Scandium fluoride (ScF3) belongs to one of the rare compounds which exhibit isotropic negative thermal expansion. Here, a facile and environmentally friendly hydrothermal synthesis method has been presented. High-quality single-crystalline ScF3 cubes, with an average size of 200nm, can be easily fabricated in a large scale. Sc(NO3)(3) and NH4HF2 were used as precursors. The as-prepared ScF3 demonstrates cubic symmetry (Pm-3m), which was confirmed by X-ray diffraction and selected-area electron diffraction. Its uniform morphology and size were characterized by high-resolution transmission electron microscopy. Furthermore, thermal analysis was also performed in argon gas atmosphere to investigate its thermal stability.