This research details the synthesis and comprehensive characterization of two isostructural lanthanide metal-organic frameworks (Ln-MOFs), Tb₂BDC₃ and Er₂BDC₃, prepared using a cost-effective room-temperature stirring method. Post-synthetic ultrasonic treatment (for 5, 10, and 15 min) was applied to modulate their physicochemical and functional properties. For the Tb₂BDC₃ MOF, PXRD confirmed structural integrity while crystal size was successfully reduced from 66.42 nm to as low as 37.96 nm. SEM confirmed the preserved needle-like morphology, and EDX verified stable elemental composition. This size reduction significantly enhanced its luminescent properties, more than doubling the quantum yield from 27.59 % to over 57 % (reaching 58.73 % with 5 min of sonication) alongside a significant increase in emission intensity and lifetime. In contrast, the initial Er₂BDC₃ material was synthesized as a metastable two-phase mixture. While sonication promoted a shift toward the stable QACTUJ phase, stability studies revealed that exposure to biological media included a complete structural transformation into a single, stable crystalline phase (PXRD). This reorganization was supported by FTIR evidence of phosphate incorporation and corresponding changes in the UV-Vis-NIR absorption profile. Biological compatibility assessments (Alamar Blue) demonstrated that neither MOF induced cytotoxicity or inhibited HaCaT cells proliferation at concentrations up to 100 µg/mL. These multi-technique findings highlight the effectiveness of ultrasonic modification for tuning the optical properties of Ln-MOFs and underscore their robust stability and excellent biocompatibility, positioning them as promising candidates for a safe and effective platform in bio-imaging and sensing applications.
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