Multilayer modified spherical polyelectrolyte brushes were prepared through alternate deposition of positively charged poly(allylamine hydrochloride) (PAH) and negatively charged poly-l-aspartic acid (PAsp) onto negatively charged spherical poly(acrylic acid) (PAA) brushes (SPBs) on a poly(styrene) core. The charge reversal determined by the zeta potential indicated the success of layer-by-layer (LBL) deposition. The change of the structure during the construction of multilayer modified SPBs was observed by small-angle X-ray scattering (SAXS). SAXS results indicated that some PAH chains were able to penetrate into the PAA brush for the PAA-PAH double-layer modified SPBs whereas part of the PAH moved towards the outer layer when the PAsp layer was loaded to form a PAA-PAH-PAsp triple-layer system. The multilayer modified SPBs were stable upon changing the pH (5 to 9) and ionic strength (1 to 100 mM). The triple-layer modified SPBs were more tolerated to high pH (even at 11) compared to the double-layer ones. SAXS is proved to be a powerful tool for studying the inner structure of multilayer modified SPBs, which can establish guidelines for the a range of potential applications of multilayer modified SPBs.

Zeolites, as crystalline materials with regular pore channels, are widely utilized in energy, environmental, and advanced manufacturing sectors. Characterizing zeolites is crucial for understanding their structure and properties, which are essential for various applications. Synchrotron Radiation‐based X‐ray Diffraction (SR‐XRD) has become an advanced tool in zeolite research, providing higher resolution, faster scans, and more precise structural information than laboratory X‐ray diffraction methods. This technique allows for detailed studies, from atomic structures to dynamic behaviors, particularly in understanding structural evolution during synthesis and monitoring changes in the framework during reactions. Moreover, SR‐XRD has made significant contributions to catalytic research by revealing structural alterations during catalytic processes and identifying active sites. However, SR‐XRD still faces challenges in data interpretation and other technological limitations. To overcome these, integrating SR‐XRD with other techniques and using AI‐assisted analysis are expected to further advance zeolite characterization and catalytic research.