The primary objective of materials science is the study of the properties of the existing materials and the development of new ones. In the present day, the use of solid-state lasers abroad has prompted material scientists globally to develop novel or enhance the properties of the existing active gain media. Materials comprising rare earth elements have historically proven effective in scintillation applications. The synthesis of LaLu1-xYbxO3 monodisperse nanopowders with a particle size of 50–62 nm via the Pechini complexing citrate method has been the subject of investigation using electron paramagnetic resonance (EPR) spectroscopy and photoluminescence (PL) measurements. The EPR data indicate that the Yb³⁺ ions predominantly create a single type of center, whereby the Yb³⁺ ion substitutes for the Lu³⁺ ion. The calculated EPR g-factors are estimated to be g1 = 3.85, g2 = 2.15, g3 = 1.55 and the 171Yb isotope hyperfine interaction constants are A1 = 600 × 10−4 cm−1, A2 = 700 × 10−4 cm−1, A3 ≈ 1800 × 10−4 cm−1. The principal values of the g factors and the hyperfine tensors indicate that the Yb site in LaLu1-xYbxO3 nanopowders exhibits orthorhombic symmetry. The PL measurements in the wavelength range of 350–1800 nm, with excitation provided by either a xenon lamp or a diode laser, indicate the presence of a broad emission band, centered at 404 nm, in addition to the well-known emission spectrum in the IR region (920–1100 nm) arising from Yb3+ ions.
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