scholarly journals Preliminary investigation of chlorine speciation in zirconolite glass-ceramics for plutonium residues by analysis of Cl K-edge XANES

MRS Advances ◽  
2019 ◽  
Vol 5 (1-2) ◽  
pp. 37-43
Author(s):  
Amber R. Mason ◽  
Stephanie M. Thornber ◽  
Martin C. Stennett ◽  
Laura J. Gardner ◽  
Dirk Lützenkirchen-Hecht ◽  
...  
Keyword(s):  
Chemical Shift ◽  
Absorption Edge ◽  
Glass Ceramic ◽  
Glass Phase ◽  
Preliminary Investigation ◽  
Glass Ceramics ◽  
Local Environment ◽  
Aluminosilicate Glass ◽  
X Ray ◽  
X Ray Absorption

ABSTRACTA zirconolite glass-ceramic material is a candidate wasteform for immobilisation of chlorine contaminated plutonium residues, in which plutonium and chlorine are partitioned to the zirconolite and aluminosilicate glass phase, respectively. A preliminary investigation of chlorine speciation was undertaken by analysis of Cl K-edge X-ray Absorption Near Edge Spectroscopy (XANES), to understand the incorporation mechanism. Cl was found to be speciated as the Cl- anion within the glass phase, according to the characteristic chemical shift of the X-ray absorption edge. By comparison with Cl K-edge XANES data acquired from reference compounds, the local environment of the Cl- anion is most closely approximated by the mineral marialite, in which Cl is co-ordinate to 4 x Na and/or Ca atoms.

scholarly journals Formation of nanostructures in Eu3+ doped glass–ceramics: an XAS study

2014 ◽  
Vol 70 (a1) ◽  
pp. C959-C959
Author(s):  
Julio Pellicer-Porres ◽  
Alfredo Segura ◽  
Gema Martínez-Criado ◽  
Ulises Rodríguez-Mendoza ◽  
Víctor Lavín
Keyword(s):  
Amorphous Phase ◽  
Glass Ceramic ◽  
Glass Ceramics ◽  
Aluminosilicate Glass ◽  
Chemical Information ◽  
Nanocrystalline Phase ◽  
X Ray Diffraction ◽  
Oxyfluoride Glass ◽  
X Ray ◽  
X Ray Absorption

Lead-aluminosilicate oxyfluoride transparent glass–ceramics doped with RE3+ ions have been revealed to be unique in the field of optical material engineering. This kind of material consists of a beta_x000C_-PbF2 fluoride nanocrystalline phase in an aluminosilicate glassy amorphous phase. In this way, the macroscopic properties of this material are characteristic of aluminosilicate glass, whereas the spectroscopic properties of the RE3+ ions remain those of low-phonon-energy fluoride crystals. The optical properties of the RE3+ ions, and therefore their interest for photonic applications, depend on the final environment of these ions in a host matrix. Exploration of the local structure of the Eu3+ ions as well as characterization of the amorphous matrix demands structural techniques that do not rely on long range order. Given the complexity of the system under study, chemical selectivity is also required. In this work [1], we describe the results of x-ray absorption experiments carried out to deduce structural and chemical information in Eu3+ doped, transparent, oxyfluoride glass and nanostructured glass–ceramic samples. The spectra were measured at the Pb and Eu–LIII edges. The Eu environment in the glass samples is observed to be similar to that of EuF3. Complementary x-ray diffraction experiments show that thermal annealing creates _x000C_beta-PbF2 type nanocrystals. X-ray absorption indicates that Eu ions act as seeds in the nanocrystal formation. There is evidence of interstitial fluorine atoms around Eu ions as well as Eu dimers. X-ray absorption at the Pb–LIII edge shows that after the thermal treatment most lead atoms form a PbO amorphous phase and that only 10% of the lead atoms remain available to form _x000C_beta-PbF2 type nanocrystals. Both x-ray diffraction and absorption point to a high Eu content in the nanocrystals. Our study suggests new approaches to the oxyfluoride glass–ceramic synthesis in order to further improve their properties.

scholarly journals Structure of NaFeSiO4, NaFeSi2O6, and NaFeSi3O8 glasses and glass-ceramics

2020 ◽  
Vol 105 (9) ◽  
pp. 1375-1384 ◽  
Author(s):  
Mostafa Ahmadzadeh ◽  
Alex Scrimshire ◽  
Lucy Mottram ◽  
Martin C. Stennett ◽  
Neil C. Hyatt ◽  
...  
Keyword(s):  
Glass Phase ◽  
Redox State ◽  
Glass Ceramics ◽  
Isothermal Heat Treatment ◽  
X Ray ◽  
Heat Treated ◽  
High Level ◽  
Iron Redox ◽  
X Ray Absorption ◽  
Iron Redox State

Abstract The crystallization of iron-containing sodium silicate phases holds particular importance, both in the management of high-level nuclear wastes and in geosciences. Here, we study three as-quenched glasses and their heat-treated chemical analogs, NaFeSiO4, NaFeSi2O6, and NaFeSi3O8 (with nominal stoichiometries from feldspathoid, pyroxene, and feldspar mineral groups, i.e., Si/Fe = 1, 2, and 3, respectively) using various techniques. Phase analyses revealed that as-quenched NaFeSiO4 could not accommodate all Fe in the glass phase (some Fe crystallizes as Fe3O4), whereas as-quenched NaFeSi2O6 and NaFeSi3O8 form amorphous glasses. NaFeSi2O6 glass is the only composition that crystallizes into its respective isochemical crystalline polymorph, i.e., aegirine, upon isothermal heat-treatment. As revealed by Mössbauer spectroscopy, iron is predominantly present as fourfold-coordinated Fe3+ in all glasses, though it is present as sixfold-coordinated Fe3+ in the aegirine crystals (NaFeSi2O6), as expected from crystallography. Thus, Na-Fe silicate can form a crystalline phase in which it is octahedrally coordinated, even though it is mostly tetrahedrally coordinated in the parent glasses. Thermal behavior, magnetic properties, iron redox state (including Fe K-edge X-ray absorption), and vibrational properties (Raman spectra) of the above compositions are discussed.

Calculation of the density of compounds from the chemical shift of the X-ray absorption edge

1982 ◽  
Vol 70 (2) ◽  
pp. K107-K111 ◽  
Author(s):  
V. Kumar ◽  
A. R. Chetal ◽  
K. S. Srivastava
Keyword(s):  
Chemical Shift ◽  
Absorption Edge ◽  
X Ray ◽  
X Ray Absorption

scholarly journals Study of the effect of Ca/Mg alkali-oxides ratio on the structure of a glass-ceramic based on an aluminosilicated glass containing 2wt.% of zirconolite crystalline phase

2014 ◽  
Vol 46 (3) ◽  
pp. 377-383
Author(s):  
R. Souag ◽  
N. Kamel ◽  
Y. Mouheb ◽  
M. Hammadi ◽  
Z. Kamel ◽  
...  
Keyword(s):  
Glass Ceramic ◽  
Glass Ceramics ◽  
Xrd Analysis ◽  
Aluminosilicate Glass ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electron Microscopy Analysis ◽  
Microscopy Analysis ◽  
Alkali Oxides ◽  
Scanning Electron

New nuclear glass-ceramics are extensively studied for the radioactive waste confinement, due to the double confinement conferred by the glass-ceramics. In this study, a glass-ceramic constituted by an aluminosilicate glass in the system: SiO2-Al2O3-CaO-MgOZrO2-TiO2, containing 2wt.% of Ca0.83Ce0.17ZrTi1.66Al0.34O7 zirconolite, has been synthesized by the discontinuous method. Cerium, an actinide surrogate is introduced both in the glass and ceramic phases. The synthesis is performed by a double melting at 1350?C, followed by a nucleation at 564?C, during 2 h, and a crystal growth at 1010?C during 3 h. Then effect of Ca/Mg ratio on the distribution of the crystalline network in the material was studied for Ca / Mg ratios ranging from 0.4 to 5.5. For the whole of the materials, Archimedes density is about 2.80 g/cm3. X-ray diffraction (XRD) analysis shows that the increase of Ca/Mg ratio leads to the increase of aluminosilicated crystalline phases with high Ca contents; the materials molar volumes remaining constant. The zirconolite phase is not affected by these additive aluminosilicated phases. The scanning electron microscopy analysis (SEM) coupled with energy dispersive X-ray (EDX) analysis confirmed these results; and shows the uniformity of distribution of the ceramics in the bulk of the materials.

Differential anomalous wide-angle X-ray scattering and X-ray absorption experiments to investigate the formation of glass ceramics in the CaO–SiO2–ZrO2system

1999 ◽  
Vol 32 (6) ◽  
pp. 1090-1099 ◽  
Author(s):  
Carlo Meneghini ◽  
Alessandro F. Gualtieri ◽  
Cristina Siligardi
Keyword(s):  
Glass Ceramic ◽  
Room Temperature ◽  
Glass Ceramics ◽  
Anomalous Scattering ◽  
X Ray Diffraction ◽  
X Ray ◽  
X Ray Scattering ◽  
Two Samples ◽  
Devitrification Process ◽  
X Ray Absorption

The structure of a CaO–SiO2–ZrO2-based glass ceramic has been investigated by X-ray diffraction, X-ray absorption spectroscopy and differential anomalous scattering techniques as a function of the thermal treatment of the sample. The microstructure of the glass has been investigated at room temperature, before the recrystallization of the glass ceramic, and on two samples annealed at 1073 and 1273 K for 1 h to follow the early stages of nucleation of the quartz and wollastonite crystalline phases. Indications on the roles of Ca, Si and Zr during the devitrification process are given.

X-Ray absorption edge elemental imaging of B. thuringienis

1989 ◽  
Vol 47 ◽  
pp. 212-213
Author(s):  
R. L. Stears
Keyword(s):  
Absorption Edge ◽  
Elemental Distribution ◽  
X Rays ◽  
Differential Absorption ◽  
Synchrotron Source ◽  
High Brightness ◽  
X Ray ◽  
Elemental Imaging ◽  
Cellular Integrity ◽  
X Ray Absorption

Because of the nature of the bacterial endospore, little work has been done on analyzing their elemental distribution and composition in the intact, living, hydrated state. The majority of the qualitative analysis entailed intensive disruption and processing of the endospores, which effects their cellular integrity and composition.Absorption edge imaging permits elemental analysis of hydrated, unstained specimens at high resolution. By taking advantage of differential absorption of x-ray photons in regions of varying elemental composition, and using a high brightness, tuneable synchrotron source to obtain monochromatic x-rays, contact x-ray micrographs can be made of unfixed, intact endospores that reveal sites of elemental localization. This study presents new data demonstrating the application of x-ray absorption edge imaging to produce elemental information about nitrogen (N) and calcium (Ca) localization using Bacillus thuringiensis as the test specimen.

Evidence of x-ray absorption-edge shift as a function of luminescence wavelength in porous silicon

2000 ◽  
Vol 62 (15) ◽  
pp. 9911-9914 ◽  
Author(s):  
G. Dalba ◽  
N. Daldosso ◽  
P. Fornasini ◽  
M. Grimaldi ◽  
R. Grisenti ◽  
...  
Keyword(s):  
Porous Silicon ◽  
Absorption Edge ◽  
X Ray ◽  
Absorption Edge Shift ◽  
X Ray Absorption
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