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INFLUENCE OF MELTING TEMPERATURE AND TIME ON THE OXYGEN CONTENT IN TiAlNb ALLOYS
Barták, Tomáš ; Zemčík, L. ; Dlouhý, Antonín
The present study investigates a cost-effective melting of TiAlNb intermetallics in a stable yttrium oxide refractory. We identify mechanisms that mainly contribute to the oxygen pick-up during melting. Systematic microstructural and chemical analysis provided evidence that erosion and dissolution of crucible wall are key factors of the process. Experiments were performed using two Ti46Al7Nb alloys with a different initial content of oxygen. The alloys were re-melted in vacuum induction furnace inside U-shaped yttria crucibles. The experiments involved three different temperatures in combination with melting times spanning from 300 to 1800 s. The oxygen content of re-melted and solidified alloys was assessed by means of inert gas fusion technique. Results of the chemical analysis provided clear evidence that the stability of the refractory wall in contact with the molten alloy and its rate of dissolution depend mainly on melting temperature. These results are further supported by microstructural observations that confirmed ever growing content of ceramic phases in the solidified intermetallic with increasing temperature of the melt. The work also contributed to the improved experimental methodology, in particular to temperature measurements of reactive melts.
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Impact of Heat Treatment Environment of Microstructure and Transformation Path in NiTi Shape Memory Alloy
Kuběnová, Monika ; Zálešák, Jakub ; Čermák, Jiří ; Barták, Tomáš ; Dlouhý, Antonín
We report results of differential scanning calorimetry (DSC) experiments in which heat flow (T) from and to Ti-50.9at%Ni shape memory samples was recorded during the temperature scan through a B2 B19’ transformation range. Prior to the DSC experiments, the samples were separately annealed in evacuated quartz capsules containing different hydrogen and helium mixtures with an overall filling pressure of 900 mbar. The quartz tubes containing the annealed samples were subsequently quenched into cold water. After quenching, the capsules were opened, martensitic transformations were investigated by DSC and the microstructure of the samples was assessed by transmission electron microscopy (TEM). Annealing in the mixtures with an increasing partial pressure of hydrogen led to a considerable drop in the latent heat associated with the B2 B19’ martensitic transformation. Results obtained using TEM suggest that hydrogen may function as a catalytic substance that accelerates the long range ordering of Ni atoms in early stages of Ni4Ti3-phase precipitation. The selected area diffraction study focused on patterns in <100>B2 and <110>B2 zones and provided evidence for diffuse scattering due to spatial modulations of the lattice constant. These variations in the background electron intensities might be related to a precursor of Ni4Ti3 phase in its early state of formation.
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Influence of Heat Treatment on Microstructure and Transformation Characteristics of NiTi Shape Memory Wires
Zálešák, Jakub ; Kuběnová, Monika ; Čermák, Jiří ; Svoboda, Milan ; Dlouhý, Antonín
The present study shows how heat treatments affect microstructure and transformation behaviour of superelastic Ni-rich NiTi shape memory wires. Wire samples were sealed into quartz tubes, filled with hydrogen reduction atmosphere, heated for 10 minutes at temperatures increasing in a range from 500 to 600°C and subsequently quenched into cold water. Characteristic transformation temperatures MS, MF, AS, AF, thermal hysteresis and latent heats were investigated using differential scanning calorimetry (DSC). We observed significant changes in DSC charts which recorded B2 → R and R → B19‘ phase martensitic transformations. Increasing temperature of the heat treatment resulted in a convergence of the two transformation peaks. R-transformation commenced at systematically lower temperatures and the beginning of the B19‘ transformation was shifted to higher temperatures with increasing temperature of the heat treatment. In parallel, latent heat of the overall B2 → B19‘ transformation clearly increases. We rationalize these significant changes in the transformation behaviour on the basis of the microstructural development during the heat treatment which is characterized by means of SEM, TEM and EBSD techniques.
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