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Early detection of nitrogen oxide gases has become a vital process even at low concentrations. Herein, iron oxide nanoparticles)IO NPs( were prepared by hydrothermal technique (homemade reactor) followed by doping with copper and gold (Cu/Au NPs) via laser ablation, and they were used for NO2 gas sensing. The microstructures of IO NPs before and after the doping were characterized by UV-Vis spectrum UV-visible spectroscopy, field emission scanning electron microscopy (FE-SEM), and X-ray diffraction (XRD). The results have shown a change in the shape, whereas the particle size has grown post the doping by 30%. The optical energy gap of pure IO NPs is approximately 3.0 eV, and the Cu/Au IO NPs are reduced to 2.75 eV. The Cu/Au IO NPs have excellent behaviour as gas sensing properties towards nitrogen dioxide (NO2) gas in the operating temperature range of RT 200 °C. Relative to IO NPs, Cu/Au IO NPs exhibited the best response of 85 towards NO2 at RT. This response is over two times as high as compared with IO NPs. The enhanced NO2 sensing mechanism of the IO NPs could be attributed to the synergistic effects of catalytic activity and chemical sensitization by doping of Cu/Au NPs. [ABSTRACT FROM AUTHOR]