This investigation demonstrates the successful synthesis of well-crystallized pristine and Ag-doped BiFeO3 microspheres using flash auto combustion technology. The effects of Ag doping on the morphology and microstructural characteristics were thoroughly examined through SEM, EDS, and powder X-ray diffraction (XRD) studies. Gas sensing experiments were performed to evaluate the response of the synthesized materials to NO gas. The results revealed a remarkable enhancement in the gas sensing capabilities of 5% wt Ag-doped BiFeO3 compared to pure BiFeO3. Specifically, the gas response towards NO was found to be 2.4 times higher for Ag-doped BiFeO3. This significant improvement can be attributed to the presence of Ag atoms within the lattice structure, which not only increased the density of holes in the material but also created additional gas molecule adsorption sites. Furthermore, the Ag dopant exhibited a catalytic effect, contributing to the excellent gas sensor performance of the material. These findings hold great promise for the development of highly sensitive and efficient gas sensors, particularly in applications where the detection of low concentrations of NO is crucial. The utilization of flash auto combustion technology in the synthesis process offers a viable route for scalable production of advanced gas sensing materials with enhanced performance.