Development of ultra-small-angle X-ray scattering–X-ray photon correlation spectroscopy

This paper describes the development of ultra-small-angle X-ray scattering–X-ray photon correlation spectroscopy (USAXS–XPCS). This technique takes advantage of Bonse–Hart crystal optics and is capable of probing the long-time-scale equilibrium and non-equilibrium dynamics of optically opaque materials with prominent features in a scattering vector range between those of dynamic light scattering and conventional XPCS. Instrumental parameters for optimal coherent-scattering operation are described. Two examples are offered to illustrate the applicability and capability of USAXS–XPCS. The first example concerns the equilibrium dynamics of colloidal dispersions of polystyrene microspheres in glycerol at 10, 15 and 20% volume concentrations. The temporal intensity autocorrelation analysis shows that the relaxation time of the microspheres decays monotonically as the scattering vector increases. The second example concerns the non-equilibrium dynamics of a polymer nanocomposite, for which it is demonstrated that USAXS–XPCS can reveal incipient dynamical changes not observable by other techniques.