CdS/ZnS core-shell microparticles were prepared by a simple two-step method combining ultrasonic spray pyrolysis and chemical bath deposition.The core-shell structures showed enhanced photocatalytic properties compared with those of CdS or ZnS spherical particles.CdS/ZnS photocatalysts with different amount of ZnS loaded as shells were prepared by adjusting the concentrations of Zn and S precursors during synthesis.The optical properties and photocatalytic activity for hydrogen production were investigated and the amount of ZnS loaded as shell was optimized.Thermal annealing and hydrothermal sulfurization treatments were applied to the core-shell structure and both treatments enhanced the material's photocatalytic activity and stability by eliminating crystalline defects and surface states.The result showed that thermal annealing treatment improved the bulk crystallinity and hydrothermal sulfurization improved the surface properties.The sample subjected to both treatments showed the highest photocatalytic activity.These results indicate that CdS/ZnS core-shell microspheres are a simple structure that can be used as efficient photocatalysts.The hydrothermal sulfurization treatment may also be a useful surface treatment for metal sulfide photocatalysts.The simple two-step method provides a promising approach to the large-scale synthesis of core-shell microsphere catalysts.