Dear Colleagues
We are currently preparing transition metal-doped rGO sheets using the classical modified Hammer method. We need to understand the composition of the prepared sample. for example, if I want to prepare Co-doped rGO sample. I mix the GO with Co acetate as precursor, then, calcination step takes place. I need to check the presence of CoO or Co3O4 in my sample. Beside the XRD, can you suggest a method for proofing the composition?
Thanks in advance
1) XPS
2) EDX
3) FTIR analysis along with XRD may help.@ Mohamed S. Mahmoud
Dear Mohamed S. Mahmoud,
Quantification from XPS is helpful for compositional analysis of such samples where mixed-valent elements are present.
Best regards,
SS
I recommend you to burt out your materials by TGA in air to quantify the final residue you have. That would help you to check out if the amount that you have impregnated ( in mass) is correct. Once your impregnation is right, and want to analyze the oxidation state of your metal, XPS is a good technique. BUT you should be careful with carbon based materials. There is XPS handbook that will help you to check the Binding Energies and their displacements in order to know which state of your metal you have. Use literature to guide you being careful what you get.
Best
Adrián
Hi Mohamed,
Apart from XRD, you can try with TGA, XPS, EDX and ICP-MS analysis.
1] TGA will help you determine extent of doping by weight loss however the environment plays vital role in determining the composition. If you carry out in N2 atmosphere, GO will not be oxidized and if you use O2 atmosphere, cobalt may oxidized to Cobalt oxide.
2] EDX will help you to determine the contents in the sample however it isrecommended not to depend on the % compositions displayed as it is confined to point of focus.
3] XPS is of great use, you can make use of it to determine the formation, composition and type of doping also.
4] Similarly, you can also go for ICP analysis, where you can determine exact contents of the sample.
Hope it helps!
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