Effects of source size and wavefront propagation on the energy resolution of a bent-crystal polychromator

2010 ◽  
Vol 1 (MEDSI-6) ◽  
Author(s):  
J. P. Sutter ◽  
M. Amboage ◽  
S. Hayama ◽  
S. Díaz-Moreno

Polychromators, or elliptically bent diffracting crystals that focus a broad-bandwidth X-ray beam onto a sample, have become a common device at synchrotron beamlines specializing in X-ray absorption spectroscopy (XAS) because they allow a full absorption spectrum to be collected in one shot. Such a device is being planned for the XAS beamline I20 of the Diamond Light Source. A bent silicon crystal diffracting 7 keV X-rays with the (1 1 1) reflection is taken as a model for the simulations of this report. Instrumental resolution is determined by the demagnification of the source, the spread of the diffracted beam during propagation and the pixel size of the position-sensitive detector placed behind the sample. The first is calculated by geometrical optics. The second is calculated by a full wave-optical treatment, which includes Takagi–Taupin integration to find the diffracted amplitude at the crystal's surface and Huygens–Fresnel propagation of the diffracted wave to the sample or detector. This sets the polychromator's intrinsic energy resolution. The pixel size of the detector is then added to find the total instrumental resolution at various sample–detector distances.

2020 ◽  
Vol 27 (6) ◽  
pp. 1618-1625
Author(s):  
Yuki Wakisaka ◽  
Bing Hu ◽  
Daiki Kido ◽  
Md. Harun Al Rashid ◽  
Wenhan Chen ◽  
...  

A bent crystal Laue analyser (BCLA) is an X-ray energy analyser used for fluorescence X-ray absorption fine-structure (XAFS) spectroscopy to separate the fluorescence X-ray emission line of a target atom from the elastic scattering X-rays and other fluorescence emission lines. Here, the feasibility of the BCLA for total reflection fluorescence XAFS (TRF-XAFS), which has a long X-ray footprint on the substrate surface owing to grazing incidence, was tested. The focal line of the BCLA was adjusted on the X-ray footprint and the XAFS signal for one monolayer of Pt deposited on a 60 nm Au film with high sensitivity was obtained. Although range-extended XAFS was expected by the rejection of Au fluorescence arising from the Au substrate, a small glitch was found in the Au L 3 edge because of the sudden change of the complex refraction index of the Au substrate at the Au edge. This abnormal spectrum feature can be removed by reflectivity correction using Au foil absorption data. BCLA combined with TRF-XAFS spectroscopy (BCLA + TRF-XAFS) is a new technique for the in situ surface analysis of highly dispersed systems even in the presence of a liquid overlayer.


Author(s):  
W. Z. Chang ◽  
D. B. Wittry

Since Du Mond and Kirkpatrick first discussed the principle of a bent crystal spectrograph in 1930, curved single crystals have been widely utilized as spectrometric monochromators as well as diffractors for focusing x rays diverging from a point. Curved crystal diffraction theory predicts that the diffraction parameters - the rocking curve width w, and the peak reflection coefficient r of curved crystals will certainly deviate from those of their flat form. Due to a lack of curved crystal parameter data in current literature and the need for optimizing the choice of diffraction geometry and crystal materials for various applications, we have continued the investigation of our technique presented at the last conference. In the present abstract, we describe a more rigorous and quantitative procedure for measuring the parameters of curved crystals.The diffraction image of a singly bent crystal under study can be obtained by using the Johann geometry with an x-ray point source.


Author(s):  
R. L. Stears

Because of the nature of the bacterial endospore, little work has been done on analyzing their elemental distribution and composition in the intact, living, hydrated state. The majority of the qualitative analysis entailed intensive disruption and processing of the endospores, which effects their cellular integrity and composition.Absorption edge imaging permits elemental analysis of hydrated, unstained specimens at high resolution. By taking advantage of differential absorption of x-ray photons in regions of varying elemental composition, and using a high brightness, tuneable synchrotron source to obtain monochromatic x-rays, contact x-ray micrographs can be made of unfixed, intact endospores that reveal sites of elemental localization. This study presents new data demonstrating the application of x-ray absorption edge imaging to produce elemental information about nitrogen (N) and calcium (Ca) localization using Bacillus thuringiensis as the test specimen.


Nano Research ◽  
2021 ◽  
Author(s):  
Alevtina Smekhova ◽  
Alexei Kuzmin ◽  
Konrad Siemensmeyer ◽  
Chen Luo ◽  
Kai Chen ◽  
...  

AbstractModern design of superior multi-functional alloys composed of several principal components requires in-depth studies of their local structure for developing desired macroscopic properties. Herein, peculiarities of atomic arrangements on the local scale and electronic states of constituent elements in the single-phase face-centered cubic (fcc)- and body-centered cubic (bcc)-structured high-entropy Alx-CrFeCoNi alloys (x = 0.3 and 3, respectively) are explored by element-specific X-ray absorption spectroscopy in hard and soft X-ray energy ranges. Simulations based on the reverse Monte Carlo approach allow to perform a simultaneous fit of extended X-ray absorption fine structure spectra recorded at K absorption edges of each 3d constituent and to reconstruct the local environment within the first coordination shells of absorbers with high precision. The revealed unimodal and bimodal distributions of all five elements are in agreement with structure-dependent magnetic properties of studied alloys probed by magnetometry. A degree of surface atoms oxidation uncovered by soft X-rays suggests different kinetics of oxide formation for each type of constituents and has to be taken into account. X-ray magnetic circular dichroism technique employed at L2.3 absorption edges of transition metals demonstrates reduced magnetic moments of 3d metal constituents in the sub-surface region of in situ cleaned fcc-structured Al0.3-CrFeCoNi compared to their bulk values. Extended to nanostructured versions of multicomponent alloys, such studies would bring new insights related to effects of high entropy mixing on low dimensions.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Seongwook Choi ◽  
Eun-Yeong Park ◽  
Sinyoung Park ◽  
Jong Hyun Kim ◽  
Chulhong Kim

AbstractX-ray induced acoustic imaging (XAI) is an emerging biomedical imaging technique that can visualize X-ray absorption contrast at ultrasound resolution with less ionizing radiation exposure than conventional X-ray computed tomography. So far, medical linear accelerators or industrial portable X-ray tubes have been explored as X-ray excitation sources for XAI. Here, we demonstrate the first feasible synchrotron XAI (sXAI). The synchrotron generates X-rays, with a dominant energy of 4 to 30 keV, a pulse-width of 30 ps, a pulse-repetition period of 2 ns, and a bunch-repetition period of 940 ns. The X-ray induced acoustic (XA) signals are processed in the Fourier domain by matching the signal frequency with the bunch-repetition frequency. We successfully obtained two-dimensional XA images of various lead targets. This novel sXAI tool could complement conventional synchrotron applications.


2010 ◽  
Vol 43 (2) ◽  
pp. 341-346 ◽  
Author(s):  
Yu Kitago ◽  
Nobuhisa Watanabe ◽  
Isao Tanaka

Use of longer-wavelength X-rays has advantages for the detection of small anomalous signals from light atoms, such as sulfur, in protein molecules. However, the accuracy of the measured diffraction data decreases at longer wavelengths because of the greater X-ray absorption. The capillary-top mounting method (formerly the loopless mounting method) makes it possible to eliminate frozen solution around the protein crystal and reduces systematic errors in the evaluation of small anomalous differences. However, use of this method requires custom-made tools and a large amount of skill. Here, the development of a device that can freeze the protein crystal semi-automatically using the capillary-top mounting method is described. This device can pick up the protein crystal from the crystallization drop using a micro-manipulator, and further procedures, such as withdrawal of the solution around the crystal by suction and subsequent flash freezing of the protein crystal, are carried out automatically. This device makes it easy for structural biologists to use the capillary-top mounting method for sulfur single-wavelength anomalous diffraction phasing using longer-wavelength X-rays.


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

1998 ◽  
Vol 5 (3) ◽  
pp. 967-968 ◽  
Author(s):  
Keiichi Hirano ◽  
Atsushi Momose

The phase shift of forward-diffracted X-rays by a perfect crystal is discussed on the basis of the dynamical theory of X-ray diffraction. By means of a triple Laue-case X-ray interferometer, the phase shift of forward-diffracted X-rays by a silicon crystal in the Bragg geometry was investigated.


1998 ◽  
Vol 5 (3) ◽  
pp. 515-517 ◽  
Author(s):  
M. Frank ◽  
C. A. Mears ◽  
S. E. Labov ◽  
L. J. Hiller ◽  
J. B. le Grand ◽  
...  

Experimental results are presented obtained with a cryogenically cooled high-resolution X-ray spectrometer based on a 141 × 141 µm Nb-Al-Al2O3-Al-Nb superconducting tunnel junction (STJ) detector in an SR-XRF demonstration experiment. STJ detectors can operate at count rates approaching those of semiconductor detectors while still providing a significantly better energy resolution for soft X-rays. By measuring fluorescence X-rays from samples containing transition metals and low-Z elements, an FWHM energy resolution of 6–15 eV for X-rays in the energy range 180–1100 eV has been obtained. The results show that, in the near future, STJ detectors may prove very useful in XRF and microanalysis applications.


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.


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