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Introduction Synthetic carbon-based nanomaterials are a large and rapidly growing class of functional materials that have many potential advantages, which include biocompatibility, low cost of precursors, and the sheer structural and chemical diversity that is ­possible.1–3 Indeed, there are myriad different structures that can be created using DNA and peptide structural programing, reticular building-block design, or control over assembly and ­crystallization.3–6 However, these complex carbon-based nanostructures are often acutely sensitive to synthesis conditions, and the typical brute force method of materials development, trial and error testing of different synthesis conditions, is not feasible.4,6,7 To  accelerate materials development, having an understanding of the fundamental chemical and physical processes that underlie their synthesis will be critical, allowing

a more systematic, informed approach to functional carbon material discovery. While organic chemistry has developed tools for understanding chemical structure in a synthesis product or intermediate at a discrete period in time, including conventional transmission electron microscopy (TEM), methods for directly observing chemical, and morphological changes in solution over time, have long eluded researchers.8–11 Most solution-phase (in situ) characterization methods rely on bulk scattering of some type of incident energy source—in carbon-based nanostructures, typically this would be light, x-rays, and neutrons.12–15 While these indirect characterization methods can provide valuable information about the ensemble structure of the sample, some with high temporal resolution, the data from these scattering experiments require fitting to

Lucas R. Parent, Innovation Partnership Building, University of Connecticut, USA; [email protected] Maria Vratsanos, Northwestern University, USA; [email protected] Biao Jin, Pacific Northwest National Laboratory, USA; [email protected] James J. De Yoreo, Pacific Northwest National Laboratory, and the University of Washington, USA; [email protected] Nathan C. Gianneschi, Northwestern University, USA; [email protected] doi:10.1557/mrs.2020.224 • VOLUME Core • mrs.org/bulletin © 2020 Materials Research Society Auckland University of Technology, on 15 Sep 2020 at 14:23:50, subject MRS BULLETIN 45 • terms SEPTEMBER 2020 Downloaded from https://www.cambridge.org/core. to the Cambridge of use, available at https://www.cambridge.org/core/terms. https://doi.org/10.1557/mrs.2020.224

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Chemical and physical transformations of carbon-based nanomaterials observed by liquid phase

carbohydrates, amino acids, and lipids, as well as their models predicated on certain assumptions to interpret the raw respective derivatives. These compounds comprise the building data, and can be unreliable for exotic structures, polydisperse blocks of the natural world and are able to natively assemble systems, or where a priori structural knowledge is lacking, as in physical materials with unparallel