Sphene based glass-ceramics (CaTiSiO5), an excellent candidate for a host lattice of ceramic materials and for nuclear waste immobilization, has been prepared from a powder mixture of CaCO3, TiO2 and SiO2 using vibro-milling for homogenization. Starting powders were melted at 1400?C for 2 h, cooled to room temperature, grounded again, then crystallized by thermal treatment yielding a sphene glass-ceramic. The evolution of the phase composition during thermal treatment was investigated by X-ray powder diffraction (XRPD), FT-IR, Raman and thermal analyses (TG-DTA). Pure synthetic single phase sphene was formed at 800?C for 4 h, even it is very hard to obtain monophase powder at such low temperature. Powder morphology was analyzed by scanning electron microscopy (SEM).