10.1002/cctc.201000057.abs　Gold　nanoparticles　were　deposited　on　the　surface　of　a　g-C3N4　semiconductor　by　deposition-precipitation,　photodeposition,　and　impregnation　methods　to　make　metal-semiconductor　junctions　for　photocatalytic　hydrogen　evolution　from　aqueous　solution　containing　an　electron　donor　with　visible　light　illumination.　The　samples　were　characterized　by　X-ray　diffraction　(XRD),　X-ray　photoelectron　spectroscopy　(XPS),　UV/Vis,　and　transmission　electron　microscopy　(TEM).　Results　show　that　the　Au/g-C3N4　prepared　by　the　deposition-precipitation　method　possessed　the　best　photocatalytic　activity,　due　to　the　formation　of　tight　Au-semiconductor　heterojunctions　effectively　promoting　the　transfer　of　charge　from　light-excited　g-C3N4.　Surface　modification　of　the　Au/g-C3N4　with　a　second　metal　further　improved　the　activity　of　the　photocatalytic　system,　which　was　explained　by　simultaneous　optimization　of　electron　transfer　by　the　gold　and　chemical　reactivity　by　the　secondary　metal.　©　2010　WILEY-VCH　Verlag　GmbH　&　Co.　KGaA,　Weinheim.