In this work dialysis was used as a technique to modify the aggregation state of montmorillonite clay. Na-montmorillonite clay suspension was treated by a dialysis process and the effect of dialysis time on the surface area of the treated clay was studied. In a clay suspension, a decrease in cation content increases the interparticle repulsion forces exponentially, leading to separation of clay into the elementary clusters of layers by osmotic swelling. During dialysis treatment, the classical delamination process and mechanism were not observed. According to N-2 adsorption isotherms, the increase of surface area concerns to the development of mesoporosity. Nevertheless, the surface area increase cannot be explained by the delamination or exfoliation of some layers, since an increase in the expected number of layers that would yield the surface area does not explain the mesoporosity observed after dialysis. Based on these results, a new mechanism of evolution of the clay aggregation state after dialysis and drying is proposed. (C) 2003 Elsevier Inc. All rights reserved.