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Advanced aluminium alloys prepared by powder metallurgy and spark plasma sintering
Molnárová, Orsolya ; Málek, Přemysl (advisor) ; Haušild, Petr (referee) ; Vojtěch, Dalibor (referee)
Mechanical properties of aluminium alloys highly depend on their phase composition and microstructure. High strength can be achieved among others by introduction of a high volume fraction of fine, homogeneously distributed second phase particles and by a refinement of the grain size. Powder metallurgy allows to prepare fine grained materials with increased solid solubility which are favourable precursors for further precipitation strengthening. Gas atomization was used for the preparation of powders of the commercial Al7075 alloy and its modification containing 1 wt% Zr. A part of gas atomized powders was mechanically milled at different conditions. Mechanical milling reduced the grain size down to the nano-size range and the corresponding microhardness exceeded the value of 300 HV. Powders were consolidated by the spark plasma sintering method to nearly fully dense compacts. Due to a short time and relatively low temperature of sintering the favourable microstructure can be preserved in the bulk material. The grain size of compacts prepared from milled powder was retained in the submicrocrystalline range and the microhardness close to 200 HV exceeded that of the specially heat treated ingot metallurgical counterparts. The prepared compacts retained their fine grained structure and high...
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Microstructure and Texture of Titanium Prepared by Powder Metallurgy
Kozlík, Jiří ; Stráský, Josef (advisor) ; Chráska, Tomáš (referee)
Bulk commercially pure titanium was prepared by powder metallurgy, namely by cryogenic milling and spark plasma sintering, with aim to produce ultra-fine grained material with enhanced strength. The microstructure of milled powders was investigated in detail by a novel method called transmission EBSD, which allowed the first direct observation of texture within the powder particles. This texture is similar to rolling texture, because of the similar nature of the defor- mation during milling. Microstructure observations revealed grains with the size under 100 nm. The influence of sintering parameters on material properties were studied by scan- ning electron microscopy including EBSD, X-ray diffraction and by microhardness measurements. The trade-off relationship between porosity and grain size was identified, fully dense material with ultra-fine grained microstructure could not be produced. Increased oxygen content was identified as a main strengthening factor, while porosity has significant deteriorating effect on mechanical properties. The texture of powder was retained in the bulk material. The possibility of stabilizing the microstructure by mechanical alloying of Ti with yttrium oxide nanoparticles was investigated with mixed results. The stabiliza- tion was successful, but several issues...
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Modification of SPS quasicrystalline compacts via electron beam treatment
Poczklán, Ladislav ; Lukáč,, František (referee) ; Čížek, Jan (advisor)
The quasicrystals are characterized by unusual rotational symmetries that are not observed in the crystalline materials, which is the cause of their interesting material properties. Because of that a particular attention was paid to quasicrystalline structures in the literature research. The research also contains a description of electron beam technology, spark plasma sintering method and introduction to the problematics of wear. As the default materials for the experimental part were selected Titanium Grade 2 powder and Cristome A5 powder which was partially composed of quasicrystalline phase. The first series of samples was sintered only from powder Cristome A5. The second series was sintered from the mixture of 80 % Titanium Grade 2 powder and 20 % Cristome A5 powder. For the compaction of samples spark plasma sintering technology was selected. Samples were then systematically modified by electron beam and subjected to pin on disc tests. Samples modified at 750 °C had the best wear resistance. Samples modified at 1150 °C contained increased amount of quasicrystalline phase.
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High entropy alloys fabricated via SPS compaction of high energy milled feedstock powders
Gubán, Ivan ; Hadraba, Hynek (referee) ; Čížek, Jan (advisor)
The subject of this thesis is preparation of CoCrFeMnNiNx high entropy mixtures via the methods of mechanical alloying and spark plasma sintering (SPS). Three series of specimens were fabricated in this thesis: samples milled in argon (benchmark materials), samples milled in nitrogen atmosphere (to observe their ability of nitrogen absorption) and samples microalloyed with CrN, FeN nitrides (to observe their dissociation into the solid solution potential). The fabricated powders and SPS compacts were subsequently observed by electron microscopy and their phase content by X-Ray diffraction (XRD) and elemental composition by EDS analysis were carried out. A method of reduction melting in inert atmosphere was used to determine the exact oxygen and nitrogen content in powders, while the respective particle size distribution measured by laser diffraction method. The influence of nitrogen content on the hardness of the samples was studied via the microhardness measured. After completing the process of mechanical alloying under the Nitrogen atmosphere was the maximal concentration of nitrogen in the structure 0,208% after 24 hours of milling (dependency on time was linear), which means, the method of milling under the Nitrogen atmosphere was successful. XRD of milled samples showed the existence of the only FCC single solid solution phase, while samples milled under the Nitrogen atmosphere showed the trend of the growth of the lattice parameter with the increasing nitrogen content. There was observed the presence of the chromium nitrides precipitates on the grain boundaries of the FCC phase in microalloyed samples. All specimen were contaminated by a mixture of metallic oxides and manganeese sulphides, which were present in the default manganeese powder. The greatest value of microhardness showed the duplex sample. The increase in values of microhardness (344 HV 0,3) in comparison with the standard sample (262,9 HV 0,3) was recorded on the samples milled under the nitrogen atmosphere, which conforms the positive influence of the nitrogen content on strength characteristics of this alloy.
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Materiály pro fúzní aplikace a jejich interakce s tokamakovým plazmatem
Klevarová, Veronika ; Janeček, Miloš (advisor) ; Šíma, Vladimír (referee)
Title: Materials for fusion applications and their interaction with tokamak plasma Author: Veronika Klevarová Department: Department of Physics of Materials Supervisor: doc. RNDr. Miloš Janeček, CSc., Department of Physics of Materials Abstract: Tungsten represents a perspective option in the context of fusion devices first-wall materials. In the first part of this work, set of tungsten samples with variable grain size was prepared by spark plasma sintering. Specimens were exposed to steady state deuterium plasma beam and high energy heat pulses, simulating thus the normal operation in the tokamak. As a consequence of the exposure, samples surfaces were roughened, as-prepared grains were recovered and in some cases cracks were formed. Moreover, post-irradiation analysis of the damaged samples revealed activation of in-grain slip systems within the loaded surfaces. Threshold grain diameter for this mechanism was determined to be between 5.5 - 6.6 μm at the particular loading conditions. However, damaged features showed to depend more on the fabrication parameters than on the grain diameter. Synergistic effects of simultaneous loading were proven to be important since those reduced the heat propagation within the volume of the tested samples. In the second part of this thesis, introduction to plasma-surface...
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The influence of heating rate on two step sintering of advanced ceramic materials
Klevetová, Tereza ; Maca, Karel (referee) ; Pouchlý, Václav (advisor)
Recently, there has been growing interest in new technologies and procedures to improve the microstructure of advanced ceramic materials. One of the most commonly used sintering methods is Two step sintering (TSS), Rapid rate sintering (RRS) and Spark plasma sintering (SPS). Within the framework of this bachelor thesis number of experiments were carried out for the research of the microstructure interconnecting the Two step sintering with the Rapid rate sintering and non-preassure Spark plasma sintering. The aim of this work was to determine the influence of the heating rate on the size of final relative density and the average grain size for ceramic materials based on ZrO2. The results of the study show that occurrence of the „core-shell“ structure on the ZrO2 doped by 3 mol.% Y2O3 (TZ-3Y) tend to production of non-homogenous microstructure with a fully compacted surface and a porous center. In the case of ZrO2 doped by 8 mol.% Y2O3 (TZ-8Y) this structure was detected only in several cases at higher heating rates. An the same time it was found that the final relative density decreases with increasing heating rate. Using cubic ZrO2 with larger grain size (TZ-8YSB), the „core-shell“ structure did not appear, however a lower relative densities of about 98 % t.d. was always achieved, regardless of the applied temperature profile. The best results were obtained with TZ-8Y using Spark plasma sintering and Rapid rate sintering. Smaller grain size was obtained as compared with conventional methods of other authors. The difference in grain size was just within the framework of the standart deviation. This work doesn’t show any positive influence of Rapid rate sintering on the resulting grain size.
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Advanced ceramic layered materials with heterogeneous microstructure for ballistic applications
Mařák, Vojtěch ; Kachlík, Martin (referee) ; Drdlík, Daniel (advisor)
This bachelor thesis deals with a preparation technology of layered ceramic materials (laminates) with heterogeneous microstructure containing Al2O3 as a matrix with addition of SiC. For the preparation of these materials, dry and wet shaping of ceramic powder with subsequent SPS (Spark Plasma Sintering) was chosen. Due to the goals of the bachelor thesis, the dry shaping proved to be less suitable due to the difficult preparation of the layered structure and the significant wear of the graphitic dies used in the SPS technology. However, the information obtained about mechanical and physical properties has led to the design of the ceramic suspension used in wet shaping (slip-casting). As optimal design 5 vol % of SiC in Al2O3 was chosen. Via this way, ceramic laminates with a sharp layer interface were prepared and the graphitic die wear was minimized. Prepared ceramic samples reached relative density up to 99 % and hardness up to 20.7 GPa. The obtained knowledge has shown the need to optimize the technology of suspension preparation to create ceramic material suitable for ballistic applications.
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High-entropy alloys – bulk alloys and surface treatments
Pišek, David ; Šiška, Filip (referee) ; Hadraba, Hynek (advisor)
Master‘s thesis deals with the preparation and evaluation single-phase high-entropy alloy based on cobalt, chromium, iron, nickel and manganese and its variants strengthened by dispersion of oxidic particles. High-entropy alloy was prepared in powder form by mechanical alloying from the equiatomic proportions of atomic powders. Obtained powder was subsequently compacted by spark plasma sintering. By the method of mechanical alloying were successfully prepared single-phase high-entropy alloy and its variant strengthened by dispersion of nanometric yttria oxides. It has been found that the oxide particles present in the microstructure of high-entropy alloy significantly block mobility of grain boundary and dislocation at elevated temperatures. As a result of this behavior were observed doubling of alloy strength and decreasing of creep rate at 800 °C.
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SPARK PLASMA SINTERING OF BALL MILLED AND ATOMIZED POWDER BASED ON Fe-Al
Šíma, V. ; Minárik, P. ; Chráska, Tomáš
High-quality compacts were prepared using the spark plasma sintering (SPS) method from powders of similar composition Fe-Al-Zr-B. The properties of the sintered compacts are strongly dependent on the morphology and properties of the feedstock powder. The first powder was obtained by ball milling of the as cast alloy and the second was prepared by atomization under argon atmosphere. The morphology and structure of the two powders are compared and mechanical properties and microstructure of compacts prepared under the same conditions of the SPS procedure are discussed. The milled powder has an irregular morphology and shape of the polycrystalline particles, which have a completely disordered BCC structure with considerable internal stresses, high concentration of structural defects and the presence of aluminum oxide. The atomized powder particles are nearly spherical, polycrystalline with ordered B2 structure, with no significant signs of internal stresses and oxidation. Microhardness of particles of both powders was measured and compared with the microhardness of compact materials, the results of compression tests of compacts at room temperature were compared and discussed.
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THE INVESTIGATION OF AN Al7075 ALLOY PREPARED BY SPARK PLASMA SINTERING OF MILLED POWDERS
Molnárová, O. ; Málek, P. ; Nemeth, G. ; Kozlík, J. ; Lukáč, František ; Chráska, Tomáš ; Cinert, Jakub
Atomized powder of an Al7075 alloy was high energy ball milled at room and cryogenic temperatures and compacted by spark plasma sintering (SPS) method. The influence of processing parameters on phase composition and microstructure was studied by X-ray diffraction, light and scanning electron microscopy. The mechanical properties were characterized by microhardness measurements. The atomized powder contained a large volume fraction of intermetallic phases located predominantly in continuous layers separating cells or dendrites in the interior of individual powder particles. Consolidation by SPS destroyed partially this morphology and replaced it by individual particles located at boundaries of original powder particles, at cell boundaries or arranged in chains in previous dendritic regions. High energy milling destroyed most intermetallic particles and enriched the matrix by solute atoms. The high deformation energy introduced into the powder during milling enhanced microhardness up to 220 HV. Consolidation of milled powders by SPS led to the formation of very fine-grained structure with the grain size even below 1 μm and with the fraction of high-angle boundaries about 0.9. Two main types of heterogeneously distributed precipitates were found. The irregularly shaped precipitates with a size about 1 μm seemed to encompass areas with rod like nano-precipitates in most samples. A drop in microhardness to 118HV was observed after SPS, predominantly due to a release of introduced deformation energy.
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