How Confinement Affects the Nucleation, Crystallization, and Dielectric Relaxation of Poly(butylene succinate) and Poly(butylene adipate) Infiltrated within Nanoporous Alumina Templates
Alegría Loinaz, Angel María
Müller Sánchez, Alejandro Jesús
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Langmuir 35 (47) : 15168−15179 (2019)
This work describes the successful melt infiltration of poly(butylene succinate) (PBS) and poly(butylene adipate) (PBA) within 70 nm diameter anodic aluminum oxide (AAO) templates. The infiltrated samples were characterized by SEM, Raman, and FTIR spectroscopy. The crystallization behavior and crystalline structure of both polymers, bulk and confined, were analyzed by differential scanning calorimetry (DSC) and grazing incidence wide angle x-ray scattering (GIWAXS). DSC revealed that a change in the nucleation process occurred from heterogeneous nucleation for bulk samples, to homogeneous nucleation for infiltrated PBA, and to surface-induced nucleation for infiltrated PBS. GIWAXS results indicate that PBS nanofibers crystallize in the α-phase, as well as their bulk samples. However, PBA nanofibers crystallize just in the β-phase, whereas PBA bulk samples crystallize in a mixture of α- and β-phases. The crystal orientation within the pores was determined, and differences between PBS and PBA were also found. Finally, broadband dielectric spectroscopy (BDS) was applied to study the segmental dynamics for bulk and infiltrated samples. The glass temperature was found to significantly decrease in the PBS case upon infiltration while that of PBA remained unchanged. These differences were correlated with the higher affinity of PBS to the AAO walls as compared to PBA, in accordance with their nucleation behavior (surface-induced versus homogeneous nucleation respectively).