Alloy NiTi with nearequiatomic composition of nickel and titan belongs to a group of metal materials with a shape memory effect (Shape memory alloys). NiTi alloys are a guite attractive materials not only as practical shape memory alloys with hight strenght and ductility but also as those exhibiting unique physical properties. The production of these matrerials is complying with chemical composition. Final charakteristics of alloy are influenced by these bounderies and also by mechanical-heat treatment. This work deal with DSC evaluation of homogenity of ingot structure of NiTi alloy containing 50,8 at.% Ni. The alloy was melted in Y2O3 cricible. In the end the results of DSC method are compared to the microstructure of alloy obtained by SEM and TEM methods.

Thesis (M.Sc. (Physics)) -- University of Limpopo, 2021 / First-principles density functional theory has been used to study the stabilities of binary TiPt, TiTa, TiNi and TiCo potential shape memory alloys. Furthermore, ternary alloys Ti50Pt50-xMx with V, Ta, Hf and quaternary Ti50(PtCo)50-xTax systems were also investigated. The structural, electronic and mechanical properties were deduced to mimic the stabilities of these alloys. Furthermore, their vibrational stability, x-ray diffraction and temperature dependence have been examined. The structures were subjected to full geometry optimization to obtain equilibrium lattice constants. It was found that the equilibrium lattice parameters for all the binary systems are in good agreement with experimental results to within 5%. The heats of formation (ΔHf) were calculated to determine the thermodynamic stability of the B2 TiM systems. It was revealed that TiPt is the most energetically favourable (most stable) whereas TiTa is the least favourable due to high ΔHf value (less stable). In addition, electronic properties suggest that TiPt, TiNi and TiCo systems are stable with TiTa being the least favourable consistent with the ΔHf. The elastic properties were also calculated to mimic the mechanical stability of these alloys. TiNi, TiCo and TiTa were found to be mechanical stable whereas TiPt is unstable. This behaviour is consistent with the phonon dispersion curves for TiPt and TiCo. TiCo structure, in particular is the most stable in line with the predicted phonon dispersion. The effect of alloying on Ti50Pt50-xMx (M = V, Ta, Hf) ternary system was carried out using the supercell approach. It was observed that the lattice parameters decrease minimally with an increase in V and increases with an increase in Ta and Hf content. The structures ii become thermodynamically less stable with an increase in V, Ta and Hf content, as depicted by heats of formation. The shear modulus (C′) of Ti50Pt50-xMx increases with an increase in M (V, Ta and Hf) concentration suggesting mechanical stability of these alloys. This has been confirmed from the phonon curves where the phonon soft modes are reduced and tend to disappear with increasing content of the alloying elements. Thus the results suggest that the V, Ta and Hf addition reduces the transformation temperatures of the TiPt alloy as indicated by its higher shear modulus C′. Furthermore, it was observed that the lattice parameters of the quaternary system decrease with an increase in Ta content in the system. Thus ΔHf of the B2 and B19 Ti50Pt43.75-xCo6.25Tax and B19 Ti50Pt31.25-xCo18.75Tax alloy system showed that the 6.25 at.% Ta addition is energetically most favourable (ΔHf<0). The DOS behaviour confirms that the 6.25 at.% Ta as least favourable whereas for B19, the 6.25 at.% Ta is most favourable. The elastic constants for B19 and B2 show the positive shear modulus (mechanical stability). Moreover, the phonon dispersions and phonon density of states for the B2 and B19 Ti50Pt43.75-xCo6.25Tax and Ti50Pt31.25-xCo18.75Tax were calculated and are consistent with the elastic constant. The LAMMPS code was employed to investigate the temperature dependence of the B19 Ti50Pt43.75-xCo6.25Tax and Ti50Pt31.25-xCo18.75Tax structures. The martensitic to austenite transformation temperature decreases with an increase in Ta concentration. Temperature variations of the XRD patterns for the B19 are in reasonable agreement with predicted lattice parameters. / National Research Foundation (NRF) and Titanium centre of competence (TiCoC)

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The goal of this study is to investigate the microstructure and microstructure-based fatigue (MSF) model of additively-manufactured (AM) metallic materials. Several challenges associated with different metals produced through additive manufacturing (Laser Enhanced Net Shaping – LENS®) have been addressed experimentally and numerically. Significant research efforts are focused on optimizing the process parameters for AM manufacturing; however, achieving a homogenous, defectree AM product immediately after its fabrication without postabrication processing has not been fully established yet. Thus, in order to adopt AM materials for applications, a thorough understanding of the impact of AM process parameters on the mechanical behavior of AM parts based on their resultant microstructure is required. Therefore, experiments in this study elucidate the effects of process parameters – i.e. laser power, traverse speed and powder feed rate – on the microstructural characteristics and mechanical properties of AM specimens. A majority of fatigue data in the literature are on rotation/bending test of wrought specimens; however, few studies examined the fatigue behavior of AM specimens. So, investigating the fatigue resistance and failure mechanism of AM specimens fabricated via LENS® is crucial. Finally, a microstructure-based MultiStage Fatigue (MSF) model for AM specimens is proposed. For calibration of the model, fatigue experiments were exploited to determine structure-property relations for an AM alloy. Additional modifications to the microstructurally-based MSF Model were implemented based on microstructural analysis of the fracture surfaces – e.g. grain misorientation and grain orientation angles were added to the MSF code.

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In NiTi, a reversible thermoelastic martensitic transformation can be induced by temperature or stress between a cubic (B2) austenite phase and a monoclinic (B19') martensite phase. Ni-rich binary compositions are cubic at room temperature (requiring stress or cooling to transform to the monoclinic phase), while Ti-rich binary compositions are monoclinic at room temperature (requiring heating to transform to the cubic phase). The stress induced transformation results in the superelastic effect, while the thermally induced transformation is associated with strain recovery that results in the shape memory effect. Ternary elemental additions such as Fe can additionally introduce an intermediate rhombohedral (R) phase between the cubic and monoclinic phase transformation. This work was initiated with the broad objective of connecting the macroscopic behavior in shape memory alloys with microstructural observations from transmission electron microscopy (TEM). Specifically, the goals were to examine (i) the effect of mechanical cycling and plastic deformation in superelastic NiTi; (ii) the effect of thermal cycling during loading in shape memory NiTi; (iii) the distribution of twins in martensitic NiTi-TiC composites; and (iv) the R-phase in NiTiFe. Both in situ and ex situ lift out focused ion beam (FIB) and electropolishing techniques were employed to fabricate shape memory alloy samples for TEM characterization. The Ni rich NiTi samples were fully austenitic in the undeformed state. The introduction of plastic deformation (8% and 14% in the samples investigated) resulted in the stabilization of martensite in the unloaded state. An interlaying morphology of the austenite and martensite was observed and the martensite needles tended to orient themselves in preferred orientations. The aforementioned observations were more noticeable in mechanically cycled samples. The observed dislocations in mechanically cycled samples appear to be shielded from the external applied stress via mismatch accommodation since they are not associated with unrecoverable strain after a load-unload cycle. On application of stress, the austenite transforms to martensite and is expected to accommodate the stress and strain mismatch through preferential transformation, variant selection, reorientation and coalescence. The stabilized martensite (i.e., martensite that exists in the unloaded state) is expected to accommodate the mismatch through variant reorientation and coalescence. On thermally cycling a martensitic NiTi sample under load through the phase transformation, significant variant coalescence, variant reorientation and preferred variant selection was observed. This was attributed to the internal stresses generated as a result of the thermal cycling. A martensitic NiTi-TiC composite was also characterized and the interface between the matrix and the inclusion was free of twins while significant twins were observed at a distance away from the matrix-inclusion interface. Incorporating a cold stage, diffraction patterns from NiTiFe samples were obtained at temperatures as low as -160ºC. Overall, this work provided insight in to deformation phenomena in shape memory materials that have implications for engineering applications (e.g., cyclic performance of actuators, engineering life of superelastic components, stiffer shape memory composites and low-hysteresis R-phase based actuators). This work was supported in part by an NSF CAREER award (DMR 0239512).

This work reports on the design, fabrication and testing of a thermal switch wherein the open and closed states are actuated by shape memory alloy elements while heat is transferred by a heat-pipe. The motivation for such a switch comes from NASA's need for thermal management in advanced spaceport applications associated with future lunar and Mars missions. For example, as the temperature can approximately vary between 40 K to 400 K during lunar day/night cycles, such a switch can reject heat from a cryogen tank in to space during the night cycle while providing thermal isolation during the day cycle. By utilizing shape memory alloy elements in the thermal switch, the need for complicated sensors and active control systems are eliminated while offering superior thermal isolation in the open state. Nickel-Titanium-Iron (Ni-Ti-Fe) shape memory springs are used as the sensing and actuating elements. Iron (Fe) lowers the phase transformation temperatures to cryogenic regimes of operation while introducing an intermediate, low hysteretic, trigonal R-phase in addition to the usual cubic and monoclinic phases typically observed in binary NiTi. The R-phase to cubic phase transformation is used in this application. The methodology of shape memory spring design and fabrication from wire including shape setting is described. Heat transfer is accomplished via heat acquisition, transport and rejection in a variable length heat pipe with pentane and R-134a as working fluids. The approach used to design the shape memory elements, quantify the heat transfer at both ends of the heat pipe and the pressures and stresses associated with the actuation are outlined. Testing of the switch is accomplished in a vacuum bell jar with instrumentation feedthroughs using valves to control the flow of liquid nitrogen and heaters to simulate the temperature changes. Various iv performance parameters are measured and reported under both transient and steady-state conditions. Funding from NASA Kennedy Space Center for this work is gratefully acknowledged.

Shape memory and superelastic applications of NiTi based alloys have typically been limited to near room temperature or to bulk length scales. The objective of this work is two-fold: first, to investigate shape memory behavior at low temperatures in the context of the R-phase transformation in NiTiFe alloys by recourse to arc-melting, differential scanning calorimetry (DSC), transmission electron microscopy (TEM) and mechanical testing at low temperatures; and second, to investigate superelasticity and two-way shape memory behavior at reduced length scales in the context of NiTi by recourse to micro-compression, micro-indentation and TEM studies. Selected compositions of ternary NiTiFe shape memory alloys were arc-melted and thermomechanically processed to investigate the influence of composition and processing parameters on the formation of the R-phase. The methodology used for the processing and characterization of the alloys was established and included microprobe analysis, DSC, TEM and mechanical testing. No phase transformation was observed in alloys with Fe content in excess of 4 at.%. Thermomechanical treatments facilitated the formation of the R-phase in Ni-rich alloys. The range of the transformation between the R-phase and austenite, and the hysteresis associated with it were influenced by the distribution and size of metastable Ni4Ti3 precipitates. The investigation of the microstructural, thermal and mechanical properties of the R-phase transformation in NiTiFe alloys revealed a complex dependence of these properties on processing parameters. The present work also highlighted the hitherto unexplored competition between the two inelastic deformation modes operating in the R-phase (detwinning and stress-induced transformation) and established the preference of one mode over the other in stress-temperature space. iv The complete micromechanical response of superelastic NiTi was examined by performing careful micro-compression experiments on single crystal pillars of known orientations using a nanoindenter tip. Specifically, the orientation dependence of the elastic deformation of austenite, the onset of its transformation to martensite, the gradient and the hysteresis in the stress-strain response during transformation, the elastic modulus of the stress-induced martensite and the onset of plasticity of the stress-induced martensite were analyzed in separate experiments. A majority of the results were explained by recourse to a quantitative determination of strains associated with austenite grains transforming to martensite variants or twinning in martensite. Microstructural studies were also performed on a micro-indentation trained NiTi shape memory alloy specimen to understand the mechanisms governing the two-way shape memory effect. In situ TEM studies at temperature on specimens obtained at different depths below the indent showed the presence of retained martensite along with the R-phase. Previously, while such twoway shape memory behavior has typically been associated with large dislocation densities, this work provides evidence of the role of retained martensite and the R-phase in cases with reduced dislocation densities. Funding support for this work from NSF (CAREER DMR-0239512), NASA (NAG3-2751) and SRI is acknowledged.