ROBL – a CRG beamline for radiochemistry and materials research at the ESRF

Matz, W.; Schell, Norbert; Bernhard, Gert; Prokert, F.; Reich, Tobias; Claußner, J.; Oehme, Wolfgang; Schlenk, R.; Dienel, S.; Funke, H.; Eichhorn, F.; Betzl, M.; Pröhl, D.; Strauch, U.; Hüttig, Gudrun; Krug, Hans; Neumann, W.; Brendler, Vinzenz; Reichel, P.; Denecke, Melissa A.; Nitsche, H.

doi:10.1107/s0909049599010663

Cited by 192 publications

(119 citation statements)

References 27 publications

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“…Bulk-EXAFS spectra at the U L III edge (17 166 eV) were collected at room temperature at BM 20 (ROBL) at the European Synchrotron Radiation Facility (ESRF) in Grenoble, France [15]. The beamline is equipped with a water-cooled Si(111) double crystal monochromator between Pt-coated mirrors for beam collimation and rejection of higher order harmonics.…”

Section: Bulk-and μ-Exafs Data Collection and Reductionmentioning

confidence: 99%

EXAFS investigation on U(VI) immobilization in hardened cement paste: influence of experimental conditions on speciation

Macé¹,

Wieland²,

Dähn³

et al. 2013

Radiochimica Acta

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U(VI) / Speciation / Cement / (Micro-)EXAFSSummary. Extended X-ray absorption fine structure (EXAFS) spectroscopy has been used to investigate the coordination environment of U(VI) in cementitious materials. The EXAFS measurements were carried out on U(VI)-doped samples prepared under varying conditions, such as samples from sorption, hydration and diffusion experiments, and using different cementitious materials, such as crushed hardened cement paste (HCP) and calcium silicate hydrates (C-S-H). The samples had U(VI) loadings ranging from 1700 μg/g to 45 000 μg/g. Applying principal component analysis (PCA) on 13 EXAFS spectra (each spectra corresponding to a minimum of five different scans) of the low loading samples, one single species is obtained indicating a similar U(VI) coordination environment for both HCP and C-S-H samples. This result confirms that C-S-H phases control the uptake of U(VI) in the complex cement matrix. The coordination environment of this species is similar to a U(VI) surface complex or to U(VI) in uranyl silicate minerals (two axial O atoms at 1.82 ± 0.02 Å; four equatorial O atoms at 2.25 ± 0.01 Å; one Si atom at 3.10 ± 0.03 Å). At high U(VI) loading, PCA revealed a second U(VI) species, with a coordination environment similar to that of U(VI) in calcium uranate (two axial O atoms at 1.94 ± 0.04 Å; five equatorial O atoms at 2.26 ± 0.01 Å; four Ca atoms at 3.69 ± 0.05 Å and five U atoms at 3.85 ± 0.04 Å).

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Section: Bulk-and μ-Exafs Data Collection and Reductionmentioning

confidence: 99%

EXAFS investigation on U(VI) immobilization in hardened cement paste: influence of experimental conditions on speciation

Macé¹,

Wieland²,

Dähn³

et al. 2013

Radiochimica Acta

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“…Europium L III -edge X -ray absorption spectra at 6976.9 eV were recorded at room temperature at the R ossendorf Beamline (ROBL) [26], ERSF Grenoble, in fluorescence (EuPAA ads ) or transmission (EuAc 3 .xH 2 0 and EuPAA) modes. For the fluorescence measurements, a 4-pixel Ge solid state detector was used.…”

Section: Introductionmentioning

confidence: 99%

Comparison of complexed species of Eu in alumina-bound and free polyacrylic acid: A spectroscopic study

Montavon

Hennig

Janvier

et al. 2006

Journal of Colloid and Interface Science

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The speciation of Eu complexed with polyacrylic acid (PAA) and alumina-bound PAA (PAA ads ) was studied at pH=5 in 0.1M NaClO 4 . Structural parameters were obtained from 7 coordination. The results show that the degree of freedom of carboxylate groups is not the same for free or adsorbed PAA. For PAA, the degree of freedom is constrained by the flexibility of the methylene chain. When PAA is adsorbed on alumina, the polymer chains cannot any more be treated as independent chains. One may rather assume formation of aggregates that form an organic layer at the mineral surface presenting a complex arrangement of carboxylate groups.

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“…13 The post-deposition annealing of identical ITO samples was carried out at two different experimental setups, the ROssendorf Beam Line (ROBL) at the European Synchrotron Radiation Facility in Grenoble, [14] and the ITO deposition facility at Forschungszentrum Rossendorf [13]. In both cases the total pressure of the residual gas was below 6 × 10 -4 Pa. During annealing the sample was placed on a boralectric heater (Tectra, Germany).…”

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confidence: 99%

Real-time evolution of the indium tin oxide film properties and structure during annealing in vacuum

Rogozin

Shevchenko

Vinnichenko

et al. 2004

Applied Physics Letters

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Indium tin oxide (ITO) is widely applied as a transparent conductive oxide coating. A standard and successful industrial route of production is its deposition by magnetron sputtering from a compound (oxide) target [1]. To increase cost efficiency, it would be preferable to sputter reactively from a metal target at sufficiently high partial pressure of oxygen. However, under this condition, a satisfactorily low resistivity of the films cannot readily be obtained, [2] so that a deposition on heated substrates or post-deposition annealing is necessary. So far, the annealing processes for reactively sputtered ITO [3,4] have only been studied for metal-rich films, in contrast to comprehensive studies after magnetron sputtering from ceramic targets [5][6][7][8][9][10]. Moreover, mainly isothermal heat treatment is considered in the literature, although annealing using a temperature ramp is of more relevance for practical application. Several investigations report on real-time in situ monitoring of the ITO film resistivity and reflectivity [9,10], which is used for an indirect characterization of the crystalline structure of the films. This approach requires simplifying assumptions on the linear dependence of the resistivity or reflectivity on the crystalline fraction, and the stability of the film roughness during annealing. Direct investigations of the influence of heat treatment on the ITO film structure are so far limited to post-annealing studies by X-ray diffraction (XRD) and scanning or transmission electron microscopy [3][4][5]7,8,11].Annealing of ITO is known to be very efficient in increasing the carrier concentration. It can be quite reasonably explained by the FrankKöstlin model [12] which accounts for tin donor activation at elevated temperatures. However, this model is valid only for crystalline ITO. The amorphous-to-crystalline transition in ITO during annealing is often assumed as the reason for this activation, but the physics behind the experimental observation is not clear. In the present letter we report the results of a real-time in situ investigation of the film properties and the structure evolution during annealing in vacuum.The films are produced by reactive pulsed middle frequency magnetron sputtering using the facility and procedure described in Ref. 13. The chamber was pumped to a base pressure of 4 × 10 -4 Pa before deposition. The deposition runs were carried out for 2.5 min at an Ar flow of 30 sccm (partial pressure 1.2 Pa) and O 2 flow of 64 sccm (0.3 Pa). The films are grown on Si (100) substrates (24 × 12 × 0.3 mm 3 ) covered with SiO 2 (510 nm), which were not heated externally during deposition. The average thickness of the deposited films is 130 nm. The as-deposited films show no crystalline peaks in the XRD patterns and are considered as amorphous.The post-deposition annealing of identical ITO samples was carried out at two different experimental setups, the ROssendorf Beam Line (ROBL) at the European Synchrotron Radiation Facility in Grenoble, [14] and the ITO deposition facility ...

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ROBL – a CRG beamline for radiochemistry and materials research at the ESRF

Cited by 192 publications

References 27 publications

EXAFS investigation on U(VI) immobilization in hardened cement paste: influence of experimental conditions on speciation

EXAFS investigation on U(VI) immobilization in hardened cement paste: influence of experimental conditions on speciation

Comparison of complexed species of Eu in alumina-bound and free polyacrylic acid: A spectroscopic study

Real-time evolution of the indium tin oxide film properties and structure during annealing in vacuum

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