Biphase composites of hydroxyapatite (HA) and β-tricalcium phosphate (TCP) with various phase compositions have been obtained by controlling the molar ratio of Ca(HPO 4 ).2H 2 O and CaCO 3 at an appropriate value between 1.5 and 2.0. In this work, biphase composites of HA and β-TCP with various phase compositions were prepared from the uncalcined Ca(H 2 PO 4 ) 2 .H 2 O and CaCO 3 mixtures. The thermal properties of uncalcined raw materials were investigated using DTA/DSC/TG. The kinetic parameters of dehydration and decomposition for uncalcined Ca(H 2 PO 4 ) 2 .H 2 O/CaCO 3 mixtures were also evaluated by non-isothermal differential thermal analysis (DTA) techniques.