Calibration of the X-Ray Photoelectron Spectroscopy Binding Energy Scale for the Characterization of Heterogeneous Catalysts: Is Everything Really under Control?

ChemPhysChem ◽  
2013 ◽  
Vol 14 (15) ◽  
pp. 3618-3626 ◽  
Author(s):  
Marc Jacquemin ◽  
Michel J. Genet ◽  
Eric M. Gaigneaux ◽  
Damien P. Debecker
2021 ◽  
Vol 11 (1) ◽  
Author(s):  
G. Greczynski ◽  
L. Hultman

AbstractChemical state analysis in X-ray photoelectron spectroscopy (XPS) relies on assigning well-defined binding energy values to core level electrons originating from atoms in particular bonding configurations. Here, we present direct evidence for the violation of this paradigm. It is shown that the C 1s peak due to C–C/C–H bonded atoms from adventitious carbon (AdC) layers accumulating on Al and Au foils splits into two distinctly different contributions, as a result of vacuum level alignment at the AdC/foil interface. The phenomenon is observed while simultaneously recording the spectrum from two metal foils in electric contact with each other. This finding exposes fundamental problems with the reliability of reported XPS data as C 1s peak of AdC is routinely used for binding energy scale referencing. The use of adventitious carbon in XPS should thus be discontinued as it leads to nonsense results. Consequently, ISO and ASTM charge referencing guides need to be rewritten.


1982 ◽  
Vol 36 (3) ◽  
pp. 290-296 ◽  
Author(s):  
Manuel Carvalho ◽  
Larry F. Wieserman ◽  
David M. Hercules

Wilkinson's catalyst, RhCl(PPh3)3 is a well known and widely used homogeneous hydrogenation catalyst. This catalyst was analyzed by ESCA which revealed that two rhodium species [Rh(I) and Rh(III)] were present, both for commercial preparations and for catalysts prepared in this laboratory. The ratio of Rh(I) to Rh(III) was 3:2 regardless of the source. A different method of synthesizing RhCl(PPh3)3 was used and produced a compound having only Rh(I) species. Additional analytical techniques such as elemental analysis, FT-IR, liquid chromatography, and 31P NMR were used to determine the origin of the higher binding energy peaks when Wilkinson's procedure was used to prepare RhCl(PPh3)3. Hydrogenation of cyclohexene was also performed to determine the effect of the higher binding energy species on catalytic activity.


2002 ◽  
Vol 09 (02) ◽  
pp. 1097-1102
Author(s):  
E. Z. KURMAEV ◽  
I. I. LYAKHOVSKAYA ◽  
J. KORTUS ◽  
M. DEMETER ◽  
M. NEUMANN ◽  
...  

Measurements of X-ray emission and absorption of the constituents of MgB 2 are presented. The results obtained are in good agreement with calculated X-ray spectra, with dipole matrix elements taken into account. The comparison of X-ray emission spectra of graphite, AlB 2, and MgB 2 in the binding energy scale supports the idea of charge transfer from σ to π bands, which creates holes at the top of the bonding σ bands and drives the high-Tc superconductivity in MgB 2.


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