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The present paper reports the synthesis, characterization and photoluminescence (PL) studies of MgO:Dy3+ nanoparticles. In this work, MgO:Dy3+ nanophosphors were prepared through solution combustion synthesis method using magnesium nitrate as oxidizer and urea as a fuel. The as-obtained MgO:Dy3+ nanomaterials were characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) analysis, Fourier transformation infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), high resolution transmission electron microscope (HRTEM), photoluminescence (PL) spectra and afterglow curve analysis. The cubic structure of the MgO phosphors is confrmed by XRD analysis and crystalline size calculated by Scherer’s formula using XRD data shows the nanocrystalline nature of the phosphor. No phase change is observed with increasing concentrations of Dy3+ ions. The surface morphology of the prepared phosphors is determined by SEM, which shows a sphere-like structure and good connectivity of the grains. The confrmation of the nanocrystalline phosphors is examined by HRTEM analysis.The photoluminescence studies revealed that the emission spectra of the prepared phosphors shows the broad emission centered at 435 nm and 480 nm due to the transition arises from the 4f→5d defect band transition of Dy3+ ions. The afterglow decay characteristics of different as synthesized MgO:Dy3+ nanophosphors are conceptually described. This is the first reported that on the synthesis of nanocrystalline MgO:Dy3+ materials by combustion method using urea as a fuel.