The electrochemical atomic layer epitaxy methodology was employed for the growth of CdSe on Ag(111). for up to 50 deposition cycles. The voltammetric analysis of the first Cd-upd peak indicates a mechanism of two-dimensional growth: this is consistent with layer-by-layer growth, which is a good prerequisite for epitaxial deposits. The amount of Cd and Se deposited in a given number of cycles, as determined by stripping the deposits first anodically and then cathodically. is a function of the number of cycles employed, again suggesting a layer-by-layer growth. The charges associated with each layer of Cd and Se. 75 muCcm(-1). give the right 1:1 stoichiometric ratio between the elements, indicating the formation of a compound. Preliminary results from a structural analysis carried out by extended X-ray absorption spectroscopy (EXAFS) at the Se K edge confirm the presence of Cd neighbors around Se. (C) 2004 Elsevier B.V. All rights reserved.