane matrix reinforced by ceramic fibre Nextel 720. Main aim of this work is optimisation of fibre matrix interface through the selection of suitable precursor of the matrix with respect to temperature stability, sufficient strength and reasonable fracture toughness. Samples of matrices were exposed to the long term heat treatment in the range 1100 – 1500 °C. The mechanical properties as hardness and indentation elastic modulus were determined after heat treatment. Selected precursors of matrices were used for composite fabrication. Elastic modulus and fracture toughness at room and elevated temperatures were studied. Discussion is dedicated to the description of changes in mechanical properties with respect to chemical processes taking place during high temperature exposition. Further, reasons of fracture behaviour of composite materials are discussed, and finally, gained knowledge and outlined possibilities of subsequent development are summarised.
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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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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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Transparent fibre reinforced ceramics
Lövy, Vít ; Drdlík, Daniel (referee) ; Chlup, Zdeněk (advisor)
This bachelor thesis summarizes possibilities of toughening of ceramic materials with various types of fibres and describes the basic principles for preparation of transparent fibre-reinforced composite materials. The role of fibre-matrix interface and the measurement methods enabling estimation of the interfacial strength and other characteristics are explained. The single fibre push-out test using a standard indentation technique was chosen for interfacial parameters determination of the composite consisting from a borosilicate matrix reinforced by SiC fibres in the practical part of this work.
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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 microstructure evaluation of advanced oxide ceramics during fast sintering
Prajzler, Vladimír ; Chlup, Zdeněk (referee) ; Maca, Karel (advisor)
The diploma thesis deals with influence of fast pressure-less sintering on the microstructure of advanced ceramic materials, namely -Al2O3 and tetragonal ZrO2 (doped by 3 mol% Y2O3) with particle sizes ranging from 60 nm to 270 nm. Fast and controlled heating rate was enabled by utilization of the special superkanthal furnace with moving sample holder. Defect-free bulk and dense samples were prepared using heating rates in order of 100-200 °C/min. Higher densities reached the samples pressed by higher pressures; the specimens with densities higher than 99 % t.d. were prepared within tens of minutes for alumina as well as for zirconia with very low thermal conductivity. Different behavior was observed only for material TZ-3Y, which exhibited core-shell structure with dense surface and porous centre after sintering at heating rates higher than 10 °C/min. It was shown in this work that such behavior was not primarily caused by the high thermal gradient resulting from high heating rates. Its creation was probably caused by chlorine impurities. The mechanism of desintering of these samples was described and eliminated by calcination of the samples at 1000 °C for 10 hours prior to fast sintering at 1500 °C, so even this material could be fast sintered up to 99.9 % theoretical density.
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