Oxygen　evolution　has　been　considered　as　the　rate-determining　step　in　photocatalytic　water　splitting　due　to　its　sluggish　four-electron　half-reaction　rate,　the　development　of　oxygen-evolving　photocatalysts　with　well-defined　morphologies　and　superior　interfacial　contact　is　highly　important　for　achieving　high-performance　solar　water　splitting.　Herein,　we　report　the　fabrication　of　Ag3PO4/MoS2　nanocomposites　and,　for　the　first　time,　their　use　in　photocatalytic　water　splitting　into　oxygen　under　LED　light　illumination.　Ag3PO4　nanoparticles　were　found　to　be　anchored　evenly　on　the　surface　of　MoS2　nanosheets,　confirming　an　efficient　hybridization　of　two　semiconductor　materials.　A　maximum　oxygen-generating　rate　of　201.6　μmol　·　L-1　·　g-1　·　h-1　was　determined　when　200　mg　MoS2　nanosheets　were　incorporated　into　Ag3PO4　nanoparticles,　which　is　around　5　times　higher　than　that　of　bulk　Ag3PO4.　Obvious　enhancements　in　light-harvesting　property,　as　well　as　electron-hole　separation　and　charge　transportation　are　revealed　by　the　combination　of　different　characterizations.　ESR　analysis　verified　that　more　active　oxygen-containing　radicals　generate　over　illuminated　Ag3PO4/MoS2　composite　photocatalysts　rather　than　irradiated　Ag3PO4.　The　improvement　in　oxygen　evolution　performance　of　Ag3PO4/MoS2　composite　photocatalysts　is　ascribed　to　wide　spectra　response　in　the　visible-light　region,　more　efficient　charge　separation,　and　enhanced　oxidation　capacity　in　the　valence　band　(VB).　This　study　provides　new　insights　into　the　design　and　development　of　novel　composite　photocatalytic　materials　for　solar-to-fuel　conversion.　©　2018　Cui,　Yang,　Xian,　Tian,　Tang　and　Liu.