The preparation of visible-light- absorbing nanostructured ZnS:Ni2+ photocatalysts using ultrasonic spray pyrolysis (USP) is presented. The nanoparticles are significantly more active and stable towards H-2 evolution from aqueous K2SO3 and Na2S solution than conventional ZnS:Ni2+ powders, owing to their good crystallinity and high surface area. This demonstrates the utility of USP in the preparation of highly active photocatalysts.