Heating–freezing effects on the pore size distribution of a kaolinite clay

This study aims to quantify the effect of heating and freezing temperatures on the pore size distribution of saturated clays. Three kaolinite clay specimens were subjected to different temperatures: 20, 70, and − 10 °C. Upon achieving the desired temperature for each specimen, the specimens were flash frozen in liquid nitrogen to preserve their microstructure. Each specimen was, then, freeze-dried for 24 h after which consecutive two-dimensional (2-D) SEM images were taken using a dual focused ion beam/scanning electron microscope. The produced 2-D images of each specimen were used to reconstruct three-dimensional tomographies of the specimens, which were analyzed to determine the pore size distribution at each temperature. Compared to the specimen at room temperature, the pores in the specimen subjected to − 10 °C were larger; this is believed to be due to the formation of ice lenses inside the pores upon freezing and potential merging between initial pores to form larger pores. On the other hand, the heated specimen showed an increase in the volume of the smaller pores and a decrease in the volume of the larger pores compared to the specimen at room temperature. This opposite behavior between the small and large pores in the heated specimen is justified considering (1) the easier flow of water out of the larger pores compared to that in the smaller pores and (2) the anisotropic nature of the thermal expansion of the clay particles.