A facile process for the conversion of clay powders to organically modified clay aerogels (OMCAs) is reported. The resultant clay aerogels are of potential interest for a variety of applications, by themselves, or as a component in composite materials. Freeze-drying aqueous clay-surfactant solutions isolates these highly organized materials. Robust OMCAs are formed from clay-surfactant compositions that initially produce stable surfactant modified clay-water suspensions. Characterization of the OMCA by FTIR, WAXD, and TGA confirms the retention of surfactant after freeze-drying, while SEM and porosimetry data show a structural reorganization of clay sheet bundles. (c) 2005 American Institute of Chemical Engineers.