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Nanostructured α-Fe2O3 thin film electrodes were deposited by aerosol assisted chemical vapour deposition (AACVD) for photoelectrochemical (PEC) water splitting on conducting glass substrates using 0.1M methanolic solution of Fe(acac)3. The XRD analysis confirmed that the films are highly crystalline α-Fe2O3 and free from other iron oxide phases. The highly reproducible electrodes have optical bandgap of ~2.15 eV and exhibit anodic photocurrent. The current-voltage characterization of the electrodes reveals that the photocurrent density strongly dependend on films morphology and deposition temperature. The SEM analysis showed a change in the surface morphology with the change in deposition temperature. The films deposited at 450 °C have nanoporous structures which provide maximum electrode/electrolyte interface. The maximum photocurrent density of 455 μA/cm 2 was acheived at 0.25V vs. Ag/AgCl/3M KCl (~ 1.23 V vs. RHE) and IPCE of 23.6% at 350 nm for the electrode deposited at 450 °C.

Electrofabricated p-Co3O4 based electrodes have shown efficient photoelectrochemical performance at low bias potentials in aqueous medium (∼6.5 mA cm−2vs. SCE at −0.3 V).

High demand and current applications have led to continuous study and subsequent improvement of TiO 2 nanoparticles. The versatility of the sol-gel method allows employing different process parameters to influence the resultant properties of TiO 2 nanoparticles. The evaluation and characterisation process of the synthesised TiO 2 nanoparticles commonly involves a series of methods and techniques. Such characterisation methods include phase, structural, morphology and size analysis. A combination of data from these evaluations provides the relationship between the synthesis parameters and the end properties of TiO 2 nanoparticles. Apart from the research findings on TiO 2 nanoparticles, the characterisation used to obtain these findings is equally important. Thus, this chapter highlights the recent characterisation techniques and practices employed for TiO 2 nanoparticles synthesised by the sol-gel method.