Sonochemical precipitation of ammonium di uranate (ADU) is studied through precipitative reaction between uranyl nitrate and gaseous ammonia using ultrasonic horn. Effort has been made to investigate the effect of different process parameters such as uranium concentration, temperature and pH of solution on evaluating the physical and morphological characteristics of ADU. ADU was characterized through particle size, surface area, XRD & SEM analysis etc. The results revealed almost a twofold increase in precipitation kinetics in sonochemical route having smaller average particles (agglomer) and superior quality of ADU crystals with respect to uniformity and crystallinity compared to that of the conventional route. Significant improvement is also noticed in surface area and tap density of the prepared ADU powder. Thus, sonochemical technique for gaseous precipitation of ADU suggested an improved quality of the precipitate amenable for downstream process steps for the fuel preparation methods.