Dear Sudeep,

just to avoid confusion, what you observe are two different chemical states or core level peaks, not a splitting. The splitting of the P2p core level into P2p_1/2 and P2p_3/2 is ~0.87 eV and not as large as 3 eV.

P2O5 could be a fitting chemical state for the high binding energy peak that you observe. Besides P and Zr, do you observe any other peaks in your survey spectrum?

Best regards

Hello Dr. Thorsten Schultz,

Thank you very much for your response. Oh yes, I think splitting is not the right word to use, thanks again for the correction.

I think P2O5 could be a possibility. However, I don't see O 1S in my survey spectrum. I think the high energy P peak might be due to [HPO4]2 units.

May I know your thoughts/opinion on this?

Also, I observe a shift in Zr 3d 3/2 and 3d 5/2 peaks to ~ 188-190 eV and 185-187 eV. I think this shift towards higher binding energy is due to the higher polarization of Zr.

May I also have your insights on this?

If you don't see an O1s core level in your survey, [HPO4]2 can be ruled out.

Do you see a carbon C1s core level from adventitious carbon?

One other possibility could be an artefact due to differential charging...meaning that some areas of your sample are not as conductive as others, therefore accumulating positive charge at the surface and shifting the peaks to higher binding energies. The same shift in your P2p and Zr3d could be an indication for this.

Thank you very much Dr. Schultz. I do account for the C 1s energy shift. In spite of making this correction, the peak is prominent. I wonder if the unequal distribution of charges results in such strong peaks.

Where are the peaks localized when you don't apply the adventitious carbon correction, or to be more precise, what is the shift that you applied by it?

What bothers me: you say you analyzed a phosphate, but you don't see any O1s in your survey, not even if you zoom in? That sounds highly strange.

Could you share an image of your C1s spectrum?

We really need to see your spectra, however I strongly suspect you do have oxygen, else you cannot have phospate. The signal at ~ 136 eV is possibly P2O5, P4O10 or possibly if you had chloride precursors at any point in synthesis, PCl5

P-F compounds would also be an option, but that's all just speculation until we see your survey spectrum

Thanks, everyone. Sorry I was out of town.

I think P-X (X=halogen) is not a possibility as I don't use any halogen precursor in my synthesis.

The C 1S spectrum is in the attachment. The survey spectrum doesn't seem to contain oxygen because the survey scan data is available up to 350 eV. I am told that there was some problem.

My assignment on phosphate is based on the article:

Article ESCA investigations of amorphous and crystalline zirconium a...

ESCA investigations of amorphous and crystalline zirconium acid phosphates

Well, assuming the splitting of your C1s into 284.3 and 287 eV is real, that might actually be an indicator of differently charged domains on your sample.

Thanks Dr. Jürgen Weippert. I will think on this.

One more thing: next time, don't write that O1s wasn't seen when it's just not in the measuring range.

Alright, noted! Thanks