In this Paper, ZnO films mixed with iron oxide were prepared by an ultrasonic spray pyrolysis method. The chemical composition and structural properties as a function of the Fe atomic ratio in the deposition solution were studied. Zinc acetate and ferrous chloride were used as precursors of Zn and Fe, respectively. Fe atomic ratio to Zn varied from 0.15 to 10.0. Substrate temperature was fixed at $250^{circ}C$. The crystallographic properties and surface morphologies of the films were studied by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. Electron probe X-ray microanalysis (EPMA) and X-ray photoelectron spectroscopy (XPS) were carried out to analyse the chemical composition and state of Zn and Fe atoms.