I have prepared MoO3 by electrodeposition and found it more stable in aqueous electrolytes than commercial MoO3. When I compared the HR-XPS spectrum of O 1s of the electrodeposited MoO3 with that of the commercial one, I found a shoulder at ~ 532.5 in the former as in the attached images. I attributed it to hydroxyl groups that probably formed at the MoO3 surface during its electrosynthesis. My questions are:
1- How to confirm the presence of hydroxyl groups on MoO3 with another technique other than XPS as this shoulder may also be attributed to adsorbed CO2?
2- Do these hydroxyl groups, if they already exist, have a role in stabilizing MoO3 in aqueous electrolytes, unlike the commercial one that severely dissolves?
Please list any relevant references.
How good is the reflectivity? You could try ATR-IR spectroscopy and look whether you find a characteristic Mo-OH vibration.
Thanks Dr Jürgen Weippert. I have no idea about the reflectivity. Is it determined from the kinetic energy of the emitted photoelectrons?
By using FTIR you could get hydroxyl frequencies and there could be a possibility of hydrogen bonding between surface hydroxyl group.
The reflectivity is not something you see in PES (that's a cross section); reflectivity is always light in- light out. By the way, a sample that's reflecting in the visible range doesn't need to be reflective in the infrared and vice versa, e.g. glazed wood doesn't reflect visible light very well but you can actually use it as an infrared mirror.
FTIR analysis is good for you to test that hydroxide group that will appear at 3500 cm-1 nearly
second the ta hydroxyl group can stabilize your oxide in water for long time through h- bonding
Perhaps, you may obtain information about the presence or absence of adsorbed CO2 by comparing the high binding energy side of the C1s peak
Thanks, Dr. S. Feliu Jr . I found a very weak peak around 292 eV in the HR-XPS scan of C1s, but I am still unsure about the shoulder at ~ 532.5 here.
Thank you, Dr. Mahmoud Fathy Moubark . Have you read any relevant work discussing the effect of H-bonding on stabilizing oxides in aqueous media?
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