Abstract. In the present study, Au-surfactant core-shell colloidal nanoparticles (NPs) with controlled dimension and composition were synthesized by sacrificial anode electrolysis. Transmission electron microscopy (TEM) revealed that Au NPs core diameter is between 8 and 12 nm, as a function of the electrosynthesis conditions. Moreover, surface spectroscopic characterization by X-ray photoelectron spectroscopy (XPS) analysis confirmed the presence of nanosized gold phase. Controlled amounts of Au NPs were then deposited electrophoretically on carbon nanotube (CNT) networked films. The resulting hybrid materials were morphologically and chemically characterized using TEM, SEM (scanning electron microscopy) and XPS analyses, which revealed the presence of nanoscale gold, and its successful deposition on CNTs. Au NP/CNT networked films were tested as active layers in a two-pole resistive NO₂ sensor for sub-ppm detection in the temperature range of 100–200 °C. Au NP/CNT exhibited a p-type response with a decrease in the electrical resistance upon exposure to oxidizing NO₂ gas and an increase in resistance upon exposure to reducing gases (e.g. NH₃). It was also demonstrated that the sensitivity of the Au NP/CNT-based sensors depends on Au loading; therefore, the impact of the Au loading on gas sensing performance was investigated as a function of the working temperature, gas concentration and interfering gases.