This paper describes a novel approach for preparation of scandium glass microspheres by combining both melt-quenching technique and an indigenously developed microwave approach. The microspheres were characterized for morphology, elemental composition, crystallinity and change in physical/chemical properties with temperature. The size of the prepared microspheres was found to be ranging from 500 to 1500 µm. The obtained glass microspheres were irradiated with thermal neutrons in a nuclear reactor to produce ⁴⁶Sc radioisotope.