Publication date: 15th December 2025
Photoelectrocatalytic (PEC) water-splitting offers a promising pathway for sustainable hydrogen production using solar energy [1]. Among the various photoanode materials studied, bismuth vanadate (BiVO₄) has emerged as leading candidate due to its suitable band gap, earth-abundance, and photostability [2] [3]. Mechanistically, BiVO₄ facilitates the oxygen evolution reaction (OER), PEC water-splitting’s bottleneck, through surface-adsorbed intermediates, where surface states and charge carrier dynamics play critical roles [4].
Spin coating has gained notoriety as a synthesis method for BiVO₄ photoelectrodes as it allows for the simple production of uniform thin films onto the conductive glass substrate from metal–organic precursor solutions. After deposition on conductive substrates, a further annealing step induces crystallization and improves adhesion.[5] In comparison, techniques such as spray pyrolysis, electrodeposition, sol–gel dipping, and hydrothermal growth can lead to higher surface areas or thicker films but often involve complex processing or morphology control.[6]
The present work focuses on the optimization of the catalytic activity of the BiVO₄ spin-coated photoanodes towards OER photoelectrocatalysis. We have implemented Design of experiment (DOE) tools to identify the optimal experimental procedures from the chosen input variables: 500, 1000 or 1500 rotations per minute; 3, 6 or 9 number of layers deposited; 10, 12 or 14 seconds of spinning and 0.04 or 0.08 M acidic organic precursor solution concentration.
As feedback for the DOE modelling, we used the obtained photoelectrocatalytic results (mA/cm2 at E = 1.23 V vs RHE) as the output variable to maximize, and find the corresponding optimal conditions for the photoanode synthesis. The PEC testing was done in a photoelectrochemical cell, in a three-electrode system, employing 0.1 M phosphate buffer solution at pH = 7.4 as electrolyte, under 100 mW AM 1.5G illumination. The morphological analysis of the samples was done by SEM imaging.
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