Thermodynamic analysis indicates that there is the possibility of chemical reactions between aluminum melt and cenosphere fly ash particles. These particles contain alumina, silica, and iron oxide, which, during solidification processing of aluminum-fly ash composites or during holding of such composites at temperatures above the melting temperature of aluminum, are likely to undergo chemical reduction. These chemical reactions between the fly ash and molten aluminum have been studied by metallographic examination, differential thermal analysis (DTA), scanning electron microscopy (SEM), energy-dispersive X-ray analysis (EDX) and X-ray analysis after holding the aluminum-fly ash composites for different periods above the liquidus temperature. The experiments indicate that there is progressive reduction of silica and mullite in the fly ash, and formation of alumina with holding time of composites at a temperature of 850 ЊC. The walls of the cenosphere fly ash particles progressively disintegrate into discrete particles as the reaction progresses. The rate of chemical reaction was high at the start of holding the composite at a temperature of 850 ЊC, and then the rate significantly decreased with time. The reaction was almost complete after 10 hours.