Combined QuEXAFS-XRD: a new technique in high-temperature materials chemistry; an illustrative in situ study of the zinc oxide-enhanced solid-state production of cordierite from a precursor zeolite

Sankar, Gopinathan; Wright, Paul A.; Natarajan, Srinivasan; Thomas, John Meurig; Greaves, G. Neville; Dent, Andrew J.; Dobson, B. R.; Ramsdale, Christine A.; Jones, Richard H.

doi:10.1021/j100140a002

Cited by 148 publications

(102 citation statements)

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“…To make it a real working system, the three-detector systems should be synchronized. The feasibility of this type of technique combination has been shown (Sankar et al, 1993). Another technique that might become possible is time-resolved anomalous X-ray scattering with an estimated time resolution of 1-5 s per frame.…”

Section: Discussionmentioning

confidence: 99%

Time-Resolved Small-Angle X-ray Scattering Combined with Wide-Angle X-ray Scattering

Bras¹,

Ryan²

1997

J Appl Cryst

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The high X-ray intensity of synchrotron radiation (SR) beamlines makes it possible to perform time-resolved small-angle X-ray scattering (SAXS) experiments. The information that can be obtained by collecting the wideangle diffraction pattern simultaneously not only increases the information content of an experiment but also increases the reliability of the time-correlations between SAXS and WAXS (wide-angle X-ray scattering) patterns. This is a great advantage for experiments with a time resolution below the level of 1 s per frame. With appropriate instrumentation, this is a time domain that is routinely accessible for a large group of research fields. This has had a considerable impact upon the understanding of fundamental aspects of phase transformations. Not only fundamental processes but also more applied fields have benefited from these developments. In polymer research this has led to a situation in which it has become possible to simulate materials processing techniques on-line. With the advent of thirdgeneration synchrotron-radiation sources (e.g. ESRF, APS, Spring8), it has become possible to develop SAXS/WAXS beamlines that will open up new research opportunities by utilizing the higher intensity, the tuneability and the higher collimation offered by these SR sources. However, some of the instrumentation limits in detector and sample environments that have become apparent in research on second-generation synchrotron-radiation sources still have not been appropriately addressed, which means that in some fields it will not be possible to take full advantage of the superior X-ray beam quality that third-generation synchrotrons can offer. A way in which these instrumentation limits can be overcome is discussed, and the instrumentation for a new bending-magnet beamline at the ESRF is used as an example.

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Section: Discussionmentioning

confidence: 99%

Time-Resolved Small-Angle X-ray Scattering Combined with Wide-Angle X-ray Scattering

Bras¹,

Ryan²

1997

J Appl Cryst

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“…For the time-resolved SAXS/WAXS experiments the sample was placed in a furnace of which the temperature can be controlled with an accuracy of ±2 °C with a maximum estimated temperature gradient over the sample of the same magnitude 15 .…”

Section: Methodsmentioning

confidence: 99%

Nanocrystal Growth in Cordierite Glass Ceramics Studied with X-ray Scattering

Bras

Clark

Greaves

et al. 2009

Crystal Growth & Design

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The development of mono-disperse crystalline particles in cordierite glass doped with Cr 3+ after a two step heat treatment is elucidated by a combination of time-resolved SAXS/WAXS experiments andwith electron microscopy. The effects of bulk and surface crystallization can clearly be distinguished and the crystallization kinetics of the bulk phase is characterized. The internal pressure due to structural differences between the crystalline and amorphous phase is measured but the physical cause of this 3 pressure can not unambiguously be attributed. The combined measurements comprise a nearly full characterization of the crystallization processes and the resulting sample morphology.

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“…In addition to studying a catalytically active material under dynamic reaction conditions, structural evolution during the preparation of the active catalysts from a precursor material has been monitored by TR-XAS, employing either a DXAS spectrometer [51,52,53,54,55,56,57,58] or the QEXAFS mode at a conventional XAS beamline [59]. Because controlled thermal treatment of a precursor material permits better tailoring of the time-resolution required, a time-resolution in the minute range was employed in many of the studies resulting in a sufficient data quality to perform a detailed EXAFS analysis.…”

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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Combined QuEXAFS-XRD: a new technique in high-temperature materials chemistry; an illustrative in situ study of the zinc oxide-enhanced solid-state production of cordierite from a precursor zeolite

Cited by 148 publications

References 1 publication

Time-Resolved Small-Angle X-ray Scattering Combined with Wide-Angle X-ray Scattering

Time-Resolved Small-Angle X-ray Scattering Combined with Wide-Angle X-ray Scattering

Nanocrystal Growth in Cordierite Glass Ceramics Studied with X-ray Scattering

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

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