Al/MgAl 2 O 4 in situ metal matrix composites have been synthesized using value-added silica sources (microsilica and rice husk ash) containing ∼97% SiO 2 in Al-5 wt.% Mg alloy. The thermodynamics and kinetics of MgAl 2 O 4 formation are discussed in detail. The MgO and MgAl 2 O 4 phases were found to dominate in microsilica (MS) and rice husk ash (RHA) value-added composites, respectively, during the initial stage of holding the composites at 750 • C. A transition phase between MgO and MgAl 2 O 4 was detected by the scanning electron microscopy and energy-dispersive spectroscopy (SEM-EDS) analysis of the particles extracted from the composite using 25% NaOH solution. This confirms that MgO is gradually transformed to MgAl 2 O 4 by the reaction 3SiO 2(s) + 2MgO (s) + 4Al (l) → 2MgAl 2 O 4(s) + 3Si (l) . The stoichiometry of MgAl 2 O 4 , n, computed by a new methodology is between 0.79 and 1.18. The reaction between the silica sources and the molten metal stopped after 55% of the silica source was consumed. A gradual increase in mean MgAl 2 O 4 crystallite size, D, from 24 to 36 nm was observed in the samples held for 10 h.