Ultrasonic treatment was employed to improve the dispersibility of the Fe 3 O 4 nanoparticles dispersed in aqueous solutions. Electrophoresis and XPS spectra indicate that the ultrasonic treatment can induce the generation of chemisorbed hydroxyl groups and the oxidation of Fe 2+ ions on the surface of the magnetic nanoparticles, thus resulting in improved dispersibility of the magnetic nanoparticles. After growth of silica protection layers on the Fe 3 O 4 nanoparticles with different times of ultrasonic treatment, Fe 3 O 4 /SiO 2 core/shell nanoparticles with different amounts of the magnetic cores were successfully prepared.