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To overcome the ever-growing organic pollutions in the water system, abundant efforts have been dedicated to fabricating efficient Fenton-like carbon catalysts. However, the rational design of carbon catalysts with high intrinsic activity remains a long-term goal. Herein, we report a new N-molecule-assisted self-catalytic carbonization process in augmenting the intrinsic Fenton-like activity of metal–organic-framework-derived carbon hybrids. During carbonization, the N-molecules provide alkane/ammonia gases and the formed iron nanocrystals act as the in situ catalysts, which result in the elaborated formation of carbon nanotubes (in situ chemical vapor deposition from alkane/iron catalysts) and micro-/meso-porous structures (ammonia gas etching). The obtained catalysts exhibited with abundant Fe/Fe–N_x/pyridinic-N active species, micro-/meso-porous structures, and conductive carbon nanotubes …