A global and extremely simple strategy to prepare a covalently attached monolayered organic film on the carbon surface is presented.

We report the experimental reassessment of the widely admitted concerted reduction mechanism for diazonium electroreduction. Ultrafast cyclic voltammetry was exploited to demonstrate the existence of a stepwise pathway, and real-time spectroelectrochemistry experiments allowed visualization of the spectral signature of an evolution product of the phenyldiazenyl radical intermediate. Unambiguous identification of the diazenyl species was achieved by radical trapping followed by X-ray structure resolution. The electrochemical generation of this transient under intermediate energetic conditions calls into question our comprehension of the layer structuration when surface modification is achieved via the diazonium electrografting technique as this azo-containing intermediate could be responsible for the systematic presence of azo bridges in nanometric films.

This work reports the first in-situ and real-time resolved spectroelectrochemical monitoring of a diazonium electrografting. Exploiting the 4-nitrobenzene diazonium salt reduction, we provide a spectral characterization of the adsorption kinetic...

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