During the past few years, bioceramics, like hydroxyapatite and β-tricalcium phosphate have been widely developed for bone reconstruction. These materials have to meet strict criteria regarding biocompatibility, degradability, and mechanical properties. This work has been focusing on the influence of synthesis parameters on the production of calcium phosphate mixes, called biphasic calcium phosphate. In this optic, powders obtained from two synthesis processes (i. e. wet precipitation and sol-gel process) were produced. The influence of pH, Ca/P molar mixing ratio, and calcination temperature was studied. These new materials were characterized in terms of composition, thermal properties, and textural properties via X-ray diffraction, infrared spectroscopy, scanning electronic microscopy, thermogravimetric analysis, and nitrogen adsorption-desorption. Wet precipitation technique produces in situ mixes with different hydroxyapatite contents while the sol-gel process ends up with ceramics contaminated by cytotoxic CaO. Wet precipitation has been demonstrated more successful to control in situ mixes with specific composition.