Hello
I've recently reached the point in my work when I will need to conduct some electrochemical measurements, but unfortunately I have to start everything from scratch, because in our lab no one was ever doing measurements of electrocatalysts. Basically, I'm looking for any kind of instructions on how to perform ORR measurements. Right now I'm playing with commercial Pt/C catalyst, I'm using glassy carbon working electrode, platinum counter electrode, Ag/AgCl pseudo-reference electrode and 0,1 M H2SO4 electrolyte. I'm trying out different inks with different Nafion concentrations, but so far all my CV spectra have no resemblance of the ones presented in literature.
Thank you in advance for any suggestions.
Dear Szymon Smykała ,
First, commercial Pt/C has to be electrochemically cleaned. In your conditions dozen of CV cycles in the potential range ~ -0.2 V to ~1.35 V. (After that replace the solutions). You can see the procedures in classical papers by Schmit and Gasteiger, for example:
T. J. Schmidt et al 1998 J. Electrochem. Soc. 145 2354 Characterization of High‐Surface‐Area Electrocatalysts Using a Rotating Disk Electrode Configuration, Article Characterization of High‐Surface‐Area Electrocatalysts Using...
This is added by RG when I put doi?or
U.A. Paulus, T.J. Schmidt, H.A. Gasteiger, R.J. Behm, Oxygen reduction on a high-surface area Pt/Vulcan carbon catalyst: a thin-film rotating ring-disk electrode study, Journal of Electroanalytical Chemistry 495 (2001) 134 – 145 . Article Oxygen reduction on a high-surface area Pt/Vulcan carbon cat...
Greetings,
prof. Grgur
Dear Szymon,
There's quite a few papers and literature reviews on this subject that include detailed discussions concerning the experimental side of things. The following article is a good example, and is focused on the ORR:
Article Oxygen Reduction Reaction Measurements on Platinum Electroca...
Hope that helps you on your way.
Best regards,
Jan
If 0,1 M H2SO4 is your electrolyte , you have to use a true reference electrode (Ag/AgCl pseudo-reference doesn't have a stable potential in an aqueous solution without Cl-). This issue can be a reason for strange CV.
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