| Abstract: | Small‐angle scattering (SAS) studies are reviewed of adsorption and capillary condensation of water, hydrocarbons and halogenated hydrocarbons near room temperature, and of nitrogen at 78 K in some mesoporous solids, mainly silicas. The theory needed for the interpretation of SAS data is briefly covered. Calculations of the scattered intensity I(q) for a model porous medium show that I(q) depends markedly on the film thickness t. Adsorption and capillary condensation of nitrogen at 78 K in mesoporous silicas was studied by use of in situ SANS, and t as function of the relative pressure P/Ps was estimated. Adsorption of N2 in defects within the silica skeleton at P/Ps<0.1 lead to a significant increase in I(q). Isolated vapor bubbles in capillary condensed nitrogen in a Gelsil® appeared on adsorption near saturation of the pore system. The kinetics of capillary condensation and of drainage were followed. Power law scattering at low q indicated the formation of ramified clusters of voids on drainage of liquid nitrogen from the xerogel Gelsil®. Similar clusters were observed on drainage of water from Vycor® glass. Provided the clusters indicate a percolation process, the desorption branch should not be used for the estimation of a pore size distribution for materials with networked pores. The adsorptive smoothing by benzene was observed of a rough interface in a controlled pore glass. |
