The imaging of ultrafine Au, Pd, CdS, and ZnS particles prepared in reverse micelles has been studied by atomic force microscopy (AFM). Mica substrates, derivatized with a monolayer of amine or thiol-terminated silanes, were used to immobilize the particles. The substrates were exposed to reverse micellar solutions containing the particles and were then immersed in appropriate solvent media to remove surfactants. This resulted in a partial coating of the surfaces by the particles. The particle size was estimated as the height of protrusion, shown on the AFM images. The size values for the Pd and CdS particles, thus obtained, were found to be almost identical to those obtained by transmission electron microscopy (TEM), whereas those for the Au and ZnS particles were larger than those obtained by TEM Scanning electron microscopy shelved that the Au particles tended to aggregate on the surfaces, while Pd particles were isolated from one another. a two (C) Academic Press.