The obtained XRD pattern of NiCo2O4 matched with JCPDS No. 73-1702. But, similar peaks arise in XRD of Co3O4 because both of these have cubic phase. In order to prove that our synthesized NiCo2O4 is free from any other oxide, melting point observation is one of the suitable ways. I could not find the reported melting point of NiCo2O4. can anyone please help?
Other suggestions are also welcome.
Manpreet Kaur
You may characterize the sample with high-resolution XPS to analyze surface electronic states and chemical composition. I hope this answer will be helpful for you. Best luck with your research !!
@Pratik Mane
I have gone through a lot XPS data into literature.... All have peaks for Co2+ ion as well which indicate there must be some other Cobalt oxides present in the sample. In NiCo2O4, Co is in +3 oxidation state.
Do area under the curve of XPS tells about the elemental composition???
In your case at first I would analize the sample by EDS after a proper metallographic preparation. Anyway some clues can be further obtained form the diffraction pattern (obviously data must be collected with care, with the highest resolution you can). Try to look at the peak shape: is the peak symmetric or asymetrically broadened (or even split)? If it's symmetric you can assume that you have a single phase, in the other cases phase separation or chemical fluctuations are likely to occur. Morevoer you cannot exclude that your sample is something like Ni1-xCo2+xO4. I would choose neutron diffraction for the best characterization od Ni and Co content in the phase.
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