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• The Fe-doped TiO 2 S-scheme anatase/rutile homojunction (F-T-A/R) was synthesized by a typical solvothermal-annealing method. • The optimized F-T-A/R photocatalyst (A/R = 98:2, Fe-2 wt%) exhibits an unprecedented NH 3 generation rate of 358 μmol gcat-1h−1. • The charge transfer mechanism of S-scheme homojunction and NH 3 production path were investigated. • The synergistic effect of S-scheme homojunction and Fe doping improved the photocatalytic nitrogen fixation. The presence of efficient catalytic active sites and an ample supply of electrons are the two indispensable factors for achieving photocatalytic nitrogen fixation. Herein, the Fe-doped TiO 2 S-scheme anatase/rutile homojunction (F-T-A/R) was synthesized as a brilliant photocatalyst for photocatalytic nitrogen fixation from N 2 to NH 3 under ambient atmosphere. The optimized F-T-A/R photocatalyst (A/R = 98:2, Fe-2 wt%) exhibits an unprecedented NH 3 generation rate of 358 μmol g cat -1h−1 in water solvent and under simulated solar light irradiation. Experimental and theoretical studies reveal that the constructed S-scheme homojunction in F-T-A/R is conducive to fluent charge separation and adequate supply of electrons on rutile with higher nitrogen fixing activity, while the tuned local electronic structure of oxygen vacancy with Fe doping is engineered to strengthen active sites, synergistically enhancing the photocatalytic nitrogen fixation. [ABSTRACT FROM AUTHOR]