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AN INTERPLAY BETWEEN HEAT TREATMENT CONDITIONS AND B2 <-> B19 ' TRANSFORMATION IN Ni-Ti SHAPE MEMORY ALLOYS
Kuběnová, Monika ; Zálešák, Jakub ; Čermák, Jiří ; Dlouhý, Antonín
This study investigates the influence of a heat treatment atmosphere on multistage martensitic transformations in a Ti-50.9at% Ni shape memory alloy. Evacuated quartz tubes were filled with hydrogen while the hydrogen partial pressure was carefully controlled in each experiment. The encapsulated specimens were subjected to heat treatments consisting of annealing and aging. After the heat treatment, the path of martensitic transformation was investigated using differential scanning calorimetry (DSC). On cooling, martensite initial temperatures decrease with the increasing partial pressure of hydrogen applied during the heat treatment. Moreover, the formation of martensite phase may not take place for partial pressures that exceed a certain limit. On the other hand, two-and multiple-step B2/R/B19' martensitic transformations are observed in specimens heat treated at lower hydrogen pressures. Results obtained using transmission electron microscopy (TEM) clearly show that the size of Ni4Ti3 precipitates becomes smaller in alloys that were heat treated at higher hydrogen pressures. The results are discussed in terms of a chain of events. It is suggested that diffusion of hydrogen into the specimen during the annealing step first influences the nucleation of the Ni4Ti3 phase. The sizes and distribution of the Ni4Ti3 precipitates than control the characteristics of B2/B19' transformation.
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Analytical electron microscopy of lead-free nanopowder solders
Buršík, Jiří ; Sopoušek, J. ; Zálešák, Jakub ; Buršíková, V.
During the last decade, the EU legislative regulations enforced lead-free solders and hence initiated an extensive search for the best replacement of lead-containing solders. Parallel to new binary and ternary bulk solders, metal nanoparticles are also considered as potential candidates for solder materials. It is known that physical, electric and thermodynamic properties of nanoobjects are significantly different from those of the bulk materials. The oxidation, high reactivity of the surfaces and aggregation are frequent problems of nanotechnology applications. The nanoparticles of pure metals and alloys exhibit the depression of the melting point compared to bulk material, hence they are able to aggregate and to form firm interlayer joints at low temperatures. Exploiting this effect can save energy, work and materials.
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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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