Hydrotalcite nanocrystals doped with Eu(III) ions were prepared by the microemulsion method. XRPD measurements revealed that europium ions are very likely incorporated in a low-symmetry hydrotalcite-type layer. TEM and AFM imaging indicated that nanocrystals have a 150 nm width and a plate shape. Luminescence measurements showed that the doped powder is luminescent and the Eu(III) ions are located in a low symmetry site.