Catalyst Immobilization methods are important for providing better recovery of catalyst in photocatalytic treatment. The aim is to characterize and evaluate the photocatalytic performance of TiO2/ZnO-coated clay beads. The titanium dioxide/zinc oxide (TiO2/ZnO)-coated clay beads were prepared via the sol-gel process. Various ZnO powder ratios gave different TiO2/ZnO composites sol. Four layers of TiO2/ZnO sol were coated on clay beads and dried in the oven at 100°C for 30 min. The coated clay beads were calcined at 500°C for one hour for every two layers. Characterization of coated clay beads was done using a scanning electron microscope and energy dispersive spectroscopy. The increased surface area on small agglomeration and optimum loading of ZnO (5 g) resulted in the highest degradation efficiency recorded at 86.57%. An effective catalyst immobilization achieved a good recycling performance on clay beads. Degradation rate data were presented by pseudo-first-order kinetics. It was observed that the average degradation rate for TiO2/5 g ZnO is 0.00836 min–1. The actual results in this work can be applied as a guideline for the preparation of TiO2/ZnO-coated clay beads with high photocatalytic performance.