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This paper represents the fabrication and characterization (microstructural, mechanical, and electrical) of Cu-2wt% B-4 wt% Ti and Cu-5wt% B-10wt% Ti alloy from the ball-milled Cu, Ti, and B powders. The in situ formation of TiB₂ was also discussed in the light of differential scanning calorimetry (DSC) and X-ray diffraction (XRD). This present work investigates the effect of various parameters on powder production and the formation of in situ TiB₂ through the thermo-mechanical route. The apparent activation energy during metastable phase formation for the two types of alloy composites has been calculated using the Johnson-Mehl-Avramani (JMA) equation and found to be 567.46 and 626.37 (KJ/mol), respectively. However, the findings of this study indicate the mechanical properties of the composite are due to the in situ formation of TiB₂ particles in the Cu matrix. The properties of the composites after heat treatment were discussed employing mechanical and electrical properties and measured ultimate tensile strength (UTS) (~375 MPa), yield strength (~300 MPa), and hardness (~150 Hv) for a higher percentage of Ti and B addition. The electrical conductivity also decreased to 53% IACS as Ti negatively impacts conductivity.