This Letter demonstrates a solvent-free efficient synthesis process to prepare self-assembled two-dimensional Eu 2 O 3 luminescent nanoplates to yield a superstructure. In the first step, Eu 2 O 2 CO 3 superstructures are fabricated by the thermolysis [700 °C] of a single precursor, europium acetate, in a closed reactor under autogenic pressure. The as-prepared Eu 2 O 2 CO 3 superstructures are further heated in air to 750 °C to facilitate the fabrication of Eu 2 O 3 superstructures. A systematic morphological, structural, and compositional characterization of Eu 2 O 3 superstructures is carried out. The photoluminescent properties and mechanism for the strong red emission of the photoexcited Eu 2 O 3 superstructures is proposed. SECTION Nanoparticles and Nanostructures