Effective control of calcium carbonate (CaCO₃) scale formation is crucial to improve the performance and economic efficiency of water systems. This study investigates the impact of various scale inhibitors on the nucleation and crystallization processes of CaCO₃. Calcium carbonate particles were synthesized by mixing CaCl₂·2H₂O and NaHCO₃ solutions, in the presence of various scale inhibitors that had not previously been investigated using the experimental techniques employed in this study. Particle size distribution and zeta potential were analyzed using dynamic light scattering (DLS), while Ca⁺² consumption and pH changes were monitored with ion-selective electrodes. Crystal morphology was evaluated using scanning electron microscopy (SEM) and cryo-transmission electron microscopy (cryo-TEM). We demonstrated that, in all samples, approximately 98% of the CaCO₃ particles (sized between 400 and 840 nm) are formed within the first 30 min of synthesis, and these particles then aggregate to form larger particles (840–1100 nm in size). Due to the solution’s high supersaturation, the inhibitors influence calcium consumption only after 5 min of synthesis. All inhibitors, especially DTPMP, decrease calcium consumption and particle size during synthesis. The zeta potential and morphology of the particles in the samples containing inhibitors differed from those in the control group. Cryo-TEM observations revealed distinct nanometric precursor phases in the calcite crystallization process without inhibitors and different nanostructures when scale inhibitors were used. Moreover, conchoidal fractures were observed in the nanoparticles formed in the presence of DTPMP. This study demonstrates the effectiveness of various inhibitors in reducing calcium consumption in solution and altering the morphology of CaCO₃ crystals, thereby preventing calcium carbonate (CaCO₃) scale formation.