In this paper, tricalcium disilicate was formed from dicalcium silicate compound powder, synthesised via a mechanochemical technique using a stoichiometric 2CaO:1SiO2. Compound CaO and SiO2 were derived from the bio-waste of eggshell and rice husk at the calcination temperature of 900oC and 800oC, respectively. The dicalcium disilicate powder was sintered for 2 hours at different temperatures ranging from 1150oC to 1350oC. Using X-ray diffraction with Rietveld analysis, it was found that the amount of tricalcium disilicate with monoclinic (beta) crystal structure increases on sintering temperature at the expense of dicalcium silicate. The complete formation of single-phase tricalcium disilicate began at a sintering temperature of 1300oC. The effect of sintering temperatures on the crystallisation and phase transition of dicalcium silicate is reported. The size of crystallites depends on the sintering temperature. The finding of this study rebound to the benefit of society by reducing the risk-off pollution cause by accessive redundant bio-waste eggshell and rice husk and also reduced the amount of CaO and SiO2 used in the fabrication of Ca3Si2O7
