Calcium phosphate-based bioceramics, mainly in the form of hydroxyapatite, Ca 10(PO 4) 6(OH) 2—HAP, is the main mineral constituent of teeth and bones with excellent biocompatibility with hard and muscle tissues. These materials exhibit several problems of handling and fabrication, which can be overcome by mixing them with a suitable binder. The dry milling process of fabrication of HAP presents the advantage that melting is not necessary and the powder obtained is nanocrystalline. The high efficiency of the dry milling process opens a new way to produce commercial amount of nanocrystalline HAP and others bioceramic. In this work dry mechanical alloying has been used to produce nanocrystalline powders of HAP using three different experimental procedures (HAPA: Ca(H 2PO 4) 2 + Ca(OH) 2; HAPB: Ca(H 2PO 4) 2 + CaCO 3; and HAPC: CaHPO 4 + CaCO 3). HAP was obtained after 5, 10 and 15 h of milling in the reactions HAPA and HAPB, but it is necessary 15 h of milling in the reaction HAPC to obtain HAP. In order to improve the mechanical properties of HAP calcium phosphate ceramics, with titanium (CaP-Ti) and zirconium (CaP-Zr), have been prepared by dry ball milling using two different experimental procedures: CaP-Ti1: Ca(H 2PO 4) 2 + TiO 2; CaP-Ti2: CaHPO 4 + TiO 2; and CaP-Zr1: Ca(H 2PO 4) 2 + ZrO 2, CaP-Zr2: CaHPO 4 + ZrO 2. The calcium titanium phosphate phase, CaTi 4P 6O 24, was obtained in the reaction CaP-Ti1. In the reactions CaP-Ti2, CaP-Zr1 and CaP-Zr2, it was not observed the formation of any calcium phosphate phase even after 15 h of dry mechanical alloying. The milled HAP and the ceramics systems obtained were characterized by X-ray powder diffraction, infrared and Raman scattering spectroscopy.