Through a one-step thermal reaction, Au nanoparticles were synthesized and self-assembled mixed films of Au nanoparticles and n-hexylthiol were prepared on iron surface. The size distribution and shape of Au nanoparticles were examined using transmission electron microscopy (TEM). Results of two electrochemical methods – electrochemical impedance spectroscopy (EIS) and polarization curves indicate that self-assembled mixed films can form on the iron surface and prevent it from corrosion effectively. Energy-dispersive X-ray spectroscopy (EDS) and scanning electron microscopy (SEM) measurements were applied to identify the formation of the mixed films on iron surface.