A nickel metal–organic framework (Ni-MOF) was successfully synthesized using ultrasound irradiation. Further to this, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FT-IR), Thermo-Gravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and nitrogen adsorption [i.e. Brunauer–Emmett–Teller (BET) Surface Area Analysis] techniques were used to characterize the synthesized Ni-MOF. In addition, the effect of sonication on the surface area, pore diameter and pore volume of the final product was systematically studied using Taguchi technique. The experiments ascertained that manufacturing of the Ni-MOF by means of the ultrasonic-assisted technique is feasible at a relatively shorter time compare to the conventional methods. The final product showed more uniform shape distribution and improved BET properties. The obtained results offered that the synthesized Ni-MOF samples could be used in several applications.