• The synthesis and characterization of nanomaterials is currently undergoing a significant and rapid evolution, driven by the deployment of artificial intelligence (AI) in workflows involving nanomaterials synthesis platforms as well as characterization modalities. In addition to improved reliability and efficiency, these new automated methods promise significant advantages compared to previous iterations, including completely novel experimental capabilities, autonomous methods towards nonequilibrium materials growth, and methods for active structure-processing-property learning with theory-in-the-loop.