Alloy segregation along with delocalized zone of interest is achieved in direct metal oxidation, DIMOX. Recycling of automotive aluminum piston scrap, alloy 6xxx, is achieved at temperature 1050oC for different holding time 10, and 60 minute. Alloying element, Boron, is added via the addition the boric acid or borax. Liquid state processing, DIMOX, along with semisolid processing, Rheocasting and Thixocasting, are introduced for the control structural micro constituents. The novel technique, DIMOX, induce in situ aluminum metal matrix Nano-composite intrinsically established. The control of composite micro-constituents location, shape and size is also established via semisolid process, Rheocasting and Thixocasting, each at 800ºC for 10 minute, holding time. Microstructural analysis and mechanical characterization are conducted. Rheocasting, induce alloy segregation more dominated into intermetallic and or ceramic alumina phases in a bulk hybrid composite matrix. In contrast, semisolid, Thixocasting, processing dominate more surface coating rather than bulk processing. Boron has a distinguishable effect as an inoculant, induce borate glass in dispersed phases, bulk whiskers or as coating phase. The application of liquid state processing, DIMOX, with the control of micro constituents with the synergetic effect of boron is introduced for new nontraditional Nano-structural hybrid materials.