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Structural elucidation of 2D polymer monolayers proving long-range order is a challenge that limits the pace in which this recent field of polymer chemistry and of synthetic 2D materials develops. To overcome this bottleneck, we here present a method in which tip-enhanced Raman spectroscopy is combined with a random growth crystallization model to obtain global features from local spectroscopic information. Concretely, we prove the nature and determine the conversion number X of the cross-links for two new 2D homopolymers and one (of three) new 2D copolymers. Assuming random and in-plane growth, our model results in crystallinity degrees of 93.1% to 99.7% and mean radii of defect-free crystalline areas of 3-15 nm for conversion numbers of 84% &lt; X &lt; 98%. Thus, we provide strong evidence for the synthetic monolayer 2D materials presented that they qualify as 2D polymers and are therefore perfectly suited for in-depth studies both in a more fundamental direction as well as toward application. This example shows how our method can affect current research on covalent sheets.

journal of the american chemical society

Structure Elucidation of 2D Polymer Monolayers Based on Crystallization Estimates Derived from Tip-Enhanced Raman Spectroscopy (TERS) Polymerization Conversion Data