ORIGINAL PAPER Underpotential deposition of selenium and antimony on gold Yuan Chen 1,2,3 & Lishi Wang 1,2 & Annie Pradel 3 & Alexandre Merlen 2,4 & Michel Ribes 3 & Marie-Christine Record 1,2 Received: 26 February 2015 /Revised: 30 April 2015 /Accepted: 6 May 2015 /Published online: 21 May 2015 # Springer-Verlag Berlin Heidelberg 2015 Abstract The present paper is a detailed study on the depo- sition of Sb 2 Se 3 thin films by electrochemical atomic layer epitaxy (EC-ALE). The related electrochemical aspects have been deeply investigated by means of cyclic voltammetry, anodic potentiodynamic scanning, and coulometry. The UPD layer of Se was obtained by first depositing both UPD Se and a small amount of bulk Se and then stripping the redundant bulk Se in blank solutions. A Btwo times rinsing^ method was developed to avoid the formation of red Se during the rinsing process. The deposition parameters were deter- mined for the first three EC-ALE cycles, and from these values, a nanofilm containing Sb and Se atoms has been ob- tained. By scanning electron microscopy and coulometry, it was shown that the deposit is compact and it has a stoichiom- etry very close to that of Sb 2 Se 3 . The Raman spectral analyses show that the deposit is made of Sb 2 Se 3 nanoclusters. Keywords Electrochemistry . Underpotential deposition . EC-ALE . Sb 2 Se 3 . Thin films Introduction Sb 2 Se 3 is the unique intermediate compound in the Sb–Se equilibrium phase diagram [1]. Sb 2 Se 3 is a semiconductor with a layered crystal structure (space group Pnma; no. 62) in which each Sb atom and each Se atom is bound to three atoms of the opposite kind that are held together by weak secondary bonds [2]. Due to its promising applications in several fields such as optoelectronic, photovoltaics, batteries, and thermoelectric energy conversion, both elaboration and characterization of this compound have been largely studied (see for example ref. [3–8]). Miniaturization of the devices requires the use of thin films which are usually prepared by physical vapor deposition methods. Electrochemical deposi- tion may provide an alternative process to these classical methods. Indeed, by contrast to other methods, electrochemi- cal deposition is a low cost, room temperature production technique, which allows one to cover substrates with complex shapes. Some studies have already been reported on electro- chemical deposition of Sb 2 Se 3 [9–12]. In these works, Sb 2 Se 3 thin films were obtained by co-deposition of antimony and selenium. The crucial point in material electrodeposition is to control the dimensions, the stoichiometric ratio, and the crystallinity of the deposited structures. The electrochemical atomic layer epitaxy (EC-ALE) technique developed by Stickney [13] was proved to be a valid approach to control these parameters for the deposition of chalcogenide com- pounds on metallic substrates [14–19]. This method is based on the alternate underpotential deposition of atomic layers of the elements that form the compound, in a cycle that can be repeated as many times as desired. The major advantage of this method is that the individual steps of each cycle can be investigated and optimized independently. The aim of the present work is to deeply investigate the deposition of Sb 2 Se 3 thin films by the EC-ALE method. The * Marie-Christine Record m-c.record@univ-amu.fr 1 Aix-Marseille University, IM2NP, 13397 Marseille Cedex 20, France 2 CNRS, UMR 7334, IM2NP, 13397 Marseille Cedex 20, France 3 Institut Charles Gerhardt Montpellier, UMR CNRS 5253, ChV, CC1503, Université Montpellier II, Place Eugène Bataillon, 34095 Montpellier Cedex 5, France 4 Université de Toulon, IM2NP, Avenue de l’Université, 83957 La Garde, France J Solid State Electrochem (2015) 19:2399–2411 DOI 10.1007/s10008-015-2881-0