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Porous double-channel α-Fe 2 O 3 /SnO 2 heterostructures with tunable surface/interface transport mechanism have been originally fabricated by the electrospinning and subsequent calcination process. With the increase of Sn content from 0 to 5 mol%, the morphology of α-Fe 2 O 3 -based materials changed from porous fibers to ribbons with both sides curled inward. Double-channel structure can provide more active sites and enhanced adsorption capacity with the large specific surface areas of 233.2 m2/g. The optimal α-Fe 2 O 3 /SnO 2 composites exhibit the highest response value (32.38) and fastest response/recovery times (33/58 s) than those of other samples to 100 ppm N,N-dimethylformamide (DMF) at 360 °C. Meanwhile, good cycling and long-term stability and high gas selectivity of the composites are conductive to the feasible detection to DMF under high temperature (≥360 °C) condition. The enhanced gas-sensitive properties of α-Fe 2 O 3 /SnO 2 composites at high temperature are closely related to phase composition, unique morphology, efficient n-n heterojunction and accelerated surface/interface charge transfer process. Significantly, the porous double-channel α-Fe 2 O 3 /SnO 2 composite is expected to be a potential candidate for DMF vapor detection in the dye or pesticide industry to prevent DMF explosion under high temperature conditions in the future. [Display omitted] • Porous double-channel α-Fe 2 O 3 /SnO 2 heterostructures is gained by electrospinning. • The special structure can provide more active sites and enhanced adsorption capacity. • Superior gas-sensing properties to DMF are obtained at high temperature (≥360 °C). • Fe/Sn-0.03 shows the highest response (32.38) and low detection limit (1 ppm) to DMF. • Sensing behavior depends on surface/interface multiple electronic transport routes. [ABSTRACT FROM AUTHOR]