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Self-assembly of colloidal nanocrystals (NCs) into superlattices (SLs) is anappealing strategy to design hierarchically organized materials with newfunctionalities. Mechanistic studies are still needed to uncover the designprinciples for SL self-assembly, but such studies have been difficult toperform due to the fast time- and short length scales of NC systems. To addressthis challenge, we developed an apparatus to directly measure the evolvingphases \textit{in situ} and in real time of an electrostatically stabilized AuNC solution before, during, and after it is quenched to form SLs using smallangle X-ray scattering (SAXS). By developing a quantitative model, we fit thetime-dependent scattering patterns to obtain the phase diagram of the systemand the kinetics of the colloidal and SL phases as a function of varying quenchconditions. The extracted phase diagram is consistent with particles whoseinteractions are short in range relative to their diameter. We find the degreeof SL order is primarily determined by fast (sub-second) initial nucleation andgrowth kinetics, while coarsening at later times depends non-monotonically onthe driving force for self-assembly. We validate these results by directcomparison with simulations and use them to suggest dynamic design principlesto optimize crystallinity within a finite time window. The combination of thismeasurement methodology, quantitative analysis, and simulation should begeneralizable to elucidate and better control the microscopic self-assemblypathways of a wide range of bottom-up assembled systems and architectures.

In situ X-ray scattering reveals coarsening rates of superlattices  self-assembled from electrostatically stabilized metal nanocrystals depend  non-monotonically on driving force