Two-Step Wetting of Nanoporous Carbons: Small-Angle Scattering Analysis of Capillary Rise

Numerous applications of nanoporous materials require their pores to be filled with liquids. In spite of its huge technological importance, the conditions for the wetting of nanometer-sized pores and its phenomenology are still poorly understood. We report on capillary rise experiments with water in carbon xerogels, with synchrotron small-angle scattering used to follow the process in situ at the nanometer scale. The data reveal a two-step wetting process whereby water permeates first into molecular-sized micropores, which is followed by the imbibition of larger mesopores. A Cassie-Baxter analysis shows that the presence of water in the micropores is central, as it turns the mesopores from being hydrophobic to hydrophilic. Based on the so-calculated contact angles, the mesopore wetting kinetics are found to be quantitatively described by a classical Washburn model. Modeling of the experimental water profile ahead of the Washburn front reveals strong surface barriers opposing water transfer from the mesopores to the micropores.