An investigation of arsine during electrochemical co-deposition of arsenic with antimony was carried out by cyclic voltammetry and galvanostatic methods. An apparent cathodic peak corresponding to the reduction of Sb(III) to Sb(0) was found before the reduction of arsine, and the amount of arsine was remarkably decreased by the addition of Sb(III). X-ray diffraction characterization indicated that the reduced As atoms were inclined to form stable bond with Sb atoms during the co-deposition process, which made these As atoms less active and then significantly reduced the probability of forming As-H bond. As a result, the evolution of arsine was inhibited efficiently during this co-deposition process. (C) 2013 The Electrochemical Society. All rights reserved.