The studies based on morphological characterization to assess the effects of ultrasound irradiation on synthesis of solid acid catalysts. Three sets of catalyst formulation were synthesized by both wet impregnation method and ultrasound assisted methods with different wt. of Ni loading on γ-Al2O3. The XRD, BET, TEM and FESEM techniques were used to characterize the nano-particles. Physicochemical characterization revealed that the synthesized catalysts particles using ultrasound irradiation were in nano size range (1-24.5 nm) with equal dispersion of metal oxide, high surface area with increase of metal loading and high phase purity than the catalysts synthesized conventional method. These catalysts were also found in various crystal structures like cubic, monoclinic and tetrahedral. The use of ultrasound irradiation has great significance over the wet impregnation method in relation to the rate of synthesis of nanocatalysts. The high surface area, high thermal stability and small particle size (up to 1 nm) are the basic elements for high activity of solid acid catalysts in hydrocracking and hydrodeoxygenation of various feedstock in petroleum industries. © 2016 Trans Tech Publications, Switzerland.