Nickel nanopillar arrays were electrodeposited onto silicon substrates using porous alumina membranes as a template. The characterization of the samples was done by scanning electron microscopy, X-ray diffraction, and alternating force gradient magnetometry. Ni nanostructures were directly grown on Si by galvanostatic and potentiostatic electrodeposition techniques in three remarkable charge transfer configurations. Differences in the growth mechanisms of the nanopillars were observed, depending on the deposition method. A high correlation between the height of the nanopillars and the charge synthesis was observed irrespective of the electrochemical technique. The magnetization measurements demonstrated a main dependence with the height of the nanopillars. The synthesis of Ni nanosystems with a controllable aspect ratio provides an effective way to produce well-ordered networks for wide scientific applications.

Nowadays, green hydrogen is an important niche of interest in which the search for a suitable composite material is indispensable. In this sense, titanium oxide nanotubes (TiO₂ nanotube, TNTs) were prepared from double anodic oxidation of Ti foil in ethylene glycol electrolyte. The morphology of the nanotubes was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Once characterized, nanotubes were used as templates for the deposition of hematite. The use of three synthetic procedures was assayed: Chemical Vapor Deposition (CVD), Successive Ionic Layer Adsorption and Reaction (SILAR), and electrochemical synthesis. In the first case, CVD, the deposition of hematite onto TiO₂ yielded an uncovered substrate with the oxide and a negative shift of the flat band potential. On the other hand, the SILAR method yielded a considerable amount of hematite on the surface of nanotubes, leading to an obstruction of the tubes in most cases. Finally, with the electrochemical synthesis, the composite material obtained showed great control of the deposition, including the inner surface of the TNT. In addition, the impedance characterization showed a negative shift, indicating the changes of the interface electrode–electrolyte due to the modification with hematite. Finally, the screening of the methods showed the electrochemical synthesis as the best protocol for the desired material.