The cathodic electrodeposition of CdS from aqueous solutions of Cd 2+ and S 2 O 3 2− at 40 °C, has been achieved using a combination of cyclic voltammetric and potentiostatic techniques. The voltammetric responses of the investigated thiosulfate, Cd 2+ both individually as well as with each other are achieved and hence the optimum conditions for the electrodeposition of CdS were determined. Interesting data was obtained and discussed in this work. The mechanism of the electrode reactions for the investigated substance have been evaluated and proposed. X-ray diffraction investigations demonstrate that the electrodeposited CdS is hexagonal polycrystalline in nature. Furthermore, the electrodeposited CdS is of n-type semiconductor was investigated by Mott-Schottky test and from it, donor concentration (N D) is also determined.