Anodized TiO2 Nanotubes Sensitized with Selenium Doped CdS Nanoparticles for Solar Water Splitting

In this research, TiO2 nanotubes (NTs) were produced by electrochemical anodization of a Ti substrate where different NH4F wt.% in the electrolyte was added. NTs with diameter of 65–90 nm and 3.3–4.9 µm length were obtained and sensitized with binary cadmium chalcogenides nanoparticles, CdS and CdSe, by successive ionic layer adsorption and reaction method (SILAR). Additionally, both anions S and Se were deposited onto Cd, labeled as CdSSe and CdSeS, to evaluate the effect of the deposition order of the anion from the precursor solution to form cadmium chalcogenides. The structural, optical, and electrochemical performance were analyzed through the SEM, XRD, XPS, UV-VIS, lineal voltammetry and chronoamperometry characterizations. The increase of NH4F wt.% from 1.5% to 4.5% produced a decrement of the diameter and length attributed to the fluoride ions concentration causing solubility of the NTs. XRD confirmed the TiO2 anatase and hexagonal CdS structures. From the EDS and XPS results, the presence of small amount of Se in the sensitized samples demonstrated the doping effect of Se instead of forming ternary semiconductor. With the sensitization of the TiO2 NTs with the nanoparticles, an improved hydrogen generation was observed (reaching 1.068 mL h−1 cm−2) in the sample with CdSSe. The improvement was associated to a synergetic effect in the light absorption and higher cadmium chalcogenide amount deposited when sulfur ions were deposited before selenium.