Abstract: To enhance the recovery of gallium and germanium from zinc powder replacement residues, an ultrasound-assisted two-stage oxygen pressure acid leaching process was developed in this study. The process was optimized at industrially relevant pressure (0.2 MPa), with systematic investigation of key parameters including liquid-to-solid ratio, ultrasonic power, and temperature. Optimal conditions were established as follows: liquid-to-solid ratio of 10:1, ultrasonic power of 360 W, and sulfuric acid concentrations of 15 g/L and 150 g/L for the first and second stages, respectively. Under these conditions, leaching efficiencies of 97.58% for gallium and 76.36% for germanium were achieved, significantly exceeding those obtained through conventional methods. The effects of ultrasonic cavitation on the residues surface structure were characterized using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and inductively coupled plasma optical emission spectrometry. Results demonstrated that ultrasonic cavitation disrupted the dense surface structure, exposing internal inclusions and reducing the adsorption of silica gel and iron hydroxide colloids. Enhanced recovery of copper, zinc, and indium was also observed. These findings highlight the considerable industrial applicability and economic potential of this technology, offering a practical approach for ultrasonic-enhanced hydrometallurgical processing of zinc powder replacement residues.