For example I would like to see is there any material deposited on the electrode surface before and after electrolysis experiments.
But it is a glassy carbon electrode and surface is surrounded by PTFE. Now because PTFE is not conducting, it is hampering the image. In that case can I use some chromium coating?
I've done EDX of such a sample in a variable pressure SEM. With a bit of air, you sample does not need to be coated, you view it in backscatter mode instead of secondary electron mode, and doing EDX is still possible, before and after your electrolysis experiments.
Do a search in your area to see if there is a VP-SEM with EDS available nearby.
Thank you all for your kind help. I will try in backscatter mode and will inform you @Gowen.
To avoid chargign you need to ensure the PTFE is not insulating the piece you want to analyse. For that it should be sufficient to either ensure its back contact is directly contacted to teh speciemn stub or, if not, add a thin line of carbon or silver conductive paint to one side of it. If you coat the sample by Cr you can still do BES imaging but SE will look different, and EDX will show Cr everywhere.
My opinion, First you will be characterized (SEM, EDX) purely form of synthesized materials, after the characterization of materials you will be deposit on the surface of electrode.
Hello,
1. You can use the glassy carbon (GC) plates for characterizing the material. Do your as usual experiment on the GC plate and then characterize it. So that the same morphology will obtain.
2. Regarding your PTFE. In general analysis of the polymeric material will charge on the SEM image. So, first reduced the HV (High voltage). The maximum HV is 30 kV and the minimum is 5 kV. Analyse your samples in 5 or 10 kV. It will not charge and you can get some good images.
3. Backscatter mode needs higher working distance and the HV of around 30 kV. So you can not get the good image in BSE.
4. In the case of EDX, you can do the analysis at 20 kV. In 5 or 10 kV you can not get the good signal. So you need to increase the HV.
If using a SEM with VP-mode (variable pressure) you need not to sputter your sample. Already mentioned by Brent E Gowen.The very low nitrogen atmosphere avoids charging. So you can analyze the electrode by EDX (N will not be detected). We carry out this measurement with a ZEISS Supra 40 VP.
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