We first synthesized gadolinium oxide (Gd2O3) by a modified “polyol” strategy and then embedded it into mesoporous silica by a simple self-assembly sol-gel reaction. Scanning electron microscope (SEM) results show that the samples have good sphericity and good dispersibility. The structure of mesoporous silica was characterized by transmission electron microscopy (TEM) and small-angle X-ray diffraction (SAXRD). Results show that the mesoporous structure has not been destroyed after gadolinium oxide imbedding. The ratio of gadolinium and silica was determined by the mean of energy dispersive spectroscopy (EDS).