CaGd3F11:Eu3+ nanocrystals with the morphologies of nanoparticles were prepared by octylamine and oleic acid as capping ligands, and anhydrous calcium chloride, rare earth nitrate, n-octanol as the raw materials with solvothermal method. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and fluorescence spectrophotometer. The results indicate that CaGd3F11 nanocrystals are well-crystallized and their sizes are uniform (about 5 nm). As a luminescence host, it shows higher emitting intensity with Eu3+ doping.