WithFe(NO3)39H2OandBi(NO3)35H2Oasrawmaterials,differentsillenite-typecompoundsandelementalbismuthwerepreparedbyafacileone-potsolvothermalmethodusingH2O,C2H5OH,(CH2OH)2andC3H8O3assolvents,respec-tively.Thestructure,morphology,elementalcompositionsandpropertiesofsampleswereexaminedbyXRD,SEM,TEM,ICP,XPS,N2adsorptionanddesorption,UV-visDRSandPL.ThephotocatalyticactivitiesofdifferentsampleswereevaluatedbythephotodegradationofRhBundervisible-lightirradiation(λ>400nm),andresultsshowthatBi36Fe2O57preparedusingC2H5OHasthesolventownstheoptimumperformance.Inordertoexplorethereactionmechanism,anadditionalexperimentwasdesignedtoinvestigatethemainactivespeciesduringthephotodegradationprocessviadissolvingdifferenttrappingagentsinthereactionsolutionbeforelightirradiation.TheresultsshowthatsuperoxideradicalanionsplayamajorroleinthissystemsincetheRhBdegradationwassignificantlysuppressedaftertheadditionofbenzoquinone.
