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Photocatalysis and oxidative degradation in bimetallic nanoparticles are two important processes in which intra- and inter-particle heterogeneity influence chemistry. Do we need ‘pure’ samples in order to obtain optimized chemical performance? Or do we require detailed knowledge, free from ensemble averaging, of how to exploit atomic-scale flaws in metal nanoparticle hybrids? NSF CAFF will answer these questions with in operando, atomic-scale spatial resolution to localize defects and their evolution as reactions progress, while nanometer spatially-resolved spectroscopy tracks energy flow. Additional transformative outcomes include new modules and data science methods to follow and control reactions in situ.