The　Fe0/C3N4/MoS2　heterostructure　was　fabricated　through　photochemical　synthesis　that　was　free　of　NaBH4.　Specifically,　the　g-C3N4/MoS2　(GCNM)　composite　was　used　as　the　substrate.　Visible　light　excited　the　electrons　from　the　valence　band　of　the　GCNM　in　the　substrate,　and　the　excited　electrons　reduced　the　Fe2+　ions　in　the　solution　nearby　GCNM　to　Fe0　and　then　created　the　Fe0/C3N4/MoS2　heterostructure.　Small　Fe0　(0　nanoparticles.　The　smaller　size　of　Fe0　provided　a　larger　number　of　active　metal　centers　and　improved　the　carrier　separation　efficiency.　As　a　result,　the　Fe0/C3N4/MoS2　heterostructure　exhibited　superior　catalytic　properties　in　the　redox　reactions　of　rhodamine　B,　Cr(VI),　Pb(II),　and　Cd(II).　It　could　also　be　readily　recycled　without　severe　loss　of　catalytic　performance.　©　2017