The　synergistic　effect　of　carbon　materials　with　high　sp(2)/sp(3　)hybridized　carbon　ratio　and　metal　materials　can　enhance　the　efficiency　of　peroxymonosulfate　(PMS)　based　advanced　oxidation　processes.　In　this　study,　a　composite　of　highly　dispersed　Fe(7)S(8　)anchored　on　sp(2)/sp(3)　hybridized　carbon　(Fe7S8@HC)　was　developed　by　a　facile　synthesis　for　PMS　activation.　Within　10　min,　the　removal　efficiency　of　the　target　pollutant　doxycycline　(DOX)　could　reach　ca.　96　%　in　optimal　Fe7S8@HC/PMS　system　through　a　O-1(2)-dominated　non-radical　pathway.　Correlation　mechanism　analysis　revealed　that　thiophene　S,　sp(2)/sp(3　)ratio　and　Fe(II)　were　critical　factors　for　elongating　of　the　O-O　bond　of　PMS.　Moreover,　the　Fe7S8@HC/PMS　system　exhibited　favorable　adaptability　to　interference　such　as　common　inorganic　anions,　humic　acid　and　pH　changes　and　could　effectively　remove　various　organic　pollutants　with　low　ionization　potential.　Moreover,　the　system　maintained　high　DOX　removal　efficiency　by　running　30　cycles　in　a　continuous　flow　reactor.　Finally,　susceptible　sites　of　DOX　and　four　degradation　pathways　were　proposed　by　density　functional　theory　calculation　and　LC-MS　detection.　This　work　not　only　offered　new　insights　into　the　design　of　high-performance　catalysts　combining　metal　and　biomass-based　carbon　materials,　but　also　provided　technical　support　for　the　remediation　of　water　bodies　containing　emerging　organic　contaminants.