ABSTRACT: Nano-carbon reinforced titanium matrix/hydroxyapatite (HA) biocomposites were successfully prepared by spark plasma sintering (SPS). The microstructure, mechanical properties, biocompatibility, and the relationship between microstructure and properties of biocomposites were systematically investigated. Results showed there are some new phases in sintered composites, such as ?-Ti, TiO?, ZrO?, etc. Moreover, a small amount of Ti17P10, CaTiO?, Ca?(PO?)? were also detected. The reaction that may occur during the preparation process is suppressed to some extent, which is because that the addition of second phases can prevent the direct contact of titanium with HA and reduce the contact areas. Transmission electron microscope (TEM) analysis proved the existence of elemental diffusion and chemical reactions in sintered composites. Compared with results of composites prepared by hot-pressed sintering before, mechanical properties (microhardness, compressive strength, and shear strength) of 0.5-GNFs composites prepared by SPS were increased by about 2.8, 4.8, and 4.1 times, respectively. The better mechanical properties of 0.5-GNFs composite in nano-carbon reinforced composites are mainly due to the lower degree of agglomeration of tubular carbon nanotubes (CNTs) compared to lamellar graphene nanoflakes (GNFs). Moreover, the strengthening and toughening mechanisms of nano-carbon reinforced titanium alloy/HA biocomposite prepared by spark plasma sintering (SPS) mainly included second phase strengthening, grain refinement strengthening, solution strengthening, graphene extraction, carbon nanotubes bridging, crack tail stripping, etc. In addition, in vitro bioactivity test revealed that the addition of nano-carbon was beneficial to promote the adhesion and proliferation of cells on the surface of titanium alloy/HA composite, because nano-carbon can enhance the formation of mineralized necks in the composites after transplantation, stimulate biomineralization and promote bone regeneration.