The fine-structure characterization of polymer-based materials is one of the fastest-evolving areas in polymer science. Modern synchrotron light sources, equipped with high-flux microfocus optics and advanced detectors, offer powerful capabilities for investigating morphology, crystallinity, and nanoscale organization. Over the past two decades, synchrotron wide- and small-angle X-ray scattering (WAXS and SAXS) beamlines have become increasingly accessible and very useful for studying complex polymer systems.

This lecture presents three representative case studies. First, synchrotron WAXS and SAXS reveal structural features associated with enzyme immobilization on engineered polyamide microparticles, an essential step in designing efficient biocatalytic materials. Second, microbeam WAXS scans of polyamide powders (grain sizes 20–50 µm) produced by in situ polymerization effectively detect micron-scale inhomogeneities caused by embedded clays or metal particles, advancing the development of smart polymer-based enzyme carriers and microdevices. Finally, in polymer microfibrillar composites (MFCs), WAXS quantifies transcrystallinity and links it directly to mechanical performance, while advanced SAXS data analysis under controlled strain demonstrates reversible, strain-induced crystallization of the matrix polymer impossible to observe by other methods.

These examples show how synchrotron-based WAXS and SAXS have become essential tools for exploring nanostructure–property relationships and guiding the design of next-generation functional and sustainable polymer materials.

University of Minho, IPC – Institute for polymers and Composites, campus of Azurem, Guimarães 4800, Portugal