As-Sb alloys have been cathodically deposited onto nickel electrodes from acidic aqueous solutions containing citric acid. The effect of complexing agent concentration, pH, angular speed of the RDE and temperature on deposition rate and alloy composition have been monitored. Increasing citric acid concentration and pH decrease the deposition current and the antimony content of the alloys (measured by EDX analyses). The opposite effect is observed when rotation speed or temperature are increased. Under most combinations of citric acid concentration and pH, the steady-state i/E curves show the current peak already observed in a previous investigation. The morphology and structure of the alloys have been studied with scanning electron microscopy and X-ray diffraction. Alloys containing greater-than-or-equal-to 74% Sb were found to be crystalline (hexagonal system).