In this study, ZnO-Zn 2 TiO 4 (ZTM) material was prepared through a novel synthesis method based on a ultrasound-assisted polyol-mediated process followed by calcination at a different temperature. Physical features of the samples were studied by using various analysis techniques including XRD, FT-IR, SEM/EDX, pH PZC , and UV–Vis DRS. Subsequently, the materials were employed as catalysts for the photocatalytic degradation of clofibric acid as a model pharmaceutical contaminant. The photocatalytic performance was evaluated under different conditions of calcination temperature, catalyst dosage, starting concentration, and initial pH of clofibric acid solution. The finding results revealed that hexagonal-tetragonal phases of ZnO-Zn 2 TiO 4 calcined at 600 °C (ZTM-600) with an average crystallite size of 97.8 Å exhibited the best degradation efficiency (99%). The primary bands characteristic of ZnO and Zn 2 TiO 4 were displayed by FT-IR analysis and the UV–visible DRS confirms the larger absorption capacity in UV–visible regions. The photogenerated electrons are the powerful reactive species involved in clofibric acid photodegradation process. This study shows a promising photocatalyst and provides new sight to rational design the facets of photocatalysis process for enhanced photocatalytic performances and effective wastewater treatment.