The effect of thermal/plasma treatment on the photocatalytic degradation of methylene blue (MB) using Au-doped Fe/TiO2 photocatalyst was investigated. Iron (Fe)-doped TiO2samples were prepared by solgel auto-combustion technique. Later, gold nano-particles (AuNPs) were deposited on the as-prepared support (Fe/TiO2) using conventional deposition–precipitation method with NaOH (DP NaOH), and the resulting catalysts were subsequently modified with thermal (at 450°C under vacuum) and plasma (at an ambient temperature under Argon atmosphere for 20 min) treatments.