Designing efficient and stable water splitting photocatalysts is an intriguing challenge for energy conversion systems. We report on the optimal fabrication of perfectly aligned nanotubes on trimetallic Ti–Mo–Fe alloy with different compositions prepared via the combination of metallurgical control and facile electrochemical anodization in organic media. The X-ray diffraction (XRD) patterns revealed the presence of composite oxides of anatase TiO2 and magnetite Fe3O4 with better stability and crystallinity. With the optimal alloy composition Ti–(5.0 atom %) Mo–(5.0 atom %) Fe anodized for 16 h, enhanced conductivity, improved photocatalytic performance, and remarkable stability were achieved in comparison with Ti–(3.0 atom %) Mo–(1.0 atom %) Fe samples. Such optimized nanotube films attained an enhanced photocatalytic activity of ∼0.272 mA/cm2 at 0.9 VSCE, which is approximately 4 times compared to the bare TiO2 nanotubes fabricated under the same conditions (∼0.041 mA/cm2 at 0.9 VSCE). That was mainly correlated with the emergence of Mo and Fe impurities within the lattice, providing excess charge carriers. Meanwhile, the nanotubes showed outstanding stability with a longer electron lifetime. Moreover, carrier density variations, lower charge transfer resistance, and charge carriers dynamics features were demonstrated via the Mott–Schottky and electrochemical impedance analyses.

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A significant effort has been dedicated to the synthesis of Cu–Zn oxide nanoparticles as a robust photocathode material for photoelectrochemical water splitting. Cu–Zn oxide nanoparticles were formed by controlled anodization of German silver (Cu–Zn–Ni) alloy in an aqueous electrolyte. Scanning electron microscopy (SEM) demonstrates the dependence of the obtained nanostructures on the anodization time. The X-ray diffraction (XRD) patterns showed the formation of copper oxide (CuO) and zinc oxide (ZnO) nanoparticles with good stability. This was also confirmed by the compositional X-ray photoelectron spectroscopy (XPS) analysis. The obtained polyhedral nanoparticles showed high optical activity with adequate bandgap energy. These optimized nanoparticles achieved boosted photocurrent of − 0.55 mA/cm2 at − 0.6 V vs. SCE under AM 1.5 illumination, confirming the role of the optimized dealloying and thermal treatment in tuning the photoelectrochemical performance of the material.

Photoelectrochemical water splitting is a promising route to realizing a clean energy economy. Herein, we report on the ability to selectively fabricate optimized Ni-doped brookite nanotube array films on fluorine-doped tin oxide (FTO) substrate using ultrarapid radio frequency sputtering followed by electrochemical anodization and thermal annealing under ambient air. Ni doping promotes photocatalytic performance by introducing impurity bands within the TiO 2 bandgap. Further, annealing at various temperatures helps to tune the photoactivity of the fabricated photoelectrodes, which is in agreement with the nature of the trap states. The nanotubes enjoy high crystallinity and enhanced photoresponse with a noticeable bandgap of 2.7 eV. The Mott−Schottky analysis reveals the variation in the charge carriers density of the fabricated nanotubes. Most importantly, the electrochemical impedance spectroscopy (EIS) analysis unravels the involved kinetics and helps to determine the charge transfer properties of the annealed nanotubular films under opencircuit voltage (OCV) and with applied potential under dark and illumination conditions. EIS analysis reveals decreased charge transfer resistance under illumination, in agreement with the obtained photocurrent, electron lifetime, and density of trap states.