Corrosion of Mo in KOH:  Time Resolved XAFS Investigations

and, Dirk Lützenkirchen-Hecht; Frahm, R.

doi:10.1021/jp003414n

Cited by 29 publications

(17 citation statements)

References 37 publications

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“…Let us quote the case of V 2 O 5 , 82 VO 2 , 83 MnO, 84 copper oxide related systems, 85 and Mo oxide. 86 Finally, we can consider also sulfur compounds as well as nanocrystalline cerium oxides. 87 As we have already seen, 88 this part of the X-ray absorption spectrum is sensitive to the size of the MoS 2 crystallite.…”

Section: Discussionmentioning

confidence: 99%

Limits and Advantages of X-ray Absorption Near Edge Structure for Nanometer Scale Metallic Clusters

2003

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International audienceWe consider the analysis of the K edge of 3d or 4d transition metals when nanometer-scale metallic clusters are considered. From a practical point of view, numerical simulation of the XANES part of the K absorption spectrum of most elements of the periodic table can be performed through full multiple scattering calculations. Then, on the basis of a linear combination of the XANES spectra of reference compounds, the presence of the different phases present inside the materials can be quantified. Here, we show that for nanometer scale metallic clusters, it is not sufficient to consider only the electronic state of the metal of interest to perform a linear combination analysis. In the case of these peculiar materials, special attention has to be paid to different structural parameters, for example, the size and morphology of the cluster, the interatomic distance (taking into account contraction/dilatation processes), and the presence of heterometallic bonds (in the case of bimetallic clusters). Moreover, this approach is not specific to the metallic state. As a conclusion, the quantitative measurement of the structural parameters coming from EXAFS analysis constitutes an invaluable starting point for the FEFF-PCA simulation. The fact that major results coming from the emergence of dynamical studies, namely, Quick-EXAFS or energy dispersive EXAFS, are now obtained will lead to significant breakthroughs in the understanding of the genesis/reactivity of nanometer-scale entities

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Section: Discussionmentioning

confidence: 99%

Limits and Advantages of X-ray Absorption Near Edge Structure for Nanometer Scale Metallic Clusters

2003

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“…A comparable number of studies employed DXAS or QEXAFS to monitor the evolution of phase composition and the short-range order structure of the materials during solid-gas reactions [60,61,62,63], solid-solid reactions [62,63,64,65,66], phase transformations [67,68,69,70], thermal treatments [71,72,73,74,75,76], and solid combustion syntheses [77]. The third largest fraction of investigations using TR-XAS falls in the area of electrochemistry, with a comparable number of studies employing DXAS [78,79,80] or conventional QEXAFS [81] or QEXAFS in the reflection mode [82,83]. There have been few reports of the use of TR-XAS to study reactions in the liquid phase [84] or under environmentally relevant conditions [85].…”

Section: Applications Of Tr-xasmentioning

confidence: 99%

Application of time-resolved in-situ X-ray absorption spectroscopy in solid-state chemistry

Ressler

2003

Analytical and Bioanalytical Chemistry

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Time-resolved X-ray absorption spectroscopy (TR-XAS) possesses excellent capabilities to reveal quantitative phase composition and average valence together with the evolution of the local structure of a system under dynamic reaction conditions. The work discussed here focused on time-resolved in situ XAS investigations aiming, first, at understanding structural evolution under dynamic conditions and, second, at revealing properties of the system studied not available from investigations under stationary conditions. Hence, not only was the local structure of a material studied under reaction conditions, but also were characteristic properties of the reaction elucidated, such as reaction intermediates or the kinetics of the reaction. The solid-gas reactions presented here clearly demonstrate the potential of TR-XAS investigations to extend the suitability of XAS for in situ studies in solid-state chemistry to investigations under dynamic conditions.

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“…Synchrotrons provide intense, monochromatic, beams of x-rays containing 10 4 or more times the flux from a laboratory source, and allow the user to select an energy in the 1 -100 keV range.…”

Section: Introductionmentioning

confidence: 99%

“…x-ray absorption spectrocopy (XAS) [2][3][4][5] , transmission x-ray microscopy 6 , and x-ray diffraction (XRD) [7][8][9] or some combination 10 . X-rays can penetrate a thickness of liquid which increases with energy, and which is a millimetre or more from energies of a few keV upwards.…”

Section: Introductionmentioning

confidence: 99%

The Use of Synchrotron X-rays To Observe Copper Corrosion in Real Time

Dowsett¹,

Adriaens²,

Martin³

et al. 2012

Anal. Chem.

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We have developed and tested two complementary methods for making time-lapse synchrotron X-ray diffraction (XRD) measurements of the growth of synthetic corrosion layers using a protocol for producing copper (I) chloride (nantokite), on copper as a test. In the first method a copper coupon was spin-coated with saturated copper (II) chloride solution in air whilst the surface was characterized in real time using XRD with a fast 1-D detector. In the second, a droplet of the same reagent was suspended from an X-ray transparent window in a hermetically sealed cell and the coupon was brought into contact with this whilst XRD diffractograms were acquired with a CCD camera. The protocol is completed by a deionized water rinse which was also studied. The XRD shows nantokite precipitation in solution as well as growth on the surface, but the end products were variable proportions of nantokite cuprite, and paratacamite.The latter two were observed forming in a reaction between the nantokite and the rinsing water.Comparisons between samples analyzed in the synchrotron and at lower power densities show that the effects of any radiolysis or slight heating of the sample are insignificant in this case. It would be simple to extend these methods to other corrosion or surface reaction systems.

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Corrosion of Mo in KOH: Time Resolved XAFS Investigations

Cited by 29 publications

References 37 publications

Limits and Advantages of X-ray Absorption Near Edge Structure for Nanometer Scale Metallic Clusters

Limits and Advantages of X-ray Absorption Near Edge Structure for Nanometer Scale Metallic Clusters

Application of time-resolved in-situ X-ray absorption spectroscopy in solid-state chemistry

The Use of Synchrotron X-rays To Observe Copper Corrosion in Real Time

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