A novel method for the synthesis of nanocrystalline zinc oxide was developed using zinc acetate, sodium hydroxide, and hexamethylenetetramine through sonication. The identity, structure, and morphology of prepared nanocrystalline zinc oxide was investigated by various techniques such as IR, PSA, SEM, TEM, and XRD. The reaction mechanism was proposed on the basis of available literature and scientific principles. It was proposed that the surfactant hexamethylenetetramine played a dual role. First, it produced a basic environment that is necessary for the formation of Zn(OH) 2 . Second, it coordinated with Zn 2C and thus stabilized the aqueous Zn 2C . Zn(OH) 2 dehydrated into ZnO when heated in microwave and subjected under ultrasonication. Here, the chemical and physical effects of high intensity ultrasound have been utilized for the preparation or modification of nanostructured zinc oxide. The results show that using ultrasound sonication is green and cost effective compared to the conventional wet chemical method for ZnO nanoparticle synthesis.