Reliable determination of chemical state in x-ray photoelectron spectroscopy based on sample-work-function referencing to adventitious carbon: Resolving the myth of apparent constant binding energy of the C 1s peak

2018 ◽  
Vol 451 ◽  
pp. 99-103 ◽  
Author(s):  
G. Greczynski ◽  
L. Hultman
2016 ◽  
Vol 45 (18) ◽  
pp. 7678-7696 ◽  
Author(s):  
Jeremy L. Bourque ◽  
Mark C. Biesinger ◽  
Kim M. Baines

The chemical state of novel gallium complexes are readily determined using X-ray Photoelectron Spectroscopy providing unprecedented insight into reactivity.


2020 ◽  
Vol 39 (1) ◽  
pp. 351-356
Author(s):  
Deman Liu ◽  
Jiang Diao ◽  
Yiyu Qiu ◽  
Guang Wang ◽  
Gang Li ◽  
...  

AbstractThe chromium valence states in the CaO–SiO2–FeO–MgO–CrOx system were investigated by X-ray photoelectron spectroscopy (XPS). The results indicated that the XPS peaks of Cr 2p3/2 and Cr 2p1/2 locate at the binding energy of ∼577 and ∼586 eV, respectively. There are three kinds of chromium ions such as bivalent Cr(ii), trivalent Cr(iii), and hexavalent Cr(vi) in the CaO–SiO2–FeO–MgO–CrOx slag. Cr(iii) is the dominant valence state, and more than 77.99% Cr is trivalent Cr(iii). The fraction of Cr(ii)/Cr is in the range of 11.24–17.22%. The fraction of Cr(vi)/Cr is below 4.80%. The fraction of Cr(ii)/Cr decreases with increasing slag basicity, Cr2O3 content, temperature, or oxygen pressure log(PO2), while the fraction of Cr(iii)/Cr increases with increasing basicity, Cr2O3 content, temperature, or oxygen pressure. The trend of change is opposite. Low log(PO2), high Cr2O3 content, and high temperature are beneficial to reduce the toxic hexavalent Cr(vi). The slag basicity has little influence on the fraction of Cr(vi)/Cr.


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.


2008 ◽  
Vol 23 (5) ◽  
pp. 1371-1382 ◽  
Author(s):  
T. Sritharan ◽  
Y.B. Li ◽  
C. Xu ◽  
S. Zhang

Three common Al–Au intermetallics, Al2Au, AlAu2, and AlAu4, were oxidized in the air and characterized using x-ray photoelectron spectroscopy in terms of the elemental chemical state. It was found that there is an increasing trend of oxidation in these intermetallics as the Au content increases. AlAu4 shows the greatest tendency to oxidize with two extra peaks appearing on the Au 4f spectra after long exposure time in air. The surface of AlAu2, although fully oxidized, reveals only one Au 4f peak shift as depth increases. Al2Au was the least oxidizing compound, and the oxide is thin. The binding energies of Al 2p and Au 4f peaks were measured and reported. The Au atoms trapped in the oxide layers exhibit higher binding energy emissions compared to those of elemental Au.


Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1969
Author(s):  
Riccardo Scarfiello ◽  
Elisabetta Mazzotta ◽  
Davide Altamura ◽  
Concetta Nobile ◽  
Rosanna Mastria ◽  
...  

The surface and structural characterization techniques of three atom-thick bi-dimensional 2D-WS2 colloidal nanocrystals cross the limit of bulk investigation, offering the possibility of simultaneous phase identification, structural-to-morphological evaluation, and surface chemical description. In the present study, we report a rational understanding based on X-ray photoelectron spectroscopy (XPS) and structural inspection of two kinds of dimensionally controllable 2D-WS2 colloidal nanoflakes (NFLs) generated with a surfactant assisted non-hydrolytic route. The qualitative and quantitative determination of 1T’ and 2H phases based on W 4f XPS signal components, together with the presence of two kinds of sulfur ions, S22− and S2−, based on S 2p signal and related to the formation of WS2 and WOxSy in a mixed oxygen-sulfur environment, are carefully reported and discussed for both nanocrystals breeds. The XPS results are used as an input for detailed X-ray Diffraction (XRD) analysis allowing for a clear discrimination of NFLs crystal habit, and an estimation of the exact number of atomic monolayers composing the 2D-WS2 nanocrystalline samples.


2021 ◽  
Vol 17 ◽  
Author(s):  
Ke Huan ◽  
Li Tang ◽  
Dongmei Deng ◽  
Huan Wang ◽  
Xiaojing Si ◽  
...  

Background: Hydrogen peroxide (H2O2) is a common reagent in the production and living, but excessive H2O2 may enhance the danger to the human body. Consequently, it is very important to develop economical, fast and accurate techniques for detecting H2O2. Methods: A simple two-step electrodeposition process was applied to synthesize Pd-Cu/Cu2O nanocomposite for non-enzymatic H2O2 sensor. Cu/Cu2O nanomaterial was firstly electrodeposited on FTO by potential oscillation technique, and then Pd nanoparticles were electrodeposited on Cu/Cu2O nanomaterial by cyclic voltammetry. The chemical structure, component, and morphology of the synthesized Pd-Cu/Cu2O nanocomposite were characterized by X-ray diffraction, scanning electron microscopy and X-ray photoelectron spectroscopy. The electrochemical properties of Pd-Cu/Cu2O nanocomposite were studied by cyclic voltammetry and amperometry. Results: Under optimal conditions, the as-fabricated sensor displayed a broad linear range (5-4000 µM) and low detection limit (1.8 µM) for the determination of H2O2. The proposed sensor showed good selectivity and reproducibility. Meanwhile, the proposed sensor has been successfully applied to detect H2O2 in milk. Conclusion: The Pd-Cu/Cu2O/FTO biosensor exhibits excellent electrochemical activity for H2O2 reduction, which has great potential application in the field of food safety.


1989 ◽  
Vol 159 ◽  
Author(s):  
E.D. Richmond

ABSTRACTFor the first time the (1102) surface of sapphire has been investigated by X-ray photoelectron spectroscopy to ascertain chemical changes resulting from annealing in vacuum at 1300° C and 1450° C. As received substrates had a substantial surface C contaminant. For substrates that were chemically cleaned before inserting them into the MBE system no trace of carbon is detected. A residual flourine contaminant results from the cleaning procedure and is desorbed by the vacuum annealing. Spectra of annealed substrates are compared to the unannealed chemically cleaned substrates. The annealed substrates exhibit 0.4 to 0.5 eV shift to higher binding energy of the Al peak and a 0.3 eV shift to higher binding energy of the O peak. In addition, a 2% depletion of oxygen from the surface occurs.


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