controlled electrical conductivity. The insulating nature of the diamond phase precluded the use of diamond in electro chemistry, and at that time conductivity could be induced in diamond films only by ion implantation. However, as indi cated by the first report [1] the results were not satisfactory because of the structural damages produced by the ions in the dia mond lattice. After the pioneering works by Derjaguin et al., [2] Varnin et al., [3] and Spitsyn et al., [4] the beginning of the "diamond electrochemistry" era started with the settling up and developing of chemical vapor deposition (CVD) metho dologies and the definition of protocols for the growth of the diamond phase under conditions far from the thermo dynamic equilibrium.The feasibility of doping the growing diamond lattice during CVD processes stimulated the development of efficient routes for the realization of highquality, robust, and wearresistant new type of carbon electrodes, to be used for the entire range of the electrochemical applications, from oxidation/reduction reactions, to qualitative and quantitative electroanalysis, to power generation and storage. [5] During the last decades the general trend was to use boron as dopant of diamond. Borondoped diamond (BDD) consti tutes certainly the more common class of conductive diamonds, due to the wellestablished ptype semiconductor behavior and the interesting electrochemical properties of such hybrid system. [6][7][8] However, there are several criticalities related to the use of B to dope CVD diamond layers. First, whereas resistivity of about 10 −3 Ω cm can be achieved with B concentrations up to 10 21 cm −3 , [9] the electrical properties of such structures are dom inated by impurity band conduction with a low mobility that degrades the conducting behavior of the material. [10] Another criticality is related to the high toxicity of boron and to the con sequent limitations in the use of Bdoped electrodes in applica tions requiring biocompatibility.Several other elements such as N, P, Na, Li, Ti, W, and Nd have been proposed as dopants to induce in diamonds a con ductive or semiconductive behavior and to match specific tech nological requirements. [5] A hybrid chemical vapor deposition (CVD)-powder flowing technique specifically developed in lab has been employed to produce high-quality polycrystalline diamond layers containing Ti inclusions. Morphology, structural features, and surface composition of nanocomposite diamond-based samples produced by different growth times have been analyzed by scanning electron microscopy, Raman and Auger spectroscopy, respectively. The CVD methodology adopted for the Ti incorporation in the diamond lattice does not perturb the crystalline quality of the diamond matrix, therefore maintaining the outstanding properties of the C-sp 3 phase. The functional properties of the nanocomposite layers have been tested by nanoindentation and I-V measurements. The electrochemical performance of the diamond/Ti electrodes is evaluated by performing cyclic voltammetry in ...