Dy3+, Nd3+, Sm3+ doped Y2O3 nanophosphors were produced with high homogeneity at low sintering temperature using the sol-gel method. To compare the structural and optical changes of different rare-earth ions included in the crystal lattice, the dopant ratio was chosen as constant 2 mol%. In the light of X-ray diffraction (XRD) analysis, the unit cell volume and average crystallite size of the doped nanophosphors and their pure Y2O3 sintered under the same heat treatment regime were calculated and compared. Scanning electron microscopy (SEM) techniques were used to describe their structures and morphologies; an average particle size histogram of nanostructures was generated. The Radioluminescence (RL) spectra of Y2O3:Ln3+ (Ln: Dy, Nd, Sm) nanophosphors were presented for the first time. Splittings were seen in detail in the emission spectra given the 200–1100 nm range. For Dy3+4F9/2 → 6H13/2, for Nd3+; in the visible region 4H11/2-4I9/2 in the NIR region 4F3/2-4I9/2, for Sm3+; in the visible region 4G5/2-6H7/2 in the NIR region 4G5/2-6F5/2 transitions were determined to have the most vigorous emission. It was observed that the optical band gap calculated from the absorption spectrum of Y2O3 was 4.97 eV; this value changed the most with Dy contribution and decreased to 4.77 eV. The thermoluminescence (TL) behaviors of nanophosphors were compared under both UV and X-ray excitation. The kinetic parameters were calculated by applying computerized glow curve deconvolution (CGDC), and various heating rate (VHR) methods to the glow curves obtained UV excitation. The obtained E (eV) values correlated with each other are highly compatible.
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