Electrochemical Pretreatment of Polycrystalline Gold Electrodes To Produce a Reproducible Surface Roughness for Self-Assembly: A Study in Phosphate Buffer pH 7.4

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Abstract
It has been emphasized in several studies that the state of the surface, including the surface roughness, is very important for the reproducible formation of high-quality self-assembled monolayers on gold. The pulsed-potential pretreatment procedure described in this paper can, in a reproducible way, reduce the surface roughness of mechanically polished polycrystalline gold electrodes by a factor 2. The developed procedure, in which the gold is alternately oxidized and reduced, has been optimized for use in a flow system (100 mM phosphate buffer pH 7.4). The influence of the pretreatment procedure on the surface roughness of the electrodes has been studied by in-situ oxygen adsorption measurements using cyclic voltammetry. The most effective pulse regime in producing a gold surface with a reproducible and relatively low surface roughness is a triple-potential pulse waveform, with potentials of +1.6, 0.0, and −0.8 V vs SCE and pulse widths of 100 ms for each potential. Prolonged pulsing for 2000−5000 s with the gold working electrode in a flow-through cell showed an electropolishing effect, i.e., a decrease of the roughness in time. Flow conditions are very important: the roughness decreased faster at higher flow rates, while an increase was observed without flow. A process of reconstruction and dissolution of gold during application of the potential pulses under flow conditions is assumed to account for the observed phenomena. A self-assembled monolayer of thioctic acid with reproducible characteristics, determined with impedance measurements, could be formed on a pretreated gold surface.