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Heteroatom-doping has been proved as an effective method to modulate the electronic, physical, and chemical properties of graphene (Gr). Developing a new strategy of heteroatom-doping for high-performance gas sensing is a pivotal issue. Here, we demonstrate novel Gr-based gas sensors through three-dimensional (3D)-structured B-/N-doping nanomaterials for high-performance NO₂ sensing. The 3D porous B- and N-doped reduced graphene oxide hydrogels (RGOH) are synthesized via one-step hydrothermal self-assembly and employed as transducing materials to fabricate room-temperature high-performance chemiresistors. The systematic characterizations of the as-synthesized B- and N-RGOH clearly show the uniform doping of the B and N heteroatoms and the formation of B and N components with C/O. In comparison with the pristine RGOH counterpart, the 3D B- and N-RGOH sensors exhibit 38.9 …