Simultaneous birefringence, small- and wide-angle X-ray scattering to detect precursors and characterize morphology...

An experimental configuration that combines the powerful capabilities of a short-term shearing apparatus with simultaneous optical and X-ray scattering techniques is demonstrated, connecting the earliest events that occur during shear-induced crystallization of a polymer melt with the subsequent kinetics and morphology development. Oriented precursors are at the heart of the great effects that flow can produce on polymer crystallization (strongly enhanced kinetics and formation of highly oriented crystallites), and their creation is highly dependent on material properties and the level of stress applied. The sensitivity of rheo-optics enables the detection of these dilute shear-induced precursors as they form during flow, before X-ray techniques are able to reveal them. Then, as crystallization occurs from these precursors, X-ray scattering allows detailed quantification of the characteristics and kinetics of growth of the crystallites nucleated by the flow-induced precursors. This simultaneous combination of techniques allows unambiguous correlation between the early events that occur during shear and the evolution of crystallization after flow has stopped, eliminating uncertainties that result from the extreme sensitivity of flow-induced crystallization to small changes in the imposed stress and the material. Experimental data on a bimodal blend of isotactic polypropylenes are presented.