Development of a differential pumping system for soft X-ray beamlines for windowless experiments under normal atmospheric conditions

Tamenori, Y.

doi:10.1107/s0909049509052571

Cited by 17 publications

(8 citation statements)

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“…These principally arise from the increased scattering and absorption events that lower-energy X-rays will be subject to, that result in a much reduced ability to penetrate matter. Developing methods (see, for instance, Tamenori, 2010Tamenori, , 2013Tamenori et al, 2011) or sample environment suitable for the study of any given process at these energies is therefore subject to considerably more constraints (both in terms of design and materials) than is the case at high energies. However, several examples exist for the study of gas-solid chemistry and catalysis (see, for example, van der Eerden et al, 2000;Hayter et al, 2002;Dathe et al, 2005;Nurk et al, 2013;Bolin et al, 2013;Kö nig et al, 2014) and studies using a liquid media (Brown et al, 2012;Fulton et al, 2012;Pin et al, 2013).…”

Section: Introductionmentioning

confidence: 99%

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al₂O₃

Thompson

Nguyen

Nicholls

et al. 2015

J Synchrotron Radiat

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Synopsis:The performance of the XMaS beamline for soft X-ray spectroscopy in the 2-4 keV range is assessed with particular relation to in situ studies of functional materials and their chemistry. X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in c-Al 2 O 3 How to cite your article in pressYour article has not yet been assigned page numbers, but may be cited using the doi:Thompson, P.B.J., Nguyen, B.N., Nicholls, R., Bourne, R.A., Brazier, J.B., Lovelock, K.R.J., Brown, S.D., Wermeille, D., Bikondoa, O., Lucas, C.A. et al. (2015). J. Synchrotron Rad. 22, doi:10.1107/S1600577515016148.You will be sent the full citation when your article is published and also given instructions on how to download an electronic reprint of your article. Proof instructionsProof corrections should be returned by 22 September 2015. After this period, the Editors reserve the right to publish your article with only the Managing Editor's corrections. Please(1) Read these proofs and assess whether any corrections are necessary.(2) Check that any technical editing queries highlighted in bold underlined text have been answered. (3) Send corrections by e-mail to tw@iucr.org. Please describe corrections using plain text, where possible, giving the line numbers indicated in the proof. Please do not make corrections to the pdf file electronically and please do not return the pdf file. If no corrections are required please let us know.If you wish to make your article open access or purchase printed offprints, please complete the attached order form and return it by e-mail as soon as possible. Thumbnail image for contents pageFiles: s/rv5038/rv5038.3d s/rv5038/rv5038.sgml RV5038 FA IU-1517/10(15)9 1516/52(15)9 () RV5038 http://dx.doi.org/10.1107/S1600577515016148 1 of 14 The 2-4 keV energy range provides a rich window into many facets of materials science and chemistry. Within this window, P, S, Cl, K and Ca K-edges may be found along with the L-edges of industrially important elements from Y through to Sn. Yet, relative to those that cater for energies above ca. 4-5 keV, there are relatively few resources available for X-ray spectroscopy below these energies. In addition, in situ or operando studies become to varying degrees more challenging than at higher X-ray energies due to restrictions imposed by the lower energies of the X-rays upon the design and construction of appropriate sample environments. The XMaS beamline at the ESRF has recently made efforts to extend its operational energy range to include this softer end of the X-ray spectrum. In this report the resulting performance of this resource for X-ray spectroscopy is detailed with specific attention drawn to: understanding electrostatic and charge transfer effects at the S K-edge in ionic liquids; quantification of dilution limits at the Cl K-and Rh L 3 -edges and structural equilibria in solution; in vacuum deposition and reduction of [Rh I (CO) 2 Cl] 2 to -Al 2 ...

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Section: Introductionmentioning

confidence: 99%

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al₂O₃

Thompson

Nguyen

Nicholls

et al. 2015

J Synchrotron Radiat

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“…[43] Ni L II -a nd L IIIedge (844-876 eV) and OK -edge (525-533 eV) X-ray absorption spectra under electrochemical polarization were recorded by the fluorescence yielding mode in order not to disturb the electrochemical measurement. Co., Ltd.) was pressed into ad isc shape and sintered at 1823 Kf or 6h.…”

Section: Methodsmentioning

confidence: 99%

“…The upstream chambers were evacuated by the differential pumping system. [43] Ni L II -a nd L IIIedge (844-876 eV) and OK -edge (525-533 eV) X-ray absorption spectra under electrochemical polarization were recorded by the fluorescence yielding mode in order not to disturb the electrochemical measurement. EIS and steady-state polarization measurements were also carried out with the same electrochemical cell by apotentiostat (VersaStat 4, Princeton Applied Research).…”

Section: Methodsmentioning

confidence: 99%

Operando Soft X‐ray Absorption Spectroscopic Study on a Solid Oxide Fuel Cell Cathode during Electrochemical Oxygen Reduction

et al. 2017

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An operando soft X-ray absorption spectroscopic technique, which enabled the analysis of the electronic structures of the electrode materials at elevated temperature in a controlled atmosphere and electrochemical polarization, was established and its availability was demonstrated by investigating the electronic structural changes of an La NiO dense-film electrode during an electrochemical oxygen reduction reaction. Clear O K-edge and Ni L-edge X-ray absorption spectra could be obtained below 773 K under an atmospheric pressure of 100 ppm O /He, 0.1 % O /He, and 1 % O /He gas mixtures. Considerable spectral changes were observed in the O K-edge X-ray absorption spectra upon changing the PO2 and application of electrical potential, whereas only small spectral changes were observed in Ni L-edge X-ray absorption spectra. A pre-edge peak of the O K-edge X-ray absorption spectra, which reflects the unoccupied partial density of states of Ni 3d-O 2p hybridization, increased or decreased with cathodic or anodic polarization, respectively. The electronic structural changes of the outermost orbital of the electrode material due to electrochemical polarization were successfully confirmed by the operando X-ray absorption spectroscopic technique developed in this study.

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“…Soft XAS measurements were performed at the beam line of BL27SU at SPring-8, JASRI, Japan. The system for soft XAS under controlled atmosphere at elevated temperature was developed based on the differential pumping system for soft XAS under normal atmospheric conditions by Tamenori [4]. In order to control partial gas pressures while ensuring the sufficient incident X-ray, the sample chamber was separated from the optical upstream part with an Si 3 N 4 thin film window of 500 nm.…”

Section: Soft X-ray Absorption Spectroscopymentioning

confidence: 99%

Development of in situ soft X-ray absorption spectroscopic technique under high temperature and controlled atmosphere

et al. 2014

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Development of a differential pumping system for soft X-ray beamlines for windowless experiments under normal atmospheric conditions

Cited by 17 publications

References 25 publications

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al₂O₃

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al₂O₃

Operando Soft X‐ray Absorption Spectroscopic Study on a Solid Oxide Fuel Cell Cathode during Electrochemical Oxygen Reduction

Development of in situ soft X-ray absorption spectroscopic technique under high temperature and controlled atmosphere

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Development of a differential pumping system for soft X-ray beamlines for windowless experiments under normal atmospheric conditions

Cited by 17 publications

References 25 publications

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al2O3

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al2O3

Operando Soft X‐ray Absorption Spectroscopic Study on a Solid Oxide Fuel Cell Cathode during Electrochemical Oxygen Reduction

Development of in situ soft X-ray absorption spectroscopic technique under high temperature and controlled atmosphere

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X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al₂O₃

X-ray spectroscopy for chemistry in the 2-4 keV energy regime at the XMaS beamline: ionic liquids, Rh and Pd catalysts in gas and liquid environments, and Cl contamination in γ-Al₂O₃