CuZnO (CZO) films have attracted increasing amounts of attention due to their promising potential applications in semiconductor devices. ZnO shows n-type conductivity, and attempts have been made to dope several elements in ZnO to improve the electrical properties. This study investigated the electrical property transitions of CZO films and determined the copper concentration at which the conductivity of CZO films will change from n-type to p-type. In this study, CZO films were fabricated by ultrasonic spray pyrolysis with copper acetate, zinc acetate, and ammonium acetate precursor solution. The concentrations of Cu ions in the CZO films were controlled by the concentration ratios of copper acetate to zinc acetate in the precursor solutions. In addition, these samples were analyzed by Hall effect measurements, X-ray diffraction, transmittance measurements, and photoluminescence measurements. The results show that the conductivity of the CZO film changes from n-type to p-type when the copper ion concentration in the film is 5%.