In this work, novolac resin with perfluorinated side chains was synthesized and cured with <i>o</i>-Cresol novolac epoxy resin to obtain epoxy resins with various fluorine contents. Attenuated total reflection Fourier transform infrared spectroscopy (ATR/FT-IR) was used to monitor the <i>in situ</i> water diffusion process in these systems. The diffusion coefficient of water first increased and then slightly decreased with increasing fluorine content, which could be attributed to two opposite effects induced by perfluorinated side chains: enhanced hydrophobicity and increased free volume. In addition, generalized two-dimensional (2D) correlation analysis was employed to investigate both the sorption and the desorption process of water diffusion, and two kinds of water molecules, named bound and free water, were found. It was interesting to find that in the sorption process, the change in the population of bound water molecules occurs earlier than the change in the population of free water molecules, while in the desorption process, the sequence was reversed.
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