Three bimetallic Ni-Co (Ni:Co ratio 1:3, 1:1 and 3:1) and two monometallic (Ni and Co) nanoparticles supported on Al2O3 were synthesized by incipient wet impregnation and characterized by various technics (N2-physisorption, XRD, H2-TPR, CO-chemisorption and elemental analysis). It was demonstrated by XRD that NiCo alloys nanoparticles were present on bimetallic solids. The catalytic properties of all catalysts were determined for the hydrodeoxygenation of m-cresol at 340 °C under 4 MPa of total pressure. It was demonstrated that NiCo alloy developed better deoxygenation catalytic properties than pure Ni metallic phase, these properties being evaluated both by the total reaction rate (kTOT) and the selectivity into deoxygenation products. Indeed, bimetallic NiCo(3:1)/Al2O3 was 1.2 times more active than Ni/Al2O3 and 8.8 times than Co/Al2O3, deoxygenated products being favored on bimetallic catalysts compared to Ni one. In addition, the kTOT values seems to be related to the amount of CO uptakes, indicating that active sites in HDO were of similar nature than those allowing the adsorption of CO, and could be oxygen vacancies which were promoted in bimetallic NiCo particles.