Diglycidyl ether of bisphenol A (DGEBA) and diglycidyl ether of bisphenol F (DGEBF) reinforced with organomontmorillonite clay nanoplatelets were investigated using anhydride-and amine-curing agents. The sonication technique was used to process epoxy/clay nanocomposites. The basal spacing of clay nanoplatelets was observed by wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS) techniques, and transmission electron microscopy. It was found that the basal spacing of clay nanoplatelets in epoxy matrix was expanded after mixing with either DGEBA/DGEBF or methyltetrahydrophthalic-anhydride (MTHPA) curing agent. The sonication technique provided larger d-spacing of clay nanoplatelets. Because of the different curing temperatures, MTHPA-cured epoxy/clay nanocomposites produced more expanded d-spacing of clay nanoplatelets modified with methyl, tallow, bis(2-hydroxyethyl) quaternary ammonium (MT2EtOH) than triethylenetetraminecured nanocomposites. Depending on the selection of curing agent and organic modification for clay nanoplatelets, the d-spacing was expanded to be up to 8.72 nm. POLYM. ENG. SCI., 46:452-463, 2006. 453 FIG. 2. FTIR spectra of neat epoxy and its clay nanocomposites at different clay compositions. (a) MTHPAcured epoxy nanocomposites and (b) TETA-cured epoxy nanocomposites. 455 FIG. 11. XRD (Rigaku DMAX-A WAXS) diffraction pattern, at small diffraction angle, of organo-montmorillonite clay nanoplatelets (Cloisite 30B), TETA-cured neat epoxy, and their nanocomposites, prepared by the sonication technique at different organo-clay compositions.