scholarly journals Diffraction imaging forin situcharacterization of double-crystal X-ray monochromators

2015 ◽  
Vol 48 (6) ◽  
pp. 1734-1744 ◽  
Author(s):  
Stanislav Stoupin ◽  
Zunping Liu ◽  
Steve M. Heald ◽  
Dale Brewe ◽  
Mati Meron

Imaging of the Bragg-reflected X-ray beam is proposed and validated as anin situmethod for characterization of the performance of double-crystal monochromators under the heat load of intense synchrotron radiation. A sequence of images is collected at different angular positions on the reflectivity curve of the second crystal and analyzed. The method provides rapid evaluation of the wavefront of the exit beam, which relates to local misorientation of the crystal planes along the beam footprint on the thermally distorted first crystal. The measured misorientation can be directly compared with the results of finite element analysis. The imaging method offers an additional insight into the local intrinsic crystal quality over the footprint of the incident X-ray beam.

2019 ◽  
Vol 75 (3) ◽  
pp. 527-540 ◽  
Author(s):  
Hamish A. Melia ◽  
Christopher T. Chantler ◽  
Lucas F. Smale ◽  
Alexis J. Illig

A characterization of the Cu Kα1,2 spectrum is presented, including the 2p satellite line, Kα3,4, the details of which are robust enough to be transferable to other experiments. This is a step in the renewed attempts to resolve inconsistencies in characteristic X-ray spectra between theory, experiment and alternative experimental geometries. The spectrum was measured using a rotating anode, monolithic Si channel-cut double-crystal monochromator and backgammon detector. Three alternative approaches fitted five Voigt profiles to the data: a residual analysis approach; a peak-by-peak fit; and a simultaneous constrained method. The robustness of the fit is displayed across three spectra obtained with different instrumental broadening. Spectra were not well fitted by transfer of any of three prior characterizations from the literature. Integrated intensities, line widths and centroids are compared with previous empirical fits. The novel experimental setup provides insight into the portability of spectral characterizations of X-ray spectra. From the parameterization, an estimated 3d shake probability of 18% and a 2p shake probability of 0.5% are reported.


Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


2016 ◽  
Vol 108 (21) ◽  
pp. 211902 ◽  
Author(s):  
Xian Chen ◽  
Nobumichi Tamura ◽  
Alastair MacDowell ◽  
Richard D. James

Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.


Nanomaterials ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 446
Author(s):  
Ioannis Spanos ◽  
Zacharias Vangelatos ◽  
Costas Grigoropoulos ◽  
Maria Farsari

The need for control of the elastic properties of architected materials has been accentuated due to the advances in modelling and characterization. Among the plethora of unconventional mechanical responses, controlled anisotropy and auxeticity have been promulgated as a new avenue in bioengineering applications. This paper aims to delineate the mechanical performance of characteristic auxetic and anisotropic designs fabricated by multiphoton lithography. Through finite element analysis the distinct responses of representative topologies are conveyed. In addition, nanoindentation experiments observed in-situ through scanning electron microscopy enable the validation of the modeling and the observation of the anisotropic or auxetic phenomena. Our results herald how these categories of architected materials can be investigated at the microscale.


2014 ◽  
Vol 47 (6) ◽  
pp. 1882-1888 ◽  
Author(s):  
J. Hilhorst ◽  
F. Marschall ◽  
T. N. Tran Thi ◽  
A. Last ◽  
T. U. Schülli

Diffraction imaging is the science of imaging samples under diffraction conditions. Diffraction imaging techniques are well established in visible light and electron microscopy, and have also been widely employed in X-ray science in the form of X-ray topography. Over the past two decades, interest in X-ray diffraction imaging has taken flight and resulted in a wide variety of methods. This article discusses a new full-field imaging method, which uses polymer compound refractive lenses as a microscope objective to capture a diffracted X-ray beam coming from a large illuminated area on a sample. This produces an image of the diffracting parts of the sample on a camera. It is shown that this technique has added value in the field, owing to its high imaging speed, while being competitive in resolution and level of detail of obtained information. Using a model sample, it is shown that lattice tilts and strain in single crystals can be resolved simultaneously down to 10−3° and Δa/a= 10−5, respectively, with submicrometre resolution over an area of 100 × 100 µm and a total image acquisition time of less than 60 s.


2014 ◽  
Vol 47 (6) ◽  
pp. 2078-2080 ◽  
Author(s):  
Monika Witala ◽  
Jun Han ◽  
Andreas Menzel ◽  
Kim Nygård

It is shown that small-angle X-ray scattering from binary liquid mixtures close to the critical point of demixing can be used forin situcharacterization of beam-induced heating of liquid samples. For demonstration purposes, the proposed approach is applied on a well studied critical mixture of water and 2,6-lutidine. Given a typical incident X-ray flux at a third-generation synchrotron light source and using a 1.5 mm-diameter glass capillary as sample container, a beam-induced local temperature increase of 0.45 ± 0.10 K is observed.


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