I run one CV with Copper sulphide. The slurry composition is as follows.
5 mg material + 850 micro L IPA + 140 microL MilliQ + 5% perfluorinated nafion. I drop cast this on glassy carbon electrode and run the experiment with NaOH as electrolyte, AgCl reference and graphite as counter electrode. But it is not showing any peaks in Cyclic voltametry. I tried with multiple changes but not able to trouble shoot the reason for the absence of peaks. Can someone help me with the same.
Sajna Ss, if possible the following steps you may follow
1. decrease the conc. of Nafion from 5% to 0.5 or 0.1%
2. if you want to study the redox behavior of materials, try to make an overlayer of Nafion (0.1 to 0.5%) instead of mixing with materials (drop cast your material, then dry it, and then overlayer with Nafion solution).
3. From the reference paper, Make sure that CuS has redox active within the potential region.
4. study with the thin layer of the modified material and with the different scan rates (especially at slow scan rate).
@ Balamurugan Thangavel, Thanks a lot for your reply. I want few clarifications.
1. How much should be the ideal concentration of nafion concentration?. I mean how much should be the maximum concentration of nafion for electrochemical work?
2. Suppose if we make an overlay of nafion on the surface of glassy carbon with dried material on its surface, whether the dried material will not get away?. I mean it will not get fallen away?
3. I could not understand the 4th point. You mean to say that the loading should be low as possible?. Say 5mg per ml or less?. Can you please tell me how much should be the loading?. I use to make 10 mg per ml or less then drop case 2 microL on the surface of glassy carbon.
Thanks a lot sir for helping me.
I read all the above comments, I feel you should add slightly more CuS and go on checking CV again till peak is observed...
Sajna Ss,
Reply to your queries,
1. No ideal conc. for Nafion for electrochemical study. The Conc. of Nafion might be depending upon the materials of interest to study. It is advisable that a low conc. of Nf (0.05% to 0.5%) in the case of sensor applications.
2. The purpose of Nf. overlayer is mainly to avoid leaching of the electrocatalyst unless specific reason like producing a negative charge on the surface. Mostly, the material may not leach from the surface of the electrode. Also, electron tunneling between the electrode substrate and the material will not be sluggish.
3. loading of materials that you have done (as you mentioned) is well.
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