Size-quantized cadmium chalcogenide nanoparticles were effectively deposited on a porous zinc oxide particulate film electrode by a one-step hydrothermal method in which an increase in the concentration of 3-mercaptopropionic acid reduced the size of deposited nanoparticles. The photoelectrochemical properties of the resulting electrodes varied depending on the kind of metal chalcogenide nanoparticles deposited and their size.