Two　transition　metal　ions　(Cu2+　and　Co2+)　and　two　rare　earth　metal　ions　(Ce3+　and　La3+)　were　used　as　the　assisted　metal　ions,　respectively　to　prepare　the　transition　metal　and　rare　metal　assisted　Fe　bimetallic　amidoximated　polyacrylonitrile　(AO-PAN)　fiber　complexes.　And　their　coordination　configuration　and　visible　light　adsorption　properties　were　examined　by　coordination　number　determination　and　UV-vis-DRS.　Then　the　catalytic　performance　of　these　complexes　was　evaluated　as　the　heterogeneous　Fenton　catalysts　in　Rhodamine　B　degradation　by　changing　the　nature　and　dosage　of　the　assisted　ions　added.　The　results　indicated　that　the　incorporation　of　the　assisted　metal　ions　led　to　Fe　bimetallic　AO-PAN　complexes　with　the　more　unsaturated　configurations　than　Fe　monometallic　AO-PAN　complex　due　to　the　changes　in　their　coordination　numbers.　The　visible　light　adsorption　properties　of　Cu-Fe　or　Ce-Fe　AO-PAN　bimetallic　complexes　varied　significantly　with　their　Cu/Fe　or　Ce/Fe　molar　ratio.　Fe　bimetallic　AO-PAN　complex　showed　a　higher　catalytic　performance　as　the　Fenton　catalysts　toward　the　dye　degradation　than　Fe　monometallic　AO-PAN　complex.　And　the　nature　and　dosage　of　the　assisted　metal　ions　can　affect　their　catalytic　activities.　Ce-Fe　bimetallic　AO-PAN　complex　was　found　to　have　a　better　stability　in　a　wider　pH　range　than　Cu-Fe　bimetallic　AO-PAN　complex.　©　2011　Elsevier　B.V.　All　rights　reserved.