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This paper reports an original nonstandard green concept to obtain TiO 2  microrods with polyhedral densely stacked 3D nanovoids prepared via the heat treatment of a hydrogen titanate. The intermediate hydrogen titanate was synthesized by a solid-liquid-solid (SLS) route from an ammonia-saturated aqueous solution of TiOSO 4  at 0 °C. The effect of the postgrowth thermal annealing procedure to remove ice (water) and the proposed mechanism to explain the underlying transitions from the intermediate precursor to nanostructured TiO 2  microrods with stacked 3D nanovoids were investigated. The small-angle X-ray scattering (SAXS) analysis indicates that at temperatures above 500 °C, the release of confined ice (water) takes place, which leads to the creation of self-assembled polyhedral nanovoids open to the surface. Their size ranges from 5 to 78 nm in both length and width, with a depth of ~3.88 nm. The first use of these stacked 1D TiO 2  microrods as the working electrode in a photoelectrochemical (PEC) cell for water splitting is demonstrated. The estimated value of ζ-potential depends on both annealing temperature and crystallite size. Anatase sample 1D TiO/800 with ζ-potential (−29.1) mV and average crystallite size ~68 nm was observed to be highly stable in aqueous suspension. The SLS method yields low-cost 1D TiO 2  materials possessing high photoreactivity with water. The PEC measurements indicate that three-dimensional hollow structures with a controlled geometry via patterned 1D TiO 2  surface are promising materials for hydrogen generation from water splitting.

TiO 2 microrods with stacked 3D nanovoids for photoelectrochemical water splitting