scholarly journals Pyrolitic Graphite Mosaic Crystal Thickness and Mosaicity Optimization for an Extended Source Von Hamos X-ray Spectrometer

2019 ◽  
Vol 4 (2) ◽  
pp. 38 ◽  
Author(s):  
Alessandro Scordo ◽  
Catalina Curceanu ◽  
Marco Miliucci ◽  
Florin Sirghi ◽  
Johann Zmeskal

Bragg spectroscopy, one of the best established experimental techniques for high energy resolution X-ray measurements, has always been limited to the measurement of photons produced from well collimated (tens of microns) or point-like sources; recently, the VOXES collaboration at INFN National Laboratories of Frascati developed a prototype of a high resolution and high precision X-ray spectrometer working also with extended isotropic sources. The realized spectrometer makes use of Highly Annealed Pyrolitic Graphite (HAPG) crystals in a “semi”-Von Hamos configuration, in which the position detector is rotated with respect to the standard Von Hamos one, to increase the dynamic energy range, and shows energy resolutions at the level of 0.1% for photon energies up to 10 keV and effective source sizes in the range 400–1200 μ m in the dispersive plane. Such wide effective source dimensions are achieved using a double slit system to produce a virtual point-like source between the emitting target and the crystal. The spectrometer performances in terms of reflection efficiency and peak resolution depend on several parameters, among which a special role is played by the crystal mosaicity and thickness. In this work, we report the measurements of the Cu(K α 1 , 2 ) and the Fe(K α 1 , 2 ) lines performed with different mosaicity and thickness crystals in order to investigate the influence of the parameters on the peak resolution and on the reflection efficiency mentioned above.

2017 ◽  
Vol 139 (49) ◽  
pp. 18024-18033 ◽  
Author(s):  
Rebeca G. Castillo ◽  
Rahul Banerjee ◽  
Caleb J. Allpress ◽  
Gregory T. Rohde ◽  
Eckhard Bill ◽  
...  

2015 ◽  
Vol 112 (52) ◽  
pp. 15803-15808 ◽  
Author(s):  
Ofer Hirsch ◽  
Kristina O. Kvashnina ◽  
Li Luo ◽  
Martin J. Süess ◽  
Pieter Glatzel ◽  
...  

The lanthanum-based materials, due to their layered structure and f-electron configuration, are relevant for electrochemical application. Particularly, La2O2CO3 shows a prominent chemoresistive response to CO2. However, surprisingly less is known about its atomic and electronic structure and electrochemically significant sites and therefore, its structure–functions relationships have yet to be established. Here we determine the position of the different constituents within the unit cell of monoclinic La2O2CO3 and use this information to interpret in situ high-energy resolution fluorescence-detected (HERFD) X-ray absorption near-edge structure (XANES) and valence-to-core X-ray emission spectroscopy (vtc XES). Compared with La(OH)3 or previously known hexagonal La2O2CO3 structures, La in the monoclinic unit cell has a much lower number of neighboring oxygen atoms, which is manifested in the whiteline broadening in XANES spectra. Such a superior sensitivity to subtle changes is given by HERFD method, which is essential for in situ studying of the interaction with CO2. Here, we study La2O2CO3-based sensors in real operando conditions at 250 °C in the presence of oxygen and water vapors. We identify that the distribution of unoccupied La d-states and occupied O p- and La d-states changes during CO2 chemoresistive sensing of La2O2CO3. The correlation between these spectroscopic findings with electrical resistance measurements leads to a more comprehensive understanding of the selective adsorption at La site and may enable the design of new materials for CO2 electrochemical applications.


2020 ◽  
Author(s):  
Philipp Jäker ◽  
Dino Aegerter ◽  
Till Kyburz ◽  
Roman Staedler ◽  
Rea Fonjallaz ◽  
...  

Photo-electro-chemical (PEC) water splitting represents a promising technology towards an artificial photosynthetic device but many fundamental electronic processes, which govern long-term stability and energetics are not well understood. X-ray absorption spectroscopy (XAS), particularly its high energy resolution fluorescence-detected (HERFD) mode, emerges as a powerful tool to study photo-excited charge carrier behavior under operating conditions. The established thin film device architecture of PEC cells provides a well-defined measurement geometry, but it puts many constraints on conducting operando XAS experiments. So far, operando cells have not been developed that enable to concurrently measure highly intense X-ray fluorescence and photo-electro-chemical current without experimental artifacts caused by O<sub>2</sub> and H<sub>2</sub> bubbles formation. Moreover, we are missing a standardized thin film exchange procedure. Here, we address and overcome the instrumental limitations for operando HERFD-XAS to investigate photo- and electrochemical thin film devices. Our cell establishes a measurement routine that will provide experimental access to a broader scientific community, particularly due to the ease of sample exchange. Our operando photo-electro-chemical cell is optimized for the HERFD-XAS geometry and we demonstrate its operation by collecting high-resolution Fe K-edge spectra of hematite (α-Fe<sub>2</sub>O<sub>3</sub>) and ferrite thin film (MFe<sub>2</sub>O<sub>4</sub>, M= Zn, Ni) photoelectrodes during water oxidation.<br>


2013 ◽  
Vol 19 (S2) ◽  
pp. 1258-1259 ◽  
Author(s):  
H. Takahashi ◽  
N. Handa ◽  
T. Murano ◽  
M. Terauchi ◽  
M. Koike ◽  
...  

Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.


1996 ◽  
Vol 67 (9) ◽  
pp. 3359-3359 ◽  
Author(s):  
Wolfgang A. Caliebe ◽  
Sas̆a Bajt ◽  
Chi‐Chang Kao

2014 ◽  
Vol 24 (03n04) ◽  
pp. 205-215
Author(s):  
M. Kavčič

While traditional proton induced X-ray emission (PIXE) analytical technique is based on the energy dispersive solid state detectors used to collect the X-ray fluorescence from the sample, wavelength dispersive X-ray (WDX) spectrometers are applied in high energy resolution PIXE (HR-PIXE) analysis. The main drawback of the WDX spectroscopy is the relatively low efficiency making it less applicable for trace element PIXE analysis. However, the efficiency was enhanced significantly in modern spectrometers employing cylindrically or even spherically curved crystals combined with position sensitive X-ray detectors. The energy resolution of such a spectrometer may exceed the resolution of the energy dispersive detector by two orders of magnitude while keeping the efficiency at a high enough level to perform trace element analysis. In this paper, the recent history and the development of HR-PIXE spectroscopy at the J. Stefan Institute in Ljubljana is presented. Our current setup based on in-vacuum Johansson-type crystal spectrometer is presented in more details followed by some most recent applications.


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