The present study reports the preparation, characterization, and investigation of properties of DNR/f-Al 2 O 3 nanocomposites through an in situ emulsion polymerization technique. The method consists of the dispersion of pretreated nanoalumina (f-Al 2 O 3 NPs) onto deproteinized natural rubber (DNR) latex, followed by the polymerization reaction with the K 2 S 2 O 8 /K 2 S 2 O 5 redox initiation system, after deproteinization of natural rubber using urea in the presence of a surfactant.