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Nanostructuring photocatalytic and catalytic materials substantially increases the surface‐to‐volume ratio, thereby exposing a greater number of active sites essential for enhanced catalytic efficiency. However, optimizing these efficiencies requires the non‐destructive,operandointerrogation of individual nanocrystals under realistic catalytic conditions—a capability that has long remained elusive. Here, this challenge is addressed by reporting three‐dimensional imaging of defects, crystal morphology, and strain dynamics in individual Bi2WO6(BWO) nanoflakes using Bragg coherent diffractive imaging (BCDI) underoperandotemperature, gas, and light‐driven conditions. It is demonstrated that maintaining a constant temperature of 40°C thermally activates charge carriers, likely enhancing their mobility and reducing recombination rates. Furthermore, an Argon (Ar) gas flow stabilizes the reaction environment, while a mixed Hydrogen–Nitrogen (H2+ N2) flow induces a hydrogen‐triggered semiconducting‐to‐metallic (SM) electronic phase transition accompanied by a structural transformation, as supported by density functional theory (DFT) calculations. Both DFT and BCDI analyses reveal that during the SM phase transition, a new structural phase nucleates near defects and propagates inhomogeneously. Notably, the onset of nanoscale cracking is observed, driven by localized strain accumulation and environmental cycling, which increases surface area and potentially introduces new reactive sites. These findings illustrate that combining advanced nanostructuring withoperandoimaging techniques can provide critical insights into the local structural features that govern photocatalytic performance, paving the way for the rational design of next‐generation photocatalytic materials.more » « lessFree, publicly-accessible full text available September 1, 2026
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null (Ed.)Defects in strongly correlated materials such as V 2 O 3 play influential roles on their electrical properties. Understanding the defects' structure is of paramount importance. In this project, we investigate defect structures in V 2 O 3 grown via a flux method. We use AFM to see surface features in several large flake-like particles that exhibit characteristics of spiral growth. We also use Bragg coherent diffractive imaging (BCDI) to probe in 3 dimensions a smaller particle without flake-like morphology and note an absence of the pure screw dislocation characteristic of spiral growth. We identified and measured several defects by comparing the observed local displacement of the crystal, measured via BCDI to well-known models of the displacement around defects in the crystal. We identified two partial dislocations in the crystal. We discuss how defects of different types influence the morphology of V 2 O 3 crystals grown via a flux method.more » « less
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