XPS and XRD Studies of Samples from the Natural Fission Reactors in the Oklo Uranium Deposits

1993 ◽  
Vol 333 ◽  
Author(s):  
S. Sunder ◽  
N.H. Miller ◽  
A.M. Duclos

ABSTRACTMineral samples from the natural fission reactors 10 and 13 in the Oklo uranium deposits were studied using X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) to gain information about the long-term behaviour of UO2 fuel in a geological disposal vault. Two samples from reactor zone 10 (samples # D81N-190292 and D73-88) and one sample from reactor zone 13 (sample # SD37-S2/CD) were analysed. Low-resolution XPS spectra were recorded to determine the major elements present in the ore. High-resolution spectra were recorded to gain information about the chemical state of the elements present in the mineral samples. The samples show low values for the U6+/U4+ ratio. The oxidation state of uranium in these samples is even lower than that in U409. The binding energies of the Pb 4f bands indicate most of the Pb is in the +2 oxidation state in these samples. The C Is band indicates the presence of organic carbon. XRD analysis shows that the main uranium-bearing phase is uraninite and lead is present mainly as galena. The significance of the results for nuclear fuel waste management is discussed.

Clay Minerals ◽  
1982 ◽  
Vol 17 (4) ◽  
pp. 477-481 ◽  
Author(s):  
S. Evans ◽  
E. Raftery

It is usually assumed that the oxidation state of the small proportion of Mn sometimes present in micas is +2, although there is evidence from electronic spectroscopy (Burns, 1970) for at least the occasional occurrence of Mn(III) in manganophyllite. We describe here X-ray photoelectron spectroscopic (XPS) measurements on the Mn in a Norwegian lepidolite which was the subject of a concurrent structural study by X-ray photoelectron diffraction (Evans & Raftery, 1982). To establish the Mn oxidation state we have compared the Mn2p core-electron binding energies (BE), the Mn2P3/2-O ls BE differences, and the Mn2p XPS peak profiles from the four common oxides of manganese (MnO, Mn3O4, Mn2O3 and MnO2) with those from the lepidolite. A re-examination of these oxides was undertaken because the agreement between reports in the literature was unsatisfactory, and uncertainty existed concerning the integrity of some of the surfaces previously examined.


1987 ◽  
Vol 41 (6) ◽  
pp. 994-1000 ◽  
Author(s):  
V. Y. Young ◽  
F. C. Chang ◽  
K. L. Cheng

X-ray photoelectron spectroscopy has been used to determine the oxidation state of nickel in the oxidized nickel (II) dimethylglyoxime complex. Core level binding energies for the Ni(2p), N(1s), and O(1s) levels; the presence or absence of shake-up satellites on the Ni(2p) levels; and the analysis of intensity data are consistent only with an assignment of +3. Structures consistent with the data are proposed for both the solid-and the solution-phase complexes.


2019 ◽  
Vol 65 (4 Jul-Aug) ◽  
pp. 345 ◽  
Author(s):  
F. Chale-Lara ◽  
M. Zapata-Torres ◽  
F. Caballero-Briones ◽  
W. De la Cruz ◽  
N. Cruz Gonzalez ◽  
...  

We report the synthesis of AlN hexagonal thin films by pulsed laser ablation, using Al target in nitrogen ambient over natively-oxidized Si (111) at 600°C. Composition and chemical state were determined by X-ray photoelectron spectroscopy (XPS); while structural properties were investigated using X-ray diffraction (XRD). High-resolution XPS spectra present a gradual shift to higher binding energies on the Al2ppeak when nitrogen pressure is incremented, indicating the formation of the AlN compound. At 30 mTorr nitrogen pressure, theAl2p peak corresponds to AlN, located at 73.1 eV, and the XRD pattern shows a hexagonal phase of AlN. The successful formation of the AlN compound is corroborated by UV-Vis reflectivity measurements.


Silicon incorporated carbon nano tube has been synthesized by radio frequency plasma enhanced chemical vapor deposition technique with acetylene gas. Tetraethyl orthosilicate solution was used for the synthesis of silicon incorporation in the CNT thin films. Energy dispersive X-ray analysis shows that the Si atomic percentage in the CNT thin films varied from 0 % to 3.82 %. The different chemical binding energies of carbon and silicon were analyzed from X-ray photoelectron spectroscopy spectra. In the XPS spectra, the peaks at ~531 eV, ~ 285 eV, ~151 eV and ~100 eV are the contributions from O 1s, C 1s, Si 2s and Si 2p respectively. Nanostructure morphologies of the Si-CNT thin films have been analyzed by field emission scanning electron microscopy. The length of the silicon incorporated carbon nano tubes ~100 nm and corresponding diameter ~20 nm. The increase of atomic percentage of Si in the CNT thin films, room temperature electrical conductivity increases. The electrical conductivity increase from 3.87x103 to 4.49x104 S cm-1 as the silicon atomic percentage in the CNT thin films increases from 0 to 3.82 % respectively. This study showed that the Si-CNTs thin films potentially useful in electrical application of varying its conductivity by changing the Si content independently from other parameters


2021 ◽  
Vol 1206 (1) ◽  
pp. 012028
Author(s):  
Sk Faruque Ahmed ◽  
Mohibul Khan ◽  
Nillohit Mukherjee

Abstract Silicon incorporated carbon nanotube (Si-CNTs) thin films was prepared by radio frequency plasma enhanced chemical vapor deposition technique. Tetraethyl orthosilicate solution was used for incorporation of silicon in CNTs thin films. Energy dispersive X-ray analysis shows that the silicon atomic percentage was varied from 0 % to 6.1 %. The chemical binding energies of carbon and silicon were analyzed from X-ray photoelectron spectroscopy data. The various peaks at ~531 eV, ~ 285 eV, ~155 eV and ~104 eV was observed in the XPS spectra due to the oxygen, carbon and silicon respectively. Surface morphologies of Si-CNTs thin films have been analyzed by field emission scanning electron microscopy, which revels that the length of the silicon incorporated carbon nanotubes ~500 nm and corresponding diameter ~80 nm. The room temperature electrical conductivity was increased whereas the activation energy was decreased with the increase of atomic percentage of silicon in Si-CNTs thin films. The room temperature electrical conductivity was increased from 4.3 × 103 to 7.1 × 104 S cm−1 as the silicon atomic percentage in Si-CNTs thin films increases from 0 to 6.1 % respectively.


1993 ◽  
Vol 07 (08) ◽  
pp. 555-564 ◽  
Author(s):  
P. SRIVASTAVA ◽  
N. L. SAINI ◽  
B. R. SEKHAR ◽  
S. K. SHARMA ◽  
H. S. CHAUHAN ◽  
...  

A thin film of superconducting YBa 2 Cu 3 O ~7 (YBCO) system (Tc ~ 89 K ) has been studied by x-ray photoelectron spectroscopy (XPS) to investigate the core level electronic structure. The Ba 3d and 4d core level XPS spectra show three binding energy components with the high binding energy component originating from the non-superconducting surface of the system. The role of oxygen ordering/disordering has been discussed to explain the origin of the other two bulk-dependent components. An attempt has been made to resolve some of the discrepancies in the Ba core level spectra reported earlier.


2009 ◽  
Vol 2009 ◽  
pp. 1-8 ◽  
Author(s):  
Valentina Krylova ◽  
Mindaugas Andrulevičius

Copper sulfide layers were formed on polyamide PA 6 surface using the sorption-diffusion method. Polymer samples were immersed for 4 and 5 h in 0.15 mol⋅  solutions and acidified with HCl (0.1 mol⋅) at . After washing and drying, the samples were treated with Cu(I) salt solution. The samples were studied by UV/VIS, X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) methods. All methods confirmed that on the surface of the polyamide film a layer of copper sulfide was formed. The copper sulfide layers are indirect band-gap semiconductors. The values of are 1.25 and 1.3 eV for 4 h and 5 h sulfured PA 6 respectively. Copper XPS spectra analyses showed Cu(I) bonds only in deeper layers of the formed film, while in sulfur XPS S 2p spectra dominating sulfide bonds were found after cleaning the surface with ions. It has been established by the XRD method that, beside , the layer contains as well. For PA 6 initially sulfured 4 h, grain size forchalcocite, , was  nm and fordjurleite, , it was 54.17 nm. The sheet resistance of the obtained layer varies from 6300 to 102 .


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.


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.


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