简介：ThesolidstateC13-NMRspectraofdifferentACFsfromvariousprecursorfiberswererecordedinthispaper,TheeffectsofactivationconditionsonchemicalstructuresofACFs,aswellasthechangesofchemicalstructuresduringcarbonizationandredoxreactionwereinverstigatedbyNMRtechnique,Atsametime,thesoildstateP31-NMRspectraofACFSarestudied.TheC13-NMRspectraofACFscanbedividedintosixbandsthatareassignedtomethylandmethylenegroups,hydroxylandethergroups.acetal(ormethylenedioxy)carbon,graphite-likearomaticcarbonstructure,phenol,andquinonegroups,respectively.OnlyphosphorouspentoxideexistsonACFsandCFs.Moreover,mostofthemarestuckoverthecrystalfacebutnotattheedgeofgraphite-likemicro-crystal.ThecarbonizationandactivationconditionsaffecttheC13-NMRspectraofACFs.TheexperimentalrsultsindicatethattheredoxreactionofACFswithoxidantsgreatlyconsumesC-Hgroup.