ESEM study of the humidity-induced swelling of clay film

Abstract : We measured the humidity-induced swelling of thin self-standing films of montmorillonite clay by a combination of environmental scanning electron microscopy (ESEM) and digital image correlation (DIC). The films were about 40 µm thick. They were prepared by depositing and evaporating a suspension of clay and peeling off the highly oriented deposits. The rationale for creating such original samples was to obtain mesoscopic samples that could be used to bridge experimentally the gap between the scale of the clay layer and the engineering scale of a macroscopic clay sample. Several montmorillonite samples were used: the reference clay Swy-2, the same clay homoionized with sodium or calcium ions, and a sodium-exchanged Cloisite. The edges of the clay films were observed by ESEM at various relative humidity values between 14% and 95%. The ESEM images were then analyzed by DIC to measure the swelling or the shrinkage of the films. We also measured the adsorption/desorption isotherms by weighing the film samples in a humidity-controlled environment. In order to analyze our results, we compared our swelling/shrinkage and adsorption/desorption data with previously published data on the interlayer spacing obtained by X-ray diffraction and with numerical estimates of the interlayer water obtained by molecular dynamics simulation. The swelling and the hysteresis of this swelling were found to be comparable for the overall macroscopic films and for the interlayer space. The same correspondence between film and interlayer space was observed for the amount of adsorbed water. This suggests that, in the range of relative humidities values explored, the films behave like freely swelling oriented stacks of clay layers, without any significant contribution from the mesoporosity. The relevance of this result for the behavior of clayey sedimentary rocks and the differences with the behavior of nonoriented samples (powders or compacted powders) are briefly discussed. © 2013 American Chemical Society.