Sulfate-radical-based　wastewater　treatment　has　received　great　interest　due　to　its　high-level　efficiency.　However,　the　preparation　of　stable　and　recyclable　nanocatalysts　remains　a　challenge.　Herein,　a　highly　efficient　catalyst　(FeCo/SC)　for　persulfate　activation　is　successfully　synthesized　via　dispersing　S　and　Fe　into　carbon　skeletons　derived　from　ZIF-67.　After　the　introduction　of　S,　FeCo/SC　exhibited　excellent　catalytic　performance.　With　the　action　of　SO4-•,　Fe(VI),　and　1O2,　the　degradation　efficiency　of　carbamazepine　(CBZ)　(10　mg　L-1)　could　be　up　to　97.9　±　2%　within　10　min.　The　results　showed　that　the　larger　surface　area　after　S　doping　decreases　the　electron　transfer　resistance.　The　S0/S2-is　beneficial　for　promoting　the　Fe(III)-to-Fe(II)　and　Co(III)-to-Co(II)　conversion　cycle.　Moreover,　the　liquid　chromatograph-mass　spectrometer　(LC-MS),　density　functional　theory　(DFT),　and　ecological　structure-activity　relationships　(ECOSAR)　revealed　the　possible　degradation　pathway　of　CBZ,　which　was　a　toxicity　attenuation　process.　In　consequence,　this　work　offers　an　innovative　scheme　for　researching　the　effect　of　trace　S-doped　bimetallic　oxide　nanoparticles　on　PDS　heterogeneous　catalytic　systems.　©　2022　American　Chemical　Society.　All　rights　reserved.