scholarly journals Applications of Sxps for Studying Surface Structure, Reaction Mechanisms and Kinetics

1994 ◽  
Vol 375 ◽  
Author(s):  
D. R. Mullins ◽  
D. R. Huntley ◽  
S. H. Overbury

AbstractSoft x-ray photoelectron spectroscopy (SXPS) from the S 2p core level has been used to study adsorbate induced reconstruction, identify reaction intermediates and study reaction kinetics on the Ni(111) surface. The S 2p binding energy is affected by the nature of the surface adsorption site. It has been determined from the number of S 2p states and their relative binding energies that adsorbed S induces a reconstruction of the Ni(111) surface and that the S adsorbs in fourfold sites on terraces and in troughs. S 2p SXPS has also been used to identify adsorbed species during the thermal decomposition of methanethiol on Ni(111). CH3SH adsorbs as CH 3S- at low temperatures. Above 200 K, the CH3S- changes adsorption site and the C-S bond begins to cleave. The relative concentrations of CH3S- in the two different sites and of atomic S have been monitored as a function of temperature and initial coverage. As a result of the sensitivity and resolution available in SXPS, reactions rates and kinetic parameters have been obtained for the decomposition of benzenethiol on Ni(111) by monitoring the changes in the surface composition continuously as a function of temperature and time.

2020 ◽  
Author(s):  
Jennifer A. Rudd ◽  
Ewa Kazimierska ◽  
Louise B. Hamdy ◽  
Odin Bain ◽  
Sunyhik Ahn ◽  
...  

The utilization of carbon dioxide is a major incentive for the growing field of carbon capture. Carbon dioxide could be an abundant building block to generate higher value products. Herein, we describe the use of porous copper electrodes to catalyze the reduction of carbon dioxide into higher value products such as ethylene, ethanol and, notably, propanol. For <i>n</i>-propanol production, faradaic efficiencies reach 4.93% at -0.83 V <i>vs</i> RHE, with a geometric partial current density of -1.85 mA/cm<sup>2</sup>. We have documented the performance of the catalyst in both pristine and urea-modified foams pre- and post-electrolysis. Before electrolysis, the copper electrode consisted of a mixture of cuboctahedra and dendrites. After 35-minute electrolysis, the cuboctahedra and dendrites have undergone structural rearrangement. Changes in the interaction of urea with the catalyst surface have also been observed. These transformations were characterized <i>ex-situ</i> using scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. We found that alterations in the morphology, crystallinity, and surface composition of the catalyst led to the deactivation of the copper foams.


2001 ◽  
Vol 702 ◽  
Author(s):  
Giovanni F Crosta ◽  
Art J Nelson ◽  
Marina C Camatini

ABSTRACTThree types of debris particles, denoted by L2, H2 and K3 respectively, originated from the abrasion of silica-filled, vulcanized rubber under different test conditions (severity) were analyzed and compared. The structural fractal dimension, DFS, of the particle perimeter was chosen as a morphological descriptor (but not necessarily as an intrinsic property of the fractured material !). Said dimension was estimated by processing light microscopy images. A value of the morphological threshold, TST, which separates the textural from the structural domain in the RICHARDSON plot was determined in order to maximize discrimination between the three particle types and rank them by increasing values of DFS. Particles from the highest severity test (K3) exhibited the highest value of DFS. X ray photoelectron spectroscopy (XPS) provided elemental composition, core level binding energies and the speciation of C, N, O, Si and S. As a result, L2 debris was found to originate from two processes: fracture of rubber and segregation of extender oil. Evidence has come both from morphology and XPS. Particles of H2 and K3 were ascribed to fracture alone. Comparison between K3 and the reference material, rasped rubber (RAS), shows the following: a) increase of the [S]/[C] surface atomic concentration ratio from RAS to K3; b) existence of multiple bonding states of S in K3 with energy peaking at 162.9 ± 0.3 eV ([-S-S-]n); c) weak contribution of R-S-O-R oxidized S species in K3 at 165 eV, not seen in RAS; d) no evidence of either SO3 or SO4 groups in any material. Although preliminary, these results prove the ability of morphological analysis and XPS to characterize the surface properties of debris particles non destructively.


Author(s):  
Sahadeb Ghosh ◽  
Mangala Nand ◽  
Rajiv Kamparath ◽  
Mukul Gupta ◽  
Devdatta M Phase ◽  
...  

Abstract Oriented thin films of β-(Ga1-xFex)2O3 have been deposited by RF magnetron sputtering on c-Al2O3 and GaN substrates. The itinerant character of Fe 3d states forming the top of the valence band (VB) of Fe substituted of β-Ga2O3 thin films has been determined from resonant photoelectron spectroscopy (RPES). Further, admixture of itinerant and localized character of these Fe 3d sates is obtained for larger binding energies i.e deeper of VB. The bottom of the conduction band (CB) for β-(Ga1-xFex)2O3 is also found to be strongly hybridized states involving Fe 3d and O 2p states as compared to that of Ga 4s in pristine β-Ga2O3. This suggests that β-Ga2O3 transforms from band like system to a charge transfer system with Fe substitution. Furthermore, the bandgap red shits with Fe composition, which has been found to be primarily related to the shift of the CB edge.


Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1725 ◽  
Author(s):  
Xiaohong Liu ◽  
Ming Li ◽  
Xuemei Zheng ◽  
Elias Retulainen ◽  
Shiyu Fu

As a type of functional group, azo-derivatives are commonly used to synthesize responsive materials. Cellulose nanocrystals (CNCs), prepared by acid hydrolysis of cotton, were dewatered and reacted with 2-bromoisobuturyl bromide to form a macro-initiator, which grafted 6-[4-(4-methoxyphenyl-azo) phenoxy] hexyl methacrylate (MMAZO) via atom transfer radical polymerization. The successful grafting was supported by Fourier transform infrared spectroscopy (FT-IR) and Solid magnetic resonance carbon spectrum (MAS 13C-NMR). The morphology and surface composition of the poly{6-[4-(4-methoxyphenylazo) phenoxy] hexyl methacrylate} (PMMAZO)-grafted CNCs were confirmed with Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). The grafting rate on the macro-initiator of CNCs was over 870%, and the polydispersities of branched polymers were narrow. The crystal structure of CNCs did not change after grafting, as determined by X-ray diffraction (XRD). The polymer PMMAZO improved the thermal stability of cellulose nanocrystals, as shown by thermogravimetry analysis (TGA). Then the PMMAZO-grafted CNCs were mixed with polyurethane and casted to form a composite film. The film showed a significant light and pH response, which may be suitable for visual acid-alkali measurement and reversible optical storage.


2018 ◽  
Vol 122 (10) ◽  
pp. 2695-2702 ◽  
Author(s):  
E. Antonsson ◽  
C. Raschpichler ◽  
B. Langer ◽  
D. Marchenko ◽  
E. Rühl

2006 ◽  
Vol 600 (18) ◽  
pp. 3749-3752 ◽  
Author(s):  
C. Biswas ◽  
S. Banik ◽  
A.K. Shukla ◽  
R.S. Dhaka ◽  
V. Ganesan ◽  
...  

2014 ◽  
Vol 16 (39) ◽  
pp. 21486-21495 ◽  
Author(s):  
Josephina Werner ◽  
Jan Julin ◽  
Maryam Dalirian ◽  
Nønne L. Prisle ◽  
Gunnar Öhrwall ◽  
...  

The water–vapor interface of aqueous solutions of succinic acid, where pH values and bulk concentrations were varied, has been studied using surface sensitive X-ray photoelectron spectroscopy (XPS) and molecular dynamics (MD) simulations.


Author(s):  
Changqing Liu ◽  
David A. Hutt ◽  
Dezhi Li ◽  
Paul P. Conway

This paper aims to gain an insight into the correlation between the microstructure and surface composition of electroless Ni-P and its behaviour during soldering with Pb free alloys including Sn-3.8Ag-0.7Cu, Sn-3.5Ag and Sn-0.7Cu. Ni-P coatings with different P contents were produced through an industrial process on copper metal substrates. The surface morphology of these coatings was observed by Scanning Electron Microscopy (SEM) and the bulk composition was analyzed by means of Energy Dispersive X-ray analysis (EDX). The mechanical properties of the coatings were evaluated by nano-indentation testing under different maximum loads. However, to understand the behaviour of P in Ni-P coatings and deterioration of the coating surfaces during exposure to air, the surfaces of the coatings were also characterised by X-ray Photoelectron Spectroscopy (XPS) for storage at different temperatures. The dependence of the solderability of Ni-P coatings on the storage time and temperature was investigated by wetting balance testing, using an inactive or active flux with or without an inert N2 atmosphere. Finally, the solderability of Ni-P coatings to Pb free solders is correlated with their composition and microstructure (e.g. surface characteristics).


2002 ◽  
Vol 57 (2) ◽  
pp. 193-201 ◽  
Author(s):  
Gülsün Gökağaç ◽  
Brendan J. Kennedy

11% Pt/C, 10% Pt + 1%Os/C, 9% Pt + 2%Os/C, 8% Pt + 3%Os/C, 7% Pt + 4%Os/C, 6% Pt + 5%Os/C and 5%Pt + 6% Os/C catalysts have been prepared for methanol oxidation reaction. Transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction and cyclic voltammetry have been used to understand the nature of the species present in these catalysts. 7% Pt + 4% Os/C was the most active catalyst, while 8% Pt + 3% Os/C was the least active one. It is found that the metal particle size and distribution on the carbon support, the surface composition and the oxidation states of the metal particles, the metal-metal and metal support interactions are important parameters to define the activity of the catalyst.


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