Low-load iron oxide nanoparticles on Al-SBA-15 prepared using a novel dry milling approach exhibited excelling activities in the microwave-assisted akylation of toluene with benzyl chloride (Lewis acids promoted reaction) and benzyl alcohol (Bronsted acids promoted reaction) as compared to the parent Al-SBA-15 and similar iron oxide nanoparticles supported on Al-MCM-41 materials. Materials prepared using the milling protocol possessed remarkably low iron loadings (<0.1 wt%) but featured highly accessible sites and small nanoparticle sizes that seemed to be related to the observed differences in activities in the systems. (C) 2012 Elsevier B.V. All rights reserved.