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Background: Stereo-digital image correlation (DIC) measurements can be challenging when working with small specimens. Achieving high-precision data requires careful selection of hardware, stereo-rig design, illumination, speckling, calibration, and minimization of noise levels. Objective: This study presents an optimized stereo-DIC setup based on parfocal zoom lenses for full-field measurements at magnifications ranging from 0.5× (14.3 × 16.9 mm2) to 2× (3.5 × 4.2 mm2). Methods: The advantages of using parfocal zoom lenses over fixed-focal-length lenses (and extension tubes) for full-field measurements at small fields of view (FOVs) are demonstrated through quantitative comparisons of the temporal evolution of pseudo-strains and null strain analysis from rigid body translation experiments. The optimal speckling parameters for each magnification are determined by analyzing gray-level histograms, mean intensity gradient ( ∇ G ¯ ), and subset size. The challenges of calibration at high magnifications are discussed, along with strategies for obtaining acceptable results. Results: The accuracy of the presented stereo-DIC setup is evaluated through the study of localized phase transformation on a 1 mm diameter superelastic NiTi wire under tension, column buckling, and compression deformations. The presented setup provides highly consistent full-field data over the 0.5–2× magnification range. Conclusion: The results highlight the benefits of using parfocal zoom lenses for stereo-DIC measurements over a range of small FOVs. [ABSTRACT FROM AUTHOR]

In the present work we explain the concentration dependence of the martensite start temperature ( M S ) in Ni–Ti-based shape memory alloys (SMAs). We briefly review the present level of understanding and show that there is a need for further work. We then investigate the strong dependence of M S on alloy composition in binary Ni–Ti, ternary Ni–Ti–X (X = Cr, Cu, Hf, Pd, V, Zr) and quaternary Ni–Ti–Cu–Y (Y = Co, Pd) SMAs. For binary Ni–Ti, we combine differential scanning calorimetry experiments with insight gained through the application of the density functional theory (DFT) to show that heats of transformation Δ H decrease as Ni concentrations increase from 50.0 to 51.2 at.%. This causes a shift in the Gibbs free energy curves of austenite G A ( T ) and martensite G M ( T ), which in turn results in a lower M S temperature. Our DFT results suggest that the strong decrease of Δ H is caused by a stabilization of the B2 phase by structural relaxations around Ni antisite atoms, together with a gradual destabilization of B19′. The martensite start temperatures and the latent heats of transformation for binary, ternary and quaternary Ni–Ti-based SMAs are closely related. We observe smaller latent heats when the geometrical differences between the crystal structures of austenite and martensite decrease. [ABSTRACT FROM AUTHOR]

Abstract: Nb occupancy in the austenite B2-NiTi matrix and Ti2Ni phase in Ni–Ti–Nb shape memory alloys was investigated by aberration-corrected scanning transmission electron microscopy and precession electron diffraction. In both cases, Nb atoms were found to prefer to occupy the Ti rather than Ni sites. A projector augmented wave method within density functional theory was used to calculate the atomic and electronic structures of the austenitic B2-NiTi matrix phase and the Ti2Ni precipitates both with and without addition of Nb. The obtained formation energies and analysis of structural and electronic characteristics explain the preference for Ti sites for Nb over Ni sites. [Copyright &y& Elsevier]

In the present work, a computer-controlled test rig for simultaneous fatigue testing of several pseudoelastic NiTi wires through bending rotation is described. Bending rotation fatigue (BRF) testing represents a displacement-controlled experiment where a straight wire is bent into a semi-circle und forced to rotate around its axis. Thus, each point on the wire surface is subjected to alternating tension and compression. A test rig, which allows to control loading amplitudes, rotation frequencies and temperatures is described. We report preliminary results of an experimental program, which aims for a better understanding of fatigue lives, crack initiation, and crack growth in pseudoelastic NiTi wires. It was found that a good surface quality is of utmost importance to avoid early crack initiation. Wöhler curves of pseudoelastic NiTi wires typically show two different regimes depending on the maximum imposed surface strain during bending rotation fatigue testing. Larger strain amplitudes, which are associated with macroscopic formation of stress-induced martensite, result in relatively low fatigue lives (LCF regime). In contrast, cycle numbers exceeding 107 were obtained for strain amplitudes where no large scale stress-induced formation of martensite occurred (HCF regime). [ABSTRACT FROM AUTHOR]

Abstract: In the present work we show how different oxygen (O) and carbon (C) levels affect fatigue lives of pseudoelastic NiTi shape memory alloys. We compare three alloys, one with an ultrahigh purity and two which contain the maximum accepted levels of C and O. We use bending rotation fatigue (up to cycle numbers >108) and scanning electron microscopy (for investigating microstructural details of crack initiation and growth) to study fatigue behavior. High cycle fatigue (HCF) life is governed by the number of cycles required for crack initiation. In the low cycle fatigue (LCF) regime, the high-purity alloy outperforms the materials with higher number densities of carbides and oxides. In the HCF regime, on the other hand, the high-purity and C-containing alloys show higher fatigue lives than the alloy with oxide particles. There is high experimental scatter in the HCF regime where fatigue cracks preferentially nucleate at particle/void assemblies (PVAs) which form during processing. Cyclic crack growth follows the Paris law and does not depend on impurity levels. The results presented in the present work contribute to a better understanding of structural fatigue of pseudoelastic NiTi shape memory alloys. [Copyright &y& Elsevier]

Abstract: High-precision data on phase transformation temperatures in NiTi, including numerical expressions for the effect of Ni on M S, M F, A S, A F and T 0, are obtained, and the reasons for the large experimental scatter observed in previous studies are discussed. Clear experimental evidence is provided confirming the predictions of Tang et al. 1999 regarding deviations from a linear relation between the thermodynamic equilibrium temperature and Ni concentration. In addition to affecting the phase transition temperatures, increasing Ni contents are found to decrease the width of thermal hysteresis and the heat of transformation. These findings are rationalized on the basis of the crystallographic data of Prokoshkin et al. 2004 and the theory of Ball and James . The results show that it is important to document carefully the details of the arc-melting procedure used to make shape memory alloys and that, if the effects of processing are properly accounted for, precise values for the Ni concentration of the NiTi matrix can be obtained. [Copyright &y& Elsevier]

Abstract: The Ti3.87Ni1.73Fe0.7O0.3, Ti3.87Ni1.73Fe0.4N0.3 and Ti3.87Ni1.73Fe0.4C0.3 alloys were investigated regarding their surface characteristics. The scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectroscopy (EDS) was used for phase characterization. The X-ray photoelectron spectroscopy (XPS) was used to analyze the chemical composition of alloy surface. The atomic force microscopy (AFM) to observe alloy surface topography after cutting and electrochemical polishing separately has been done. The transmission electron microscopy (TEM) with X-ray diffraction was carried out to get a high contrast images and the diffraction pattern from alloy surface. The results clearly shown, that all alloys were multiphase, and their surface was totally oxidized with no pure metals. [Copyright &y& Elsevier]

Abstract: An ultrafine-grained pseudoelastic NiTi shape-memory alloy wire with 50.9at.% Ni was examined using synchrotron X-ray diffraction during in situ uniaxial tensile loading (up to 1GPa) and unloading. Both macroscopic stress–strain measurements and volume-averaged lattice strains are reported and discussed. The loading behavior is described in terms of elasto-plastic deformation of austenite, emergence of R phase, stress-induced martensitic transformation, and elasto-plastic deformation, grain reorientation and detwinning of martensite. The unloading behavior is described in terms of stress relaxation and reverse plasticity of martensite, reverse transformation of martensite to austenite due to stress relaxation, and stress relaxation of austenite. Microscopically, lattice strains in various crystallographic directions in the austenitic B2, martensitic R, and martensitic B19′ phases are examined during loading and unloading. It is shown that the phase transformation occurs in a localized manner along the gage length at the plateau stress. Phase volume fractions and lattice strains in various crystallographic reflections in the austenite and martensite phases are examined over two transition regions between austenite and martensite, which have a width on the order of the wire diameter. Anisotropic effects observed in various crystallographic reflections of the austenitic phase are also discussed. The results contribute to a better understanding of the tensile loading behavior, both macroscopically and microscopically, of NiTi shape-memory alloys. [Copyright &y& Elsevier]

High entropy shape memory alloys (HE-SMAs) show reversible martensitic phase transformations at elevated temperatures. HE-SMAs were derived from binary NiTi, to which the elements Cu, Pd, Zr and Hf are added. They represent ordered complex solid solutions. Their high temperature phase is of B2 type, where the added elements occupy sites in the Ni-(Cu, Pd) and Ti-sub-lattices (Zr, Hf). In the present study, advanced microstructural and thermal characterization methods were used to study the effects of the additional alloy elements on microstructures and phase transformations. The ratios of Ni-equivalent (Ni, Cu, Pd) and Ti-equivalent (Ti, Zr, Hf) elements in HE-SMAs were varied to establish systems that correspond to stoichiometric, under- and over-stoichiometric binary alloys. It is shown that basic microstructural features of cast and heat-treated HE-SMAs are inherited from the nine binary X–Y subsystems (X: Ni, Cu, Pd; Y: Ti, Zr, Hf). The phase transition temperatures that characterize the martensitic forward and reverse transformations depend on the concentrations of all alloy elements. The data obtained demonstrate how martensite start temperatures are affected by deviations from the composition of an ideal stoichiometric B2 phase. The findings are discussed in the light of previous work on the concentration dependence of SMA transformation temperatures, and directions for the development of new shape memory alloy compositions are proposed. • Effects of deviations from ideal stoichiometry on microstructures and martensitic transformations are studied. • Detailed microstructural, chemical and crystallographic data are presented. • Strategies and relevant factors for the interpretation of microstructures in chemically complex SMAs are discussed. • The dependence of martensite start temperatures on compositions of chemically complex shape memory alloys is analyzed. • New directions for the development of shape memory alloys are proposed. [ABSTRACT FROM AUTHOR]

To reveal mechanisms of martensite stabilization by prestrain in shape memory alloys, details of reverse martensitic transformation (MT) in prestrained Ni 45 Ti 46 Nb 9 alloy were studied using calorimetry, dilatometry and resistivity. The first reverse MT is burst-like and is shifted to higher temperatures by ~120 K as compared to the nominal MT. During thermal cycling approaching the first reverse MT, stabilized martensite shows "forbidden" behaviours like burst-like reverse MT not during heating, but during cooling and under isothermal conditions. These unusual effects are attributed to non-thermoelastic nature of the first reverse MT in stabilized martensite under high chemical driving force. Image, graphical abstract [ABSTRACT FROM AUTHOR]

Martensitic Ni 50 Ti 50 wires and sheets with different textures were tensile tested in the temperature range between −100 °C and 60 °C. The effect of texture and temperature on reorientation of martensite variants was investigated. After deformation, all material states were heated into the austenite regime to study their shape memory behavior. During room temperature tensile testing, in-situ digital image correlation revealed that the reorientation of martensite variants is associated with the nucleation and propagation of a macroscopic Lüders band. A comparison between the mechanical data obtained for wire and sheet specimens revealed a strong effect of texture. The plateau stresses of sheets were found to be 25–33% larger and their recoverable strains were 30% lower than for wires. However, the product of plateau stress and recoverable strain, which represents the external work per unit volume required for martensite variants reorientation does not depend on texture. The tensile tests performed at different temperatures revealed that in the temperature range considered the recoverable strain does not depend significantly on temperature. In contrast, the plateau stress as well as the external work required to reorient martensite decrease with increasing testing temperature. We use a thermodynamic approach involving the elastic strain energy associated with the growth of reoriented martensite variants to rationalize these temperature dependencies. [ABSTRACT FROM AUTHOR]

Abstract: Crack extension in pseudoelastic binary NiTi shape memory alloy (SMA) compact tension (CT) specimens was examined during static loading. The material composition of 50.7at.% Ni (austenitic, pseudoelastic) was investigated using high-energy synchrotron X-ray diffraction. A miniature CT specimen was developed, which is small enough to allow in situ testing in a synchrotron beam line to identify phases, textures and lattice strains in front of a crack tip. Stress-induced martensite in pseudoelastic NiTi SMAs was mapped in front of the crack of a CT specimen during static loading using synchrotron radiation. The phase volume fraction and lattice microstrain results are discussed and compared with results from thermographic measurements. The Poisson effect is observed by comparing the lattice strains in the loading direction and transverse to the loading direction. [Copyright &y& Elsevier]

Abstract: Nickel–Titanium shape memory alloys (NiTi-SMA) are of biomedical interest due to their unusual range of pure elastic deformability and their elastic modulus, which is closer to that of bone than any other metallic or ceramic material. Newly developed porous NiTi, produced by Selective Laser Melting (SLM), is currently under investigation as a potential carrier material for human mesenchymal stem cells (hMSC). SLM enables the production of highly complex and tailor-made implants for patients on the basis of CT data. Such implants could be used for the reconstruction of the skull, face, or pelvis. hMSC are a promising cell type for regenerative medicine and tissue engineering due to their ability to support the regeneration of critical size bone defects. Loading porous SLM-NiTi implants with autologous hMSC may enhance bone growth and healing for critical bone defects. The purpose of this study was to assess whether porous SLM-NiTi is a suitable carrier for hMSC. Specimens of varying porosity and surface structure were fabricated via SLM. hMSC were cultured for 8days on NiTi specimens, and cell viability was analyzed using two-color fluorescence staining. Viable cells were detected on all specimens after 8days of cell culture. Cell morphology and surface topography were analyzed by scanning electron microscopy (SEM). Cell morphology and surface topology were dependent on the orientation of the specimens during SLM production. The Nickel ion release can be reduced significantly by aligned laser processing conditions. The presented results clearly attest that both dense SLM-NiTi and porous SLM-NiTi are suitable carriers for hMSC. Nevertheless, before carrying out in vivo studies, some work on optimization of the manufacturing process and post-processing is required. [Copyright &y& Elsevier]

Abstract: Thermal cycling of NiTi shape memory alloys is associated with functional fatigue: the characteristic phase transformation temperatures decrease with increasing number of cycles, and the transformation behavior changes from a single- to a two-stage martensitic transformation involving the intermediate R-phase. These effects are usually attributed to a gradual increase of dislocation density associated with micro-plasticity during repeated cycling through the transformation range. Here, these changes are shown to increase at a higher maximum temperature (in the fully austenitic state) during differential scanning calorimetric cycling of a Ni-rich alloy. Additional thermal cycling experiments without repeated phase transformations, and post-mortem microstructural observations by transmission electron microscopy, demonstrate that a relevant portion of functional fatigue is due to the formation of nano-scale Ni-rich precipitates of type Ni4Ti3 even at temperatures relatively close to the austenite finish temperature. These results show that both dislocation generation during the diffusion-less phase transformation, and diffusion-controlled nucleation and growth of Ni4Ti3 precipitates, can interact and contribute to the evolution of functional properties during thermal cycling of Ni-rich NiTi. [Copyright &y& Elsevier]

Abstract: Crack extension under static loading in pseudoplastic and pseudoelastic binary NiTi shape memory alloy (SMA) compact tension (CT) specimens was examined. Two material compositions of 50.3at.% Ni (martensitic/pseudoplastic) and 50.7at.% Ni (austenitic/pseudoelastic) were investigated. The SMAs were characterized using differential scanning calorimetry to identify the phase transformation temperatures and tensile testing to characterize the stress–strain behavior. A miniature CT specimen was developed, which yields reliable critical fracture mechanics parameters. At 295K, cracks propagate at similar stress intensities of into martensite and pseudoelastic austenite. Integrating the miniature CT specimen into a small test device which can be fitted into a scanning electron microscope shows that this is due to cracks propagating into regions of detwinned martensite in both materials. Investigating a pseudoelastic miniature CT specimen in a synchrotron beam proves that martensite forms in front of the crack in the center of the CT specimen, i.e. under plane strain conditions. [Copyright &y& Elsevier]