The use of carbon materials (graphene, multiwall carbon nanotubes, and fullerene) as templates for comparative electrodeposition of Ni-Co nanostructures is described. Operating conditions and parameters were found to influence in a challenging manner the morphology and electrochemical activity of the electrodeposited Ni-Co nanoparticles. The electrocatalytic properties of Ni-Co/carbon material-modified electrode toward the glucose oxidation were analyzed via cyclic voltammetry and amperometry. The studies showed that Ni-Co/MWNT electrode displayed the highest electrocatalytic activity, attributed to the high density of Ni-Co nanoparticles deposited on the carbon nanotubes support. A low detection limit of 1.8 mu M glucose with a good sensitivity of 1868 A mu A mM(-1) cm(-2) was obtained for electrochemical detection at Ni-Co deposited on MWNT.