Graphite phased carbon nitride (g‐C 3N 4) has attracted extensive attention attributed to its non‐toxic nature, remarkable physical–chemical stability, and visible light response properties. Nevertheless, the pristine g‐C 3N 4 suffers from the rapid photogenerated carrier recombination and unfavorable specific surface area, which greatly limit its catalytic performance. Herein, 0D/3D Cu‐FeOOH/TCN composites are constructed as photo‐Fenton catalysts by assembling amorphous Cu‐FeOOH clusters on 3D double‐shelled porous tubular g‐C 3N 4 (TCN) fabricated through one‐step calcination. Combined density functional theory (DFT) calculations, the synergistic effect between Cu and Fe species could facilitate the adsorption and activation of H 2O 2, and the separation and transfer of photogenerated charges effectively. Thus, Cu‐FeOOH/TCN composites acquire a high removal efficiency of 97.8%, the mineralization rate of 85.5% and a first‐order rate constant k = 0.0507 min −1 for methyl orange (MO) (40 mg L −1) in photo‐Fenton reaction system, which is nearly 10 times and 21 times higher than those of FeOOH/TCN ( k = 0.0047 min −1) and TCN ( k = 0.0024 min −1), respectively, indicating its universal applicability and desirable cyclic stability. Overall, this work furnishes a novel strategy for developing heterogeneous photo‐Fenton catalysts based on g‐C 3N 4 nanotubes for practical wastewater treatment.
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