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Graphene oxide (GO) doping and reduction allow for physicochemical property modification to suit practical application needs. Herein, the challenge of simultaneous low‐thermal‐budget heteroatom doping of GO and its reduction in ambient air is addressed through the synthesis of B‐doped reduced GO (B@rGO) by flash irradiation of boric acid loaded onto a GO support with intense pulsed light (IPL). The effects of light power and number of shots on the in‐depth sequential doping and reduction mechanisms are investigated by ex situ X‐ray photoelectron spectroscopy and direct millisecond‐scale temperature measurements (temperature >1600 °C, < 10‐millisecond duration, ramping rate of 5.3 × 105 °C s−1). Single‐flash IPL allows the large‐scale synthesis of substantially doped B@rGO (≈3.60 at% B) to be realized with a thermal budget 106‐fold lower than that of conventional thermal methods, and the prepared material with abundant B active sites is employed for highly sensitive and selective room‐temperature NO2 sensing. Thus, this work showcases the great potential of optical annealing for millisecond‐scale ultrafast reduction and heteroatom doping of GO in ambient air, which allows the tuning of multiple physicochemical GO properties. [ABSTRACT FROM AUTHOR]