Unitized regenerative fuel cells (URFCs) have become more attractive for some time due to its potentially wide energy storage application such as in fields of space and renewable energy. In this study, TiC supported Pt–Ir electrocatalysts (Pt–Ir/TiC) for oxygen electrode in URFCs were synthesized, respectively, by chemical reduction process and plasma reduction process. Their physical and electrochemical properties are characterized and compared using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), cyclic voltammogram (CV), potentiostatic technique, and electrochemical impedance spectroscopy (EIS). The results from XRD, XPS and TEM demonstrate that the plasma process gives a finer metal crystals and higher metal dispersion on the TiC support. The CV, polarization, potentiostatic and EIS results show that the Pt–Ir/TiC electrocatalyst prepared by the plasma reduction process is obviously more active than that by the chemical reduction process, in agreement with the above metal-dispersion observations. The plasma process is a promising way for the preparation of supported electrocatalysts.