A uranyl–europium heterobimetallic compound, (TEA)₃[(UO₂)₆Eu(H₂O)₄(PPA)₆] (H₃PPA = phosphonoacetic acid, TEA = tetraethylammonium cation), was synthesized under mild hydrothermal conditions. The emission spectrum contains characteristic electronic transition features of both Eu³⁺ and UO₂²⁺, while the peak intensity of Eu³⁺ is notably higher than that of UO₂²⁺. This is primarily attributed to the energy transfer from uranyl to europium in the structure. Significantly, a positive correlation between the Eu³⁺ peak intensity at 621 nm and the D₂O content can be established in the aqueous system, while the uranyl peak intensity is almost unchanged, allowing for the full-range ratiometric detection of D₂O in H₂O.