Al 7075 surface composites (SCs) successfully fabricated with additive three different nano-scale particles multi-walled carbon nanotubes (MWCNTs), graphene (GNP), and titanium dioxide (TiO2) by friction stir processing (FSP). The consecutive two-pass FSP was executed under a controlled cooling environment at −20 °C with methanol pumped beneath the workpiece in a specially designed fixture. All of the SCs exhibited homogenous dispersion of filler nanoparticles in their microstructures. The grain size of SCs was remarkably reduced from that of the substrate. The enhancement in hardness and strength was ascribed fundamentally to the grain refinement and Zener (pinning) effect expedited by coolant circulation. The effect of second phase matrix on grain evolution and precipitate-intermetallics formed after FSP was characterized by scanning electron microscope (SEM) and XRD pattern. It has been recorded that there is around 95–110% increase in hardness values in SCs. The wear rate is also dropped in SCs owing to enhanced hardness and the formation of lubricating coating in the case of carbonaceous composites.
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