Novel fluorescent Eu-containing layered double hydroxides (Eu-LDHs) were prepared by direct ion-exchange of EuMgAl-NO 3 LDHs precursors with MoO42− anions. The samples were characterized by elemental analyses, powder X-ray diffraction (XRD), Fourier transform infrared (FT–IR), Raman spectra, photoluminescence spectroscopy. The results indicated that Eu 3+ ions were likely incorporated into the hydrotalcite lattice and MoO42− anions were successfully intercalated into interlayer region of the LDHs with the Mo/Al molar ratio close to 0.40. The luminescence properties were largely enhanced compared with the EuMgAl-NO 3 LDHs precursors, which were attributed to the energy transfer between Eu 3+ and MoO42−.