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In the process of photocatalytic ammonia synthesis, efficient activation of nitrogen molecules constitutes a fundamental challenge. During the N 2 activation, the close interdependence between the acceptance and donation of electron results in their mutual limitation, leading to high energy barrier for N 2 activation and unsatisfactory photocatalytic performance. This work decoupled the electron acceptance and donation processes by constructing Fe-Bi dual active sites, resulting in enhancing N 2 activation through the high electron trapping ability of Fe 3+ and strong electron donating ability of Bi 2+ . The photocatalytic nitrogen reduction efficiency of 3%Fe/Bi 2 O 2.33 (118.71 μmol g cat -1 h -1 ) is 5.3 times that of Bi 2 O 2.33 (22.41 μmol g cat -1 h -1 ). In-situ Fourier transform infrared (In situ FTIR) spectroscopy and density functional theory (DFT) calculations manifest that Fe 3+ -Bi 2+ dual active sites work together to promote nitrogen adsorption and activation, and the reaction path is more inclined toward alternate hydrogenation path. N 2 adsorption and activation properties are optimized by heteronuclear bimetallic active sites, which offers a new way for the rational design of nitrogen-fixing photocatalysts., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier Inc. All rights reserved.)