HA (Ca10(PO4)6(OH)2), (HA) – based biomaterials are used as medical implants to repair and reconstruct diseased or damaged hard tissues of the body. However, HA has low fracture strength therefore a second phase reinforcement is required to achieve the necessary mechanical strength to support high loads [1]. Titania (TiO2) addition to hydroxyapatite leads to the formation of a composite with improved mechanical properties and high biocompatibility, serving to enhance cell vitality [2]. The aim of this work was to develop TiO2/HA based biocomposites starting from titanium hydride (TiH2) and commercial HA (Aldrich) ( HA : TiH2 = 3 :1 ratio) by powder metallurgy technology. Further, two-step sintering (TSS) method [3] was used to obtain high density and nanoparticles simultaneously. TiO2/HA composites were structurally and morphologically characterized by X-ray diffraction and scanning electron microscopy (SEM). Functional groups of the HA – TiH2 mixture heated up to different temperatures have been investigated by Fourier Transform Infrared Analysis (FT-IR). Crystallinity degree and quantitative assessment of the PO43- and OH- substitution byCO32- from the deconvoluted Raman spectra of the studied samples were reported. The reactions between HA and TiH2 at sintering were investigated by simultaneous high temperature thermogravimetry coupled with differential scanning calorimetry (TG-DSC) in order to study the reaction mechanism of the TiO2/HA formation. TiH2 decomposition heat of 73.3 kJ·mol-1 obtained in this work is within the values reported in literature, 67 kJ·mol-1 [4] and 136 kJ·mol-1 [5]. TiO2/HA nanocomposite with specific properties for applications in tissue engineering such as, a densified nanostructure, high stability of HA component and superior wear resitance, was obtained.