Dicalcium silicate (Ca₂ SiO₄) has been reported as an interesting candidate for biomaterials use due to its attractive bioactive properties. Here, we report on how dicalcium silicate was prepared by a sol-gel route using calcium nitrate tetrahydrate and tetraorthosilicate as the precursors chemicals for CaO and SiO₂ , respectively. The synthesized powders were characterized using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) method, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). High purity dicalcium silicate at a CaO/SiO₂ molar ratio of 2:1 could be formed by the sol-gel method without a washing process and was then calcined at 800°C. The effects of the molar ratio of CaO/SiO₂ , the washing process, and the calcination temperature have been shown to affect the purity, the formation, and the particle size of the nanoparticles, which have been investigated and discussed.