Single crystals of PbS in the form pyramids with a high proportion of high energy {3 3 1} faces are obtained by the use of a novel reaction technique at the interface of water and toluene. The pyramids spontaneously form a monolayer spread across the entire water-toluene interface. The influence of deposition parameters such as temperature, solution concentration, reaction time on the nature and properties of interfacial films are studied. In addition, the effect of solvo-static parameters such as column height and interfacial area are investigated. The obtained films are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and high resolution transmission electron microscopy (HRTEM). (C) 2010 Elsevier Inc. All rights reserved.