| Summary: | Synthesis of Ni- and N-doped Titania Nanotube Arrays (Ni-N-TiNTAs) was conducted to produce photocatalysts for hydrogen production from a glycerol–water mixture. Ni-N-TiNTAs were synthesized in two steps, namely anodization and chemical reduction. Ti foil was anodized at 50 V for two h in an electrolyte solution containing 0.2% urea as a source of N atoms. Ni doping (at various content of 5%, 10%, 15%, and 20% wt) was performed by one-hour chemical reduction with sodium borohydride as a reducing agent. The photocatalyst was annealed at different temperatures, i.e., 500 °C, 550 °C, and 600 °C under 60 mL/min N<sub>2</sub> gas for two h. On the basis of X-ray Diffraction (XRD) patterns, Ni-N-TiNTAs are mostly of anatase crystallite phase when annealed at 500 °C and 550 °C, while that of rutile was observable when calcination was done at 600 °C. The morphology of the photocatalysts was scrutinized by means of Field Emission Scanning Electron Microscopy (FESEM) imaging, which reveals nanotubular structures, with elemental composition measured by Energy Dispersive X-ray (EDX). The bandgap of the photocatalysts was analyzed using Ultraviolet Diffuse Reflectance Spectroscopy (UV DRS), which showed a lower value for the case of Ni-N-TiNTAs as compared to those of TiNTAs and N-TiNTAs. Photocatalytic tests showed that the highest amount of hydrogen produced (ca. 30973 μmol/m<sup>2</sup>) was obtained in the case of Ni-N-TiNTAs with a Ni content of 10wt%.
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