Quantitative measurements of phase transitions in nano- and glassy materials

Novel approaches to the collection and treatment of total x-ray scattering using high energy (> 65 keV) x-ray beams and area detectors allow in situ studies of unprecedented precision to be performed on nano-crystalline (n) and glassy materials at extremes of pressure (p) and temperature (T). Gradual structural transitions in glasses, liquids and nano-materials occurring via continuous changes in density, or involving phases related by pseudo symmetry are inherently difficult to identify due to their disordered nature. In such cases supplementary physical measurements along with modeling of the pair distribution function (PDF) provide powerful constraints on the possible models for the transition. Examples include transitions from n-FeS with a mackinawite-like structure to high p forms with structures related to NiAs structure-type. The distinction between the various high p models – MnP-type, troilite, FeS-III related or mixtures of these phases – is subtle; great care needs to be exercised in refining structure models to fit the observed data. Acoustic techniques are particularly valuable in identifying high p phase transitions in glasses, since measured changes in compressional velocities relate to density changes in the glass while shear waves provide an insight into network rigidity.