This study explores the influence of various precursors including ammonium metatungstate (AMT) and peroxotungstic acid (PTA) in water, and tungsten hexachloride (WCl6 in MeOH or EtOH), as well as the role of ammonium chloride incorporation on the structural, morphological, and photoelectrochemical characteristics of WO3 layers synthesized by spray pyrolysis. X-ray diffraction (XRD) analysis revealed that films annealed at 550 °C crystallized in the monoclinic phase of WO3 with a polycrystalline structure without amorphous parts. Different morphological features of the samples were identified by scanning electron microscopy (SEM): dense grains for films formed using PTA, aggregated grains for films synthesized from AMT, smooth and uniform surfaces for films based on WCl6, and porous architectures resulting from NH4Cl incorporation. Photoelectrochemical measurements under UV and simulated solar illumination demonstrated that AMT/NH4Cl - derived WO3 films significantly enhanced the initial photocurrent density, reaching values of up to ∼3 mA cm-2 under UV light. Topological energy dispersive spectroscopy (EDS) revealed the existence of Cl rich areas responsible for this effect. With prolonged exposition to light and bias, Cl in these areas was oxidatively exhausted and average current densities as in samples obtained with other precursors were obtained. These findings highlight the critical role of precursor selection and doping in determining the photoelectrochemical performance of spray-deposited WO3 photoanodes.

Department of Inorganic Technology University of Chemistry and Technology Prague Technická 5 166 28 Prague 6 Czech Republic

J Heyrovský Institute of Physical Chemistry Czech Academy of Sciences Dolejškova 2155 3 182 23 Prague 8 Czech Republic

Molecular and Fluorescence Spectroscopy Lab Central Laboratories Network National Research Centre 12622 Dokki Giza Egypt

Solid State Physics Department National Research Centre 12622 Dokki Giza Egypt

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