A method has been developed to produce composition modulated Bi1−x Sb x alloys by electrodeposition. The electrolyte which consists of NaCl 4 M and HCl 1 M (pH 0) in aqueous medium, allows codeposition of bismuth and antimony to be accomplished at room temperature on glassy carbon. The composition of the films, their crystal structure, morphology and resistivity were studied as a function of electrochemical parameters and bath composition. It is shown that the electrodeposits are monophasic and exhibit a polycrystalline state. The obtained alloys represent a continuous series of solid solution. The film composition is dependent on the applied current density. The electrical resistivity is of the order of 3–7 μΩm.