A　series　of　Cu-Fe　bimetal　amidoximated　polyacrylonitrile　(PAN)　fiber　complexes　with　different　molar　ratios　of　Cu2+　to　Fe3+　ions　was　prepared　using　a　simple　exhaustion　method,　and　characterized　using　FTIR,　DRS　and　XPS,　respectively.　Then　they　were　tested　as　the　heterogeneous　Fenton　catalysts　for　Rhodamine　B　degradation　with　H2O2　in　the　dark　and　under　visible　light　irradiation.　The　results　indicated　that　Cu-Fe　bimetal　amidoximated　PAN　fiber　complexes　could　more　effectively　catalyze　the　dye　degradation　in　water　than　Fe　amidoximated　PAN　fiber　complex,　especially　in　the　dark.　And　introduction　of　Cu2+　ions　significantly　increased　their　catalytic　performance.　0.56　was　the　optimum　molar　ratio　of　Cu2+　to　Fe3+　ions　to　achieve　the　best　catalytic　activity　and　stability.　This　was　mainly　due　to　the　synergetic　effect　in　the　bimetal　complexes.　Visible　light　irradiation　improved　the　catalytic　activity　of　the　complexes,　especially　with　a　low　molar　ratio　of　Cu2+　to　Fe3+　ions.　©　2011　Elsevier　B.V.