Application of in-situ nano-scanning calorimetry and X-ray diffraction to characterize Ni-Ti-Hf high-temperature shape memory alloys

Combinatorial nanocalorimetry and synchrotron X-ray diffraction were combined to study the martensite-austenite (M-A) phase transformation behavior of Ni-Ti-Hf shape memory alloys. A thin-film library of Ni-Ti-Hf samples with a range of compositions was deposited on a parallel nano-scanning calorimeter device using sputter deposition. Crystallization of each amorphous as-deposited sample by local heating at approximately 104 K/s produced a nanoscale grain structure of austenite and martensite. Individual samples were then cycled through the M-A transformation, while the transformation enthalpy was measured by nanocalorimetry and the low- and high-temperature phase compositions were determined by X-ray diffraction. The techniques enable correlation of the observed behavior during thermal cycling with the thermodynamic and structural properties of the samples.