Sonochemistry was employed to assist the in-situ synthesis hydroxyapatite by sol-gel process aqueous using Ca(NO3)2·4H2O and (NH4)H2PO4 (HApS). The synthesis by assisted sonochemistry reduced the reaction time from 3 h to 11 min. The formation of HApS, hidroxiapatite (HAp) and other compounds during heat treatment at 0, 120, 350 and 700 0C were identified and characterized by FTIR, Raman Dispersive, X-ray and SEM. The spectroscopy characterization showed that chemical bonds in the HApS are the same position that HAp on the main phosphate group peaks appeared at 1098, 1034, 962, 604 and 562 cm− 1 for IR while at 796 cm− 1 for Raman, which was attributed to the asymmetric stretching mode of PO43−. By means of X-ray diffraction, the hexagonal structure of HApS obtained by sonochemistry could be verified. The morphology characterized by SEM showed the similar structure satisfying the porosity and needles of the scaffold bone. This study compared the formation hydroxyapatite with and without sonochemistry.