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Microstructure of commercially pure titanium after cryogenic milling and spark Plasma sintering
Kozlík, J. ; Harcuba, P. ; Stráský, J. ; Chráska, Tomáš ; Janeček, M.
Commercially pure titanium was prepared by advanced powder metallurgy methods with the aim to produce the ultra-fine grained material. Cryogenic attritor milling was used as a first step to refine the microstructure at liquid argon temperatures to suppress recovery and dynamic recrystallization. Spark plasma sintering was subsequently employed to produce bulk material, exploiting its ability to achieve fully dense structure in short time and thus to reduce the grain growth. In order to understand the undergoing microstructural changes during the process, detailed investigation was performed after each preparation step. Powder morphology was changed significantly after milling, while particle fragmentation was only limited. Grain size after sintering was in micrometer scale, relatively independent of sintering conditions.
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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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Morphology and hardness of particles of titanium powder prepared by cryogenic milling
Ibragimov, Ilya ; Stráský, Josef (advisor) ; Janeček, Miloš (referee)
The effect of cryogenic milling on morphology and microhardness of titanium powder was investigated. Initial powder of commercially pure titanium was subjected to cryogenic milling in liquid argon (LAr) using two different milling speeds. Prepared powders were subsequently cleaned by ethanol. The cleaning procedure was done in two ways: in the air and in the inert atmosphere in the glovebox. Particle size and morphology were investigated my scanning electron microscopy and subsequent automated image analysis. Microhardness of powder particles was determined by Vickers hardness measurement using small loads. The milling did not cause significant powder refiniment, while the shape of powder particles changes substantially. Milling speed affected particle shape and powder contamination. Application of stearic acid as the processing control agent prevented cold-welding of powder particles, but contaminated the powder by oxygen and hydrogen. Stearic acid could be successfully removed by cleaning in ethanol. The using of glovebox for cleaning did not have significant effect on the resultiing contamination.
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