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Electrochemical Roughening of Thin-Film Platinum Macro and Microelectrodes

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Diffusional surface voltammetry as a probe of adsorption energetics.

Juan José Calvente¹, Miguel Molero, Rafael Andreu

¹Departamento de Química Física, Facultad de Química, Universidad de Sevilla, 41012 Sevilla, Spain. pacheco@us.es

Analytical Chemistry

|December 2, 2011

Summary

Diffusional surface voltammetry (DSV) now quantifies adsorption free energy for low surface coverages. This technique determines group contributions to adsorption, linking hydrophobicity to interfacial behavior.

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Probing Surface Electrochemical Activity of Nanomaterials using a Hybrid Atomic Force Microscope-Scanning Electrochemical Microscope (AFM-SECM)

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Published on: February 10, 2021

Area of Science:

Electrochemistry
Surface Science
Physical Chemistry

Background:

Determining adsorption free energy at low surface coverages (Henry limit) requires sensitive techniques.
Existing methods struggle with high sensitivity to both amount and energetics of adsorbed molecules.

Purpose of the Study:

To demonstrate diffusional surface voltammetry (DSV) for direct determination of adsorption free energy at extremely low surface coverages.
To derive a general analytical expression for DSV surface voltammetric peak potential.
To establish strategies and diagnostic criteria for quantitative insight into electrosorption energetics.

Main Methods:

Derivation of a general analytical expression for the surface voltammetric peak potential of DSV.
Utilizing DSV in its stripping mode to determine group contributions to adsorption free energy.
Applying the protocol to homologous series of alkylthiolates adsorbed at mercury electrodes.

Main Results:

DSV successfully determines adsorption free energy for electroactive adsorbates at low surface coverages.
Group contributions of CH(n) groups (n=0-3) to adsorption free energy were quantified for alkylthiolates.
Adsorption energetics correlate linearly with hydrophobicity, as indicated by octanol-water partition coefficients.

Conclusions:

DSV enhances the capability to probe adsorption energetics down to the micromolar level.
The study provides a unified approach for treating stripping and film voltammetries.
Adsorption of hydrocarbon groups at the mercury/solution interface is governed by hydrophobicity.