The two-layer-structured ZnO p-n homojunctions were prepared on single-crystal Si (100) substrate by depositing undoped n-type ZnO film on N–In codoped p-type ZnO film using ultrasonic spray pyrolysis. The crystal structure and morphology of the obtained ZnO homojunctions were examined by x-ray diffraction, scanning electron microscopy, and atomic force microscopy. The two-layer structure was confirmed by secondary ion mass spectroscopy depth profile analysis. The current–voltage (I–V) characteristics derived from the undoped ZnO/N–In codoped ZnO two-layer structure clearly show the rectifying characteristics of typical p-n junctions. © 2004 American Institute of Physics.