The dependence of grain orientation on stress-induced martensitic transformation in superelastic, polycrystalline Nickel-Titanium sheet was examined at the microstructural length scale. Fullfield strains, indicative of transformation extent, were characterized in fields of view of nominally 100 µm x 100 µm using a custom combination of scanning electron microscopy with distortion-corrected digital image correlation. It was found that similarly oriented grains do not necessarily transform similarly, in contrast to a common assumption in mean-field theories. Specifically, grains with similar orientation (as determined by the misorientation of the grain and specimen axes) showed variation in both the mean strain of the grain as well as the range (heterogeneity) of strain across the grain, as determined from surface measurements. Additionally, neither grain size nor degree of misorientation (of common crystal axes from the loading axis) affected the mean strain and strain range.
A combined experimental and analytical study to determine the configurations of transforming martensite during ambient temperature cyclic deformation of superelastic Nickel-Titanium has been conducted. Full-field, sub-grain-size microscale strain measurements were made in situ during cycling using distortion-corrected Digital Image Correlation combined with Scanning Electron Microscopy (SEM-DIC). Using grain orientation maps from Electron Backscatter Diffraction analysis, possible configurations of martensite formed during cyclic deformation were identified by matching the calculated and measured strain fields. This analysis showed that the inclusion of Correspondence Variants (CVs) in addition to Habit Plane Variants (HPVs) of transformed martensite was necessary to provide a robust fit between calculated and measured strain fields. The approach also provided evidence that there was a more rapid accumulation of residual strain in CV regions and that a correlation existed between residual strain accumulation and the loss of actively transforming martensite in later cycles. It was also found that regions of CVs could coexist with untransformed austenite and Habit Plane Variants (HPVs) in individual grains throughout the microstructure, and that these regions of CVs formed before the end of the macroscopic stress plateau. The CV structure that forms during the initial superelastic deformation of Nickel-Titanium plays a critical role in shaping and stabilizing subsequent martensite recovery during cyclic loading.
Nitinol tubes were manufactured from Standard Grade VIM-VAR ingots using Tube Manufacturing method ''TM-1.'' Diamond-shaped samples were laser cut, shape set, then fatigued at 37°C to 10 7 cycles. The 50, 5, and 1% probabilities of fracture were calculated as a function of number of cycles to fracture and compared with probabilities determined for fatigue data published by Robertson et al. (J Mech Behav Biomater 51:119-131, 2015). Robertson tested similar diamonds made from the same standard grade of Nitinol as in the current study, two other standard grades of Nitinol, and two high-purity grades of Nitinol expressly designed to improve fatigue life. Robertson's tubes were manufactured using Tube Manufacturing method ''TM-2.'' Fatigue performance of TM-1 and TM-2 diamonds were compared: At 10 7 cycles, strain amplitudes corresponding to the three probabilities of fracture of the TM-1 diamonds were 2-3 times those of the TM-2 diamonds made from the same grade of Nitinol, and comparable to TM-2 diamonds made from the higherpurity materials. This difference is likely a result of the differences in tube manufacturing techniques and effects on resulting microstructures. Microstructural analyses of samples revealed a correlation between the median probability of fracture and median inclusion diameter that follows an inverse power-law function of the form y & x -1 .
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