The Synthesis and Property Study of NH-Ac-Anchored Multilayer 3D Polymers

This study reports the synthesis, characterization, and property analysis of four novel multilayer 3D polymers (<b>1A</b> to <b>1D</b>) with 1,3-phenyl bridge architectures spanning 248 to 320 layers. High-molecular-weight polymers were successfully synthesized via catalytic Suzuki-Miyaura cross-coupling over a four-day reaction period. Structures, thermal, and optical properties were examined using multiple analytical techniques. Fourier transform-infrared (FT-IR) spectroscopy was used to study the hydrogen bonding within the polymer system, suggesting the formation of the polymer through the Suzuki-Miyaura coupling reaction. Ultraviolet-visible (UV-vis) spectroscopy indicated strong electronic delocalization, with maximum absorbance peaks between 257 and 280 nm. Thermal characterization, using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), was used to investigate the thermal stability. TGA results showed that all four polymers retained more than 20% of their initial mass at 1000 °C, indicating good thermal stability across the series. DSC analysis revealed that polymer <b>1A</b> exhibited a glass transition temperature (Tg) of 167 °C, indicating the presence of a network formed by aromatic conjugation and hydrogen bonding. Furthermore, the subtle Tg step observed for <b>1A</b> suggests a degree of crystallinity within the polymer matrix, which was further supported by X-ray diffraction (XRD) analysis. Aggregation-induced emission (AIE) experiments provided further insights into intermolecular packing, and scanning electron microscopy (SEM) contributed to a better understanding of the morphology of the obtained polymers. These results highlight the potential of these polymers as thermally stable and conductive materials for biomedical and industrial applications.