The urgency of finding solutions to global energy, sustainability, and healthcare challenges has motivated rethinking of the conventional chemistry and material science workflows. Self‐driving labs, emerged through integration of disruptive physical and digital technologies, including robotics, additive manufacturing, reaction miniaturization, and artificial intelligence, have the potential to accelerate the pace of materials and molecular discovery by 10–100X. Using autonomous robotic experimentation workflows, self‐driving labs enable access to a larger part of the chemical universe and reduce the time‐to‐solution through an iterative hypothesis formulation, intelligent experiment selection, and automated testing. By providing a data‐centric abstraction to the accelerated discovery cycle, in this perspective article, the required hardware and software technological infrastructure to unlock the true potential of self‐driving labs is discussed. In particular, process intensification as an accelerator mechanism for reaction modules of self‐driving labs and digitalization strategies to further accelerate the discovery cycle in chemical and materials sciences are discussed.

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We present the use of a coiled-flow inverter (CFI) for continuous-flow photochemistry at competitive photon efficiencies. The static mixer is placed inside a reaction chamber, whereas a dark adjacent chamber allows for orthogonal online reaction monitoring via fluorescence spectroscopy. The study of the aqueous visible-light induced degradation of fluorescein with ZnO-APTMS-Au photocatalyst showcases the challenge of uniformly irradiating photoreactors with nonplanar surfaces. Fluorescence imaging is introduced as a simple method to visualize spatial gradients in the irradiance at the outer surface of such complex photoreactor geometries, allowing the analysis of photoreactor efficiency as a function of lighting configuration. We compared uniaxial and multiaxial lighting configurations and discuss the challenges associated with attaining uniform irradiance distribution of incident light on coiled-flow inverters, where chaotic advection combats light attenuation. A first calculation of the photochemical space-time yield (PSTY) for a "photo-CFI" indicates that a competitive photon efficiency can be reached as compared to other photoreactor designs.

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