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Mg/Al/Ln (Ln = Nd, Sm, Eu) layered double hydroxides (LDHs) were synthesized using sol-gel method for the first time to the best our knowledge. The obtained materials were characterized by X-ray diffraction analysis and fluorescence spectroscopy. The phase composition and luminescent properties of these LDHs were investigated and discussed. The Ln³⁺ substitution effects were investigated in the Mg₃Al_{1-x}Ln_{x} LDHs by changing the Ln³⁺ concentration in the metal cation layers up to 10 mol%. It was demonstrated that only Mg₃Al_{1-x}Eu_{x} LDHs showed luminescence properties, however, no any light emission was observed for the Mg₃Al_{1-x}Nd_{x} and Mg₃Al_{1-x}Sm_{x} LDH samples.
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