X-Ray Absorption Spectroscopy as an in-situ Tool in Materials Science

1997 ◽  
Vol 502 ◽  
Author(s):  
T. Ressler ◽  
Joe Wong ◽  
W. Metz

ABSTRACTIn addition to being an established technique for ex-situ structural studies, x-ray absorption spectroscopy (XAS) has recently been realized to be a powerful tool for in-situ time-resolved investigations in materials science. This paper describes two complementary techniques: quick-scanning EXAFS (QEXAFS) and energy-dispersive XAS (DXAS) which offer time resolution in the seconds and milliseconds range, respectively. Formation of a heterogeneous catalyst from a solid-state reaction of a precursor is presented as an example of a time-resolved XAS application.

2020 ◽  
Vol 56 (71) ◽  
pp. 10329-10332 ◽  
Author(s):  
Paulo F. M. de Oliveira ◽  
Adam A. L. Michalchuk ◽  
Ana Guilherme Buzanich ◽  
Ralf Bienert ◽  
Roberto M. Torresi ◽  
...  

A new tandem approach combines XRD and XANES for time-resolved in situ monitoring of the mechanochemical synthesis of gold nanoparticles.


2005 ◽  
Vol 7 (2) ◽  
pp. 366-372 ◽  
Author(s):  
A. Rose ◽  
O. South ◽  
I. Harvey ◽  
S. Diaz-Moreno ◽  
J. R. Owen ◽  
...  

ChemInform ◽  
2005 ◽  
Vol 36 (27) ◽  
Author(s):  
Guido Schimanke ◽  
Manfred Martin ◽  
Jan Kunert ◽  
Herbert Vogel

2009 ◽  
Vol 16 (2) ◽  
pp. 264-272 ◽  
Author(s):  
Dirk Lützenkirchen-Hecht ◽  
Ralph Wagner ◽  
Ulrich Haake ◽  
Anke Watenphul ◽  
Ronald Frahm

The hard X-ray beamline BL8 at the superconducting asymmetric wiggler at the 1.5 GeV Dortmund Electron Accelerator DELTA is described. This beamline is dedicated to X-ray studies in the spectral range from ∼1 keV to ∼25 keV photon energy. The monochromator as well as the other optical components of the beamline are optimized accordingly. The endstation comprises a six-axis diffractometer that is capable of carrying heavy loads related to non-ambient sample environments such as, for example, ultrahigh-vacuum systems, high-pressure cells or liquid-helium cryostats. X-ray absorption spectra from several reference compounds illustrate the performance. Besides transmission measurements, fluorescence detection for dilute sample systems as well as surface-sensitive reflection-mode experiments have been performed. The results show that high-quality EXAFS data can be obtained in the quick-scanning EXAFS mode within a few seconds of acquisition time, enabling time-resolved in situ experiments using standard beamline equipment that is permanently available. The performance of the new beamline, especially in terms of the photon flux and energy resolution, is competitive with other insertion-device beamlines worldwide, and several sophisticated experiments including surface-sensitive EXAFS experiments are feasible.


2020 ◽  
Author(s):  
Paulo F M de Oliveira ◽  
Adam Michalchuk ◽  
Ana de Oliveira Guilherme Buzanich ◽  
Ralf Bienert ◽  
Roberto M. Torresi ◽  
...  

<div>The development of time-resolved in situ approaches for monitoring mechanochemical</div><div>transformations has revolutionized the field of mechanochemistry. Currently, the established in</div><div>situ approaches greatly limit the scope of investigations that are possible. Here we develop a new</div><div>approach to simultaneously follow the evolution of bulk atomic and electronic structure during a</div><div>mechanochemical synthesis. This is achieved by coupling two complementary synchrotron-based</div><div>X-ray methods: X-ray absorption spectroscopy and X-ray diffraction. We apply this method to</div><div>investigate the bottom-up mechanosynthesis of technologically important Au nanoparticles in the</div><div>presence of three different reducing agents. Moreover, we demonstrate how X-ray absorption</div><div>spectroscopy offers unprecedented insight into the early stage generation of growth species (e.g.</div><div>monomers and clusters), which lead to the subsequent formation of nanoparticles. These</div><div>processes are beyond the detection capabilities of diffraction methods. The approach is general,</div><div>and not limited to monitoring NP mechanosynthesis. This combined X-ray approach paves the</div><div>way to new directions in mechanochemical research of advanced electronic materials.</div>


RSC Advances ◽  
2019 ◽  
Vol 9 (58) ◽  
pp. 34004-34010 ◽  
Author(s):  
Jacinta Xto ◽  
Reto Wetter ◽  
Camelia N. Borca ◽  
Christophe Frieh ◽  
Jeroen A. van Bokhoven ◽  
...  

We introduce a new in situ cell for time-resolved reactions involving aerosols/droplets using tender X-ray absorption spectroscopy and related methods.


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