This paper presents an experimental investigation of the rectangular diffusion hole. The effects of rectangular aspect ratio and lateral diffusion angle on film-cooling effectiveness were studied at a low-speed flat-plate experimental facility. The pressure-sensitive paint (PSP) measurement technique was employed to determine the adiabatic effectiveness. The experiments were performed at a density ratio of DR = 1.38 and a mainstream turbulence intensity of Tu = 3.5%. The blowing ratio was varied from M = 0.5 to M = 2.5. Three aspect ratios and three lateral diffusion angles were chosen to match the semicircle and straight-line sidewall shape of the rectangular cross section. A comparative investigation was performed among a typical fan-shaped hole and ten rectangular diffusion holes. The experimental results exhibited diversified film distribution patterns of the rectangular diffusion hole, including single-, bi-, and tripeak patterns. The overall cooling effectiveness increased with the increase of rectangular aspect ratio. The improved magnitude was amplified as blowing ratio increased. The holes with semicircle sidewall were shown to be more suitable for high blowing ratio conditions. The maximum increase of cooling effectiveness was over 70% compared to the fan-shaped hole. The reduction of the lateral diffusion angle affected the film distribution pattern significantly, thereby influencing the cooling effectiveness. To obtain a fixed coverage ratio of film hole row, the rectangular diffusion hole with a larger cross-sectional aspect ratio and a slightly smaller lateral diffusion angle is a preferred scheme.