Publication date: 15th December 2025
The efficiency and stability of photoelectrochemical (PEC) materials are governed by processes that occur at interfaces and surfaces, where atomic structure, electronic states, and chemical reactions meet. Disorder, local defects, and dynamic surface transformations strongly influence charge dynamics and transfer, often limiting performance under realistic operating conditions. At the same time, material stability is highly sensitive to nanoscale imperfections, which frequently initiate and accelerate degradation processes.
To reveal the impact and dominant role of nanoscale behavior on the macroscopic properties of PEC systems, operando techniques capable of probing interfacial structure and dynamics with nano- to micrometer resolution under realistic conditions are required. In this work, we employ nanoscale in-situ scanning probe microscopy to investigate the interfacial stability of TiO2/Pt photocathodes by directly monitoring localized surface transformations and detachment processes during operation. To tailor interfacial morphology, Pt catalysts were deposited onto conformal TiO2 coatings using sputtering and atomic layer deposition (ALD). Whereas sputtering produces a continuous Pt film, ALD forms discrete Pt nano-islands, enabling atom-efficient utilization of precious metals.
Under photoelectrochemical operation, both systems exhibit comparable onset potentials and saturation current densities; however, chronoamperometry reveals markedly improved long-term stability for the nanostructured ALD-Pt films. Specifically, we show that continuous Pt layers undergo delamination from the substrate, while ALD-Pt structures maintain their integrity. This contrasting behavior is attributed to distinct bubble formation and detachment processes at the catalyst–semiconductor interface.
These nanoscale insights highlight the importance of interfacial and morphological engineering, as well as the need to control dynamic conversion processes, to achieve durable and efficient PEC material systems.
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