AlSb is a group III–V compound semiconductor material that is conventionally grown by high temperature processes such as Czochralski and Bridgman methods. Development of a method to synthesize AlSb at room temperature will be more economical to help modulate the electronic properties. In this investigation, a pulsed potential electrodeposition method using a room temperature molten salt system (aluminum trichloride, AlCl 3 /1-methyl-3-ethylimidazolium chloride, EMIC) with an addition of SbCl 3 is discussed. The potential pulse parameters were established by carrying out cyclic voltammetry at different concentrations of SbCl 3 and with varying molar ratios of AlCl 3 /EMIC. Stoichiometric AlSb deposits were obtained from an acidic AlCl 3 /EMIC (1.5:1 molar ratio) melt containing 4×10 −3 mol/l of SbCl 3 onto an ordered TiO 2 nanotubular template. The AlSb compound was predominantly amorphous in as-deposited condition and annealing at 350°C for 2h in argon transformed into crystalline phase. The AlSb deposit showed a high resistivity in the order of 10 9 Ω-cm and a defect concentration of 10 16 cm −3 which was attributed to presence of carbon. The deposits obtained from a basic melt (0.67:1 molar ratio of AlCl 3 /EMIC) were enriched with antimony.