A novel and facile approach for the preparation of exfoliated/delamination kaolinite was reported in this study. Kaolinite was mechanochemically activated by grinding with dimethylsulfoxide in a globe mill for different periods of time, and then the activated samples were treated for several hours at 120 degrees C to obtain the precursors of kaolinite. The resulting materials were characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy. The experimental data indicated that the clay layers were well exfoliated/delamination under mechanochemical effect in a significantly short intercalation time. The expansion of the basal spacing (d(0 0 1)) of raw kaolinite by 0.40 nm pointed out that the hydrogen bonds between adjacent kaolinite layers were partially broken as a result of the intercalation with dimethylsulfoxide. (C) 2010 Elsevier Ltd. All rights reserved.