Barrie, Fatmata Haja (2009-12). Effects of Constrained Aging on the Shape Memory Response of Nickel Rich Niti Shape Memory Alloys. Master's Thesis.
Ni50.6Ti49.4 single and Ni52Ti48 polycrystalline shape memory alloy samples were subjected to aging under a uniaxial stress, to form a single Ni4Ti3 precipitate variant and to investigate the effects of single versus multi-variant coherent precipitates on the shape memory characteristics including two-way shape memory effect (TWSME). Shape memory and superelasticity properties along with the effects of stress and temperature on the transformation temperatures, strain, hysteresis, dimensional stability, and R-phase formation were investigated. This was accomplished through the use of isobaric thermal cycling and superelasticity experiments and various microscopy techniques that included transmission electron microscopy (TEM), scanning electron microscopy, and optical microcopy.
The results showed that it is feasible to use constrained aging to bias R-phase martensite variants upon cooling from austenite without any external stress, however, accomplishing this with B19'martensite was much harder as complete TWSME was only found in the Ni50.6Ti49.4 single crystalline sample oriented along the  direction. The onset of irrecoverable strain corresponded to the R-phase temperature hysteresis increase in the single crystalline samples regardless of the aging conditions. Through TEM analysis it was discovered that  and  twins were found in austenite due to plastic deformation of martensite during the superelasticity experiments. Since  twins are theoretically impossible to form in austenite, and since martensite was plastically deformed,  austenite twins were attributed to the transformation of compound twins in martensite, in particular  martensite twins formed during the plastic deformation of martensite, into austenite twins.
In the Ni52Ti48 polycrystalline samples, a compressive R-phase variant was biased through constrained aging under 100 and 200 MPa uniaxial tensile stresses at 400?C and 450?C. Aging, in all conditions, produced a high density of Ni4Ti3 precipitates that was most likely responsible for the small transformation strain observed, less that 2%, upon transformation to martensite.
In the future, samples with compositions between 50.8 and 51.5 Ni atomic percent, in addition to altered solution and aging heat treatments as compared to those used in this study should be investigated as it is believed that samples with these compositions will yield better and consistent TWSME responses through constrained aging.