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(Photo)electrocatalysts capture sunlight and use it to drive chemicalreactions such as water splitting to produce H2. A major factor limitingphotocatalyst development is their large heterogeneity which spatiallymodulates reactivity and precludes establishing robust structure-functionrelationships. To make such links requires simultaneously probing of theelectrochemical environment at microscopic length scales (nm to um) and broadtimescales (ns to s). Here, we address this challenge by developing andapplying in-situ steady-state and transient optical microscopies to directlymap and correlate local electrochemical activity with hole lifetimes, oxygenvacancy concentration and the photoelectrodes crystal structure. Using thiscombined approach alongside spatially resolved X-Ray absorption measurements,we study microstructural and point defects in prototypical hematite (Fe2O3)photoanodes. We demonstrate that regions of Fe2O3, adjacent to microstructuralcracks have a better photoelectrochemical response and reduced back electronrecombination due to an optimal oxide vacancy concentration, with the filmthickness and carbon impurities also dramatically influencing activity in acomplex manner. Our work highlights the importance of microscopic mapping tounderstand activity and the impact of defects in even, seemingly, homogeneoussolid-state metal oxide photoelectrodes.

Correlating activity and defects in (photo)electrocatalysts using in-situ transient optical microscopy