A simple but effective method, ultrasonic vibration, has been used to prepare the nanoscale (hereafter n‐) Ga droplets. The n‐Ga droplets with average particle size of about 60–80 nm in diameter dispersed in polystyrenes (PS) have been successfully obtained. The low frequency internal friction of solid polystyrenes containing n‐Ga droplets was measured. We observed for the first time, that the internal friction peak caused by n‐Ga droplets appears around 313 K. The peak shifts to higher temperature with increasing frequency, indicating a relaxation peak. It is suggested that the internal friction peak is associated with the relaxation of n‐Ga droplets in the cavities of matrix under applied stress.