The physicochemical properties were studied to observe the influence of ultrasound irradiation on the synthesis of bimetallic solid acid catalyst (Ni-Mo/γ-Al2O3). A set of catalyst was synthesized using conventional method and sonochemical method. The physicochemical characterizations were studied. The characterization techniques such as XRD, FESEM, EDX, TEM, BET surface area and temperature program reduction (H2-TPR) are highlighted in this manuscript. The XRD analysis revealed that with application of ultrasound irradiation, Ni-Mo particles are homogeneously distributed with the support in different crystal structures. The FESEM and TEM analysis confirmed that the nano catalyst synthesized via sonochemical method presents with average size of 15 nm i.e. smaller than the catalyst prepared via impregnation method. The BET surface area, pore size and pore volume also raised up to a certain level. H2-TPR profile showed lower reduction temperature 428 °C for sonochemically synthesized catalyst which assumed to be more active than conventionally synthesized catalyst. © 2016 The Authors.