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The in-situ synthesis of piezoelectric-reinforced metal matrix composites has been attempted with a variety of target matrix and reinforcement materials using reaction synthesis and high energy ball milling. Zinc oxide (ZnO) and barium titanate (BaTiO₃) have been successfully synthesized within copper and iron matrices in a range of volume percentages using reaction synthesis. The microstructures of these composites have been analyzed and found to partially consist of an interpenetrating microstructure. After considering experimental findings and thermodynamic issues involved with synthesis, ideal reaction system parameters have been identified that promote the creation of a composite with ideal microstructure and formulated composition. Reactive high energy ball milling has been used to create copper matrix composites reinforced with zinc oxide and copper matrix composites reinforced with lead titanate (PbTiO₃). The microstructures and compositions of each volume percentage formulation of the composite powders have been analyzed. In this work, several promising piezoelectric-reinforced metal matrix composite systems have been identified as having potential to be synthesized in an in-situ manner. Master of Science