Scanning tunneling microscopy was used to probe the molecular scale structures of pure and mixed composition self‐assembled monolayers of CH3(CH2)15SH and CH3O2C(CH2)15SH on gold. A predominant defect structure is found for both films, and is assigned as a void defect in the thiolate overlayer. The mixed composition films are observed to phase segregate into domains of the pure component thiolates. Time‐lapse series of scanning tunneling microscope images reveal kink‐driven motion at step edges and exchange of thiolate molecules on terraces.

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