我的样品是氧化物粉末，之前审稿人要求补测XPS,修回之后审稿人又指出C1s 校正是不准确的。想问下大家平时是怎么测XPS的 怎么处理数据的。
审稿意见如下：1. XPS experimental details are not complete. What was the excitation source, electron emission angle, the size of analyzed area? Where samples sputter-etched prior to analyses? If so, what was the Ar+ energy and incidence angle? What was the base pressure during analyses? Was charge neutralizer used? All of these aspects are crucial for the correct interpretation of experimental results.
2. "The adventitious C1s peak at 284.8 eV was used to charging correction." Note that aligning the spectra to the C 1s peak of adventitious carbon is a highly risky procedure and was recently shown to lead to unphysical results (ChemPhysChem 18 (2017) 1507 and Angewandte Chemie Int. Ed. 59 (2020) 5002). Therefore, I strongly suggest to avoid it. Adventitious carbon is in general an unknown compound, not an inherent part of the sample, does not make proper electrical contact to the analyzed sample, BE of the C 1s peak varies in a wide range.
Alternatives:
- Measure density of states close to the Fermi level and use the Fermi edge as the energy reference ("0 eV" of the binding energy scale)
- Work function method (see: Appl. Surf. Sci. 451 (2018) 99)
- Use well-defined peaks from the sample itself (instead of C 1s peak from the contaminating carbon layer).
