Nonequilibrium synthesis provides a powerful route to access metastable structural states that are inaccessible under near-equilibrium conditions, yet quantitative links between growth kinetics, defect structure, and functional response remain poorly understood. Here, we investigate the microwave-assisted synthesis of Eu3+- and Tb3+-doped Lu2O3 nanocrystals as a model system to elucidate how nonequilibrium crystallization kinetically encodes lattice microstrain and governs material properties. Time-resolved X-ray diffraction, transmission electron microscopy, and kinetic modeling reveal diffusion-controlled crystallite growth consistent with Ostwald ripening, accompanied by persistent microstrain that relaxes only partially with microwave irradiation time. Williamson–Hall analysis demonstrates that dopant chemistry systematically modulates the magnitude and evolution of microstrain, indicating a coupling between defect formation and mass transport under microwave heating. Photoluminescence spectroscopy shows that Eu3+ hypersensitive transitions and Eu–O charge-transfer states track microstrain directly, establishing lattice strain as an internal structural field that tunes local symmetry and electronic structure. In contrast, Tb3+ emission is primarily quenched by defect-mediated nonradiative processes, highlighting dopant-selective coupling to strain. These structure–optical correlations are mirrored in photocatalytic performance, where intermediate strain levels maximize activity by balancing internal electric fields and defect recombination. Together, these results demonstrate that microwave-assisted nonequilibrium synthesis enables the kinetic encoding of lattice microstrain, providing a general strategy to rationally design functional oxide nanomaterials through controlled growth pathways rather than composition alone.
Vasconcelos et al. (Mon,) studied this question.
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