A novel method to prepare Pt–Fe 2O 3 nanoparticles (NPs) for organic matter degradation was developed in this study. The main feature of this study was to prepare a gold nano-wire substrate through integration of holographic lithography, microfabrication techniques and electrochemical co-deposition methods. The catalytic gold nano-wire substrate was used for the electrochemical co-deposition of Pt–Fe 2O 3 NPs. The surface morphology of the prepared Pt–Fe 2O 3 NPs was characterized by scanning electron microscope imaging. It was found that the Pt–Fe 2O 3 NPs formed upon the Au nano-wire surface and in the gap between the adjacent nanowires. The X-ray photoelectron spectrum analysis showed that Pt and Fe 2O 3 were the main chemical components of the NPs. The Pt–Fe 2O 3 NPs exhibited a high electrochemical catalytic activity toward methyl orange (MO) degradation under neutral condition, with 93.5% of MO degraded within 6 h at the voltage of −1.5 V. It demonstrated a high potential to be used for degradation of azo dyes under neutral conditions without the addition of any chemical agent and causing any further pollution problem.