Structural refinement of neutron powder diffraction data of two-stage martensitic phase transformations in Ti50.75Ni47.75Fe1.50 shape memory alloy

Transformation behaviors of the technologically important polycrystalline Ti50.75Ni47.75Fe1.50 shape memory alloy were investigated using differential scanning calorimeter (DSC) and powder diffraction techniques. DSC revealed that there are two-stage (i.e., cubic -> trigonal -> monoclinic) martensitic phase transformations on cooling and a one-step transformation (monoclinic -> cubic) on heating. In situ structural refinement of cubic -> trigonal -> monoclinic on cooling was carried out using the D1A high-resolution neutron powder diffractometer at the Institut Laue-Langevin Neutrons for Science in Grenoble, France. Results showed that the phases involved during the phase transition are consistent with the differential scanning calorimeter cooling curve, and the refined crystal structure parameters obtained from Rietveld refinements with the generalized spherical harmonic description agreed reasonably well with X-ray single-crystal data. Subsequently, a combined neutron and synchrotron structural refinement for each phase was conducted because the trial refinements initially using only the synchrotron data of trigonal phase yielded a false minimum with a somewhat high goodness-of-fit chi(2). Results obtained from the combined neutron and synchrotron data of the cubic, trigonal, and monoclinic phases show that the same minimum goodness-of-fit indices were always obtained. (C) 2007 International Centre for Diffraction Data.