I am using the attached link protocol in order to clean a gold electrode to obtain a stable self-assembled monolayer. My electrode is a electrode tip from Autolab Metrohm, where there is a PEEK substrate with a gold electrode in the center. So, in this case, I can't use the piranha solution, since PEEK is not compatible with strong mineral acids. Then, I did only the polishing and the electrochemical cleaning.
Well, after doing the polishing, cleaning and sonicating the electrode with ethanol and electrochemically cleaning the electrode, for some electrodes, I keep getting this CV profile of gold (in H2SO4 0.5M) with two low-intensity reduction peaks. This is also happens when I deposit a SAM in the electrode and try to clean it without the polishing and only with the electrochemical cleaning. The reason for that is to maintain the same surface roughness (which can change with each polishing).
Protocol link: https://www.nature.com/articles/nprot.2013.007
Any insights in how to properly clean and eliminate these doubled reduction peaks? Or any article that discuss about the gold electrode behaviour in acid media?
Hello everyone! I don't know if it is too late to answer, but I try. I am using the same protocol used by Rodrigo to prepare the Au surface electrode for functionalization with SAM. I noticed that this type of phenomenon occurs when the H2SO4 solution is not replaced, after cyclic voltammetry. It is advisable to always replace the solution after each voltammetry, for more effective cleaning of surface electrode. If you replace the H2SO4 solution, every time, the problem does not occur and after a certain number of cyclic voltammetries (it depends on a certain number of factors), the typical voltammogram of a clean Au electrode is obtained (only one peak for the reduction of Au oxides).
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