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The hybrid metal matrix composites are characterized on the basis of five samples of different composition of hybrid metal matrix composite (MMC) Al-2014/SiC/Fly-Ash an average particle size (APS) of 25 µm. The fabrication of hybrid metal matrix composite is done by liquid stir-casting route. The hybrid MMC is characterized by the Microstructure analysis, X-Ray Diffraction (XRD) analysis and Differential Thermal analysis (DTA), Thermogravimetric analysis (TGA). The results reveal that the reinforcement (SiCp and Fly-ash) particles are uniformly distributed in the composite material. X-Ray Diffraction shows that no other elements are present while mixing reinforcement with Al alloy matrix. The DTA/TGA result shows that Al-2014/15% SiC/5% Fly ash hybrid composite has minimum loss of mass in comparison with other compositions which have been taken.