In this work, a facile route using a simple solvothermal reaction and sequential heat treatment process to prepare porous Y 2 O 3 microcubes is presented. The as-synthesized products were characterized by X-ray powder diffraction (XRD), scanning electronic microscope (SEM), energy dispersive spectrometer (EDS), thermogravimetric analysis (TG), and differential thermal analysis (DTA). The thermal decomposition process of the Y 2 O 3 precursor was investigated. SEM results demonstrated that the as-prepared porous Y 2 O 3 microcubes were with an average width of about 20 µm and thickness of about 8 µm. It was found that the morphology of the Y 2 O 3 precursor could be readily tuned by varying the molar ratio of 2 2 8 S O − to Y 3+ . Y 2 O 3 :Eu 3+ (6.6%) microcubes were also prepared and their photoluminescence properties were investigated.