NiFe layered double hydroxide/carbon nitride (NiFe-LDH/g-C3N4) nanocomposite was prepared by a hydrothermal methodology and its performance was investigated as catalyst for sonocatalytic decomposition of tetracycline hydrochloride (TCH), as a prime instance of a newly recognized pollutant in aqueous solution. FE-SEM, EDX, XRD, FTIR, BET, and TGA were performed on the synthesized samples to collect information about the morphology and structure of sonocatalyst. In order to show the sonocatalytic operational efficiency of NiFe-LDH/g-C3N4 nanocomposite, the effect of the fundamental performance indicators on the deterioration of TCH was investigated. The best sonocatalytic effectiveness of 88.5 % was attained by employing 40.25 mg L−1 catalyst, 30.41 mg L−1 TCH and 349 W ultrasonic power at pH = 7.3 within 30 min. A proposed mechanism for the breakdown of TCH in the presence of NiFe-LDH/g-C3N4 nanocomposite within the sonocatalytic circumstances was also presented. The optimal sonocatalytic efficiency was evaluated by experimental design. The reusability assessment of the NiFe-LDH/g-C3N4 nanocomposite for the decomposition of TCH demonstrated consistent performance over five consecutive cycles, with no observable decline.