Abstract
The initial adsorption, structural transition, and polymeric growth of 1‐octyne‐3‐ol on iron electrode from sulfuric acid solutions have been examined by using time‐resolved in situ automatic ellipsometry. The adsorption occurs in two different configurations, flat and partly upright. The structural transition of the adsorbed octynol molecules is characterized by a large time constant indicating adsorption‐reorientation mechanism. The linear growth of the polymer layer together with the current oscillations for hydrogen evolution reaction suggests a thin porous loosely bonded structure. The optical properties are related to the small conjugated units within the compact domains of the film.