β-tricalcium phosphate (β-TCP) is a widely studied calcium phosphate phase because of its well-defined crystal structure and its capacity for ionic substitution within the lattice, which enables tailoring of functional properties. In this work, β-TCP powders were synthesized through a controlled precipitation route and subsequently modified by partially substituting Ca²⁺ with Zn²⁺ to investigate the effect of Zn incorporation on phase formation, structural evolution, and microstructural features. Phase purity and successful formation of β-TCP, together with the absence of detectable secondary phases, were confirmed by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and thermal analysis. The results indicate that Zn²⁺ substitution produces distinct, quantifiable changes in diffraction characteristics consistent with lattice modification, while also promoting higher crystallinity. SEM observations further reveal improved microstructural uniformity and more homogeneous particle morphology for Zn-containing powders compared with unsubstituted β-TCP. Overall, these findings demonstrate that controlled Zn²⁺ incorporation is an effective strategy to tune the structural and physicochemical characteristics of β-TCP powders, providing a promising basis for designing compositionally optimized calcium phosphate materials.