HomogeneousNi2+-dopedtitaniagelwassynthesizedbyasol-gelprocess,andthexerogelwasthenobtainedthroughaginganddrying,leadingtotheformationofNi/TiO2nanocompositeafterheattreatmentunderasuitablereducingatmosphere.TheresultingnanocompositewascharacterizedbyTGA-DSC,TEM,XRDandBETmethods.Theresultsshowthatthestructureandgrainsizeofthenanocompositescouldbemanipulatedbyalteringtheheat-treatmentconditions,andthatthenanocompositepossessesamesoporousstructurewithaporeradiusofca.28nmandaspecifictheanatase-rutilephasetransformation.