Investigating the Impact of the Calcination Temperature on the Structural Properties and Composition of NaMgF 3 NPs

ABSTRACT NaMgF 3 nanoparticles were successfully synthesized via a co‐precipitation method and calcined at 500–700°C for different durations to investigate the influence of thermal treatment on their structural and compositional properties. XRD confirmed a stable single‐phase orthorhombic NaMgF 3 structure under all conditions. Increasing the calcination temperature resulted in crystallite coarsening from 34.1 to 39.8 nm, while prolonged treatment at 700°C (12 h) further enhanced grain growth up to 46.7 nm, accompanied by a significant reduction in microstrain (from 0.33% to 0.25%) and dislocation density (from 0.73 to 0.52 × 10 −3 nm −2 ), indicating defect annealing and lattice relaxation. XPS revealed temperature‐dependent shifts in Na 1s, Mg 1s and F 1s binding energies, suggesting stabilization of cation coordination environments and reduction in surface defects. EDS and XPS confirmed stoichiometric composition with good agreement to the theoretical NaMgF 3 ratio. These findings demonstrate that calcination plays a critical role in tuning the structural integrity, defect distribution, and chemical stability of NaMgF 3 nanoparticles, which is essential for their integration in radiation detection, dielectric, and optoelectronic applications.