A Small-Angle X‑ray Scattering Study of the Development of Morphology in Films Formed from the 3M Perfluorinated Sulfonic Acid Ionomer

An extensive SAXS investigation of the 3M perfluorinated sulfonic acid ionomer was performed to investigate the morphological changes that occur during and after annealing at temperatures above the <i>T</i>_α. The effect of film thickness in the range studied, 11–45 μm, was found to be negligible. These properties were studied as a function of equivalent weight from 700 to 1100 and correlated with the water uptake as measured by dynamic vapor sorption. Isoscattering points were observed in dynamic annealing experiments of the unboiled annealed films at <i>q</i> = 0.023, 0.096 Å^–1. On initial water uptake these films also showed isoscattering points at <i>q</i> = 0.024, 0.220 Å^–1; <i>q</i> = 0.029, 0.223 Å^–1; and <i>q</i> = 0.030, 0.211 Å^–1 at 50, 80, or 95 °C, respectively, indicating a decrease in the symmetry of the scattering objects in these size regimes. Isoscattering points were absent in similar water uptake experiment for the films after boiling