<p>Apatitic calcium phosphates have a mineral phase close to that of bone and are commonly used as substitutes or fillers in bone surgery. Also, they are used for their excellent biocompatibility and bioactivity. The purpose of this study is to produce directly biphasic calcium phosphate (BCP) from calcium-deficient apatite (CDHA), by the hydrothermal process. The precursors used were calcium acetate (CH<sub>3</sub>COO)<sub>2 </sub>Ca, phosphoric acid (H<sub>3</sub>PO<sub>4</sub>) and triethylamine N (CH<sub>2</sub>CH<sub>3</sub>)<sub>3</sub>, the product was calcined at 900°C. The composition phase, morphology, particle size and the molecular structure of the product were studied using these techniques: X-Ray Diffraction techniques, Scanning Electron Microscopy (SEM), Transmission Electron Microscopy, Fourier Transforms Infrared spectroscopy (FT-IR ) to reveal its phase content, Inductively Coupled Plasma-Atomic Emission Spectrometers (ICP-AES), Thermogravimetric analysis, Thermo-Differentials (ATG / ATD). The results showed that the synthesized product is CDHA. It gives after calcination at 900°C, the biphasic calcium phosphate (a mixture of HA + β-TCP). The product is also found with a new percentage and high crystallinity and nanometric size.</p>