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Crystals
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Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials
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Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Inorganic Crystalline Materials".

Deadline for manuscript submissions: closed (12 June 2021) | Viewed by 18793

Special Issue Editor

Dr. Mikhail Platunov

E-Mail Website
Guest Editor
Kirensky Institute of Physics, Federal Research Center KSC SB RAS, Krasnoyarsk, Russia
Interests: magnetic materials; interfacial magnetism; interplay between structure and magnetism; local structure; phase transitions; strong correlated electron systems; X-ray absorption fine structure; X-ray dichroism techniques
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

One of the strengths of modern X-ray science is its endeavor to provide unique tools and methods to understand and picture how atoms interact in the materials that are the basis for new technologies. Understanding materials for electronic devices is an example of the key challenges for which we need to improve our capacity to design future materials, technological processes, etc. These ambitious goals of 21st-century science require fundamental understanding and visualization of interactions with full continuity from macroscopic objects down to interactions on the level of a single atom. Future X-ray science at modern synchrotrons will bridge the gap between visible light and electron microscopy, i.e., it will give full access to study all possible changes—all of this with spatial and temporal resolutions that will be approaching a few atoms in space (nanometer) and interatomic motion in time (femtosecond), respectively. Such incredible resolution and range in space and time is made possible by the absolutely impressive and never-ending improvements of brightness, spectral range, and degree of spatial and temporal coherence and resolution of accelerator-based X-ray sources. Application of synchrotron-based techniques could help to unravel the nature of many interactions that remain challenges in condensed-matter physics.

This Special Issue aims at covering all the relevant aspects of synchrotron-based X-ray techniques for the study of materials. Furthermore, articles or short reviews highlighting the several applications of synchrotron-based techniques are also welcome.

Dr. Mikhail PLATUNOV
Guest Editor

Manuscript Submission Information

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Crystals is an international peer-reviewed open access monthly journal published by MDPI.

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Keywords

  • Development and use of synchrotron and XFEL sources
  • Synchrotron experimental stations
  • Extreme condition experiments
  • Data collection and processing

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Published Papers (6 papers)

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Research

11 pages, 2303 KiB  
Article
Suppressing Diffraction-Related Intensity Losses in Transmissive Single-Crystal X-ray Optics
by Nataliya Klimova, Irina Snigireva, Anatoly Snigirev and Oleksandr Yefanov
Crystals 2021, 11(12), 1561; https://doi.org/10.3390/cryst11121561 - 14 Dec 2021
Cited by 4 | Viewed by 2174
Abstract
The highest-quality X-ray optics can be made of single-crystal materials such as silicon, germanium, or, even better, diamond. Unfortunately, such X-ray optics have one drawback: diffraction losses or the “glitch effect”. This effect manifests itself as follows: at some energies of X-rays, the [...] Read more.
The highest-quality X-ray optics can be made of single-crystal materials such as silicon, germanium, or, even better, diamond. Unfortunately, such X-ray optics have one drawback: diffraction losses or the “glitch effect”. This effect manifests itself as follows: at some energies of X-rays, the intensity of the transmitted beam drops due to the fact that some crystalline planes have satisfied the diffraction condition. Diffraction losses are usually observed in spectroscopic experiments when the energy of the X-rays changes in a certain range. However, this effect might also influence any experiment using X-rays, especially at higher energies. In this paper, we propose a method to overcome the glitch problem in transmissive optics. This is achieved using small rotations of the optical element. We describe the algorithm for “glitch-free” measurements in detail and the theory behind it. Full article
(This article belongs to the Special Issue Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials)
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10 pages, 2420 KiB  
Article
Determination of Absolute Structure of Chiral Crystals Using Three-Wave X-ray Diffraction
by Ksenia Kozlovskaya, Elena Ovchinnikova, Jun Kokubun, Andrei Rogalev, Fabrice Wilhelm, Francois Guillou, Francois de Bergevin, Alisa F. Konstantinova and Vladimir E. Dmitrienko
Crystals 2021, 11(11), 1389; https://doi.org/10.3390/cryst11111389 - 15 Nov 2021
Cited by 4 | Viewed by 3180
Abstract
We propose a new method to determine the absolute structure of chiral crystals, which is based on the chiral asymmetry of multiple scattering diffraction. It manifests as a difference in the azimuthal dependence of the forbidden Bragg reflection intensity measured with left and [...] Read more.
We propose a new method to determine the absolute structure of chiral crystals, which is based on the chiral asymmetry of multiple scattering diffraction. It manifests as a difference in the azimuthal dependence of the forbidden Bragg reflection intensity measured with left and right circularly polarized X-ray beams. Contrary to the existing ones, the suggested method does not use X-ray anomalous dispersion. The difference between the Renninger scans with circularly polarized X-rays has been experimentally demonstrated for the 001 reflection intensities in the right- and left-handed quartz single crystals. A Jmulti-based code on model-independent three-wave-diffraction approach has been developed for quantitative description of our experimental results. The proposed method can be applied to various structures including opaque, organic and monoatomic crystals, even with only light elements. To determine the type of isomer, the Renninger plot of a single forbidden reflection is sufficient. Full article
(This article belongs to the Special Issue Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials)
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10 pages, 2177 KiB  
Article
In-Situ X-ray Photoelectron Spectroscopy and Raman Microscopy of Roselite Crystals, Ca2(Co2+,Mg)(AsO4)2 2H2O, from the Aghbar Mine, Morocco
by Jacob Teunis Kloprogge, Barry James Wood and Danilo Octaviano Ortillo
Crystals 2021, 11(6), 670; https://doi.org/10.3390/cryst11060670 - 10 Jun 2021
Cited by 1 | Viewed by 2090
Abstract
Roselite from the Aghbar Mine, Morocco, [Ca2(Co2+,Mg)(AsO4)2 2H2O], was investigated by X-ray Photoelectron and Raman spectroscopy. X-ray Photoelectron Spectroscopy revealed a cobalt to magnesium ratio of 3:1. Magnesium, cobalt and calcium showed single bands [...] Read more.
Roselite from the Aghbar Mine, Morocco, [Ca2(Co2+,Mg)(AsO4)2 2H2O], was investigated by X-ray Photoelectron and Raman spectroscopy. X-ray Photoelectron Spectroscopy revealed a cobalt to magnesium ratio of 3:1. Magnesium, cobalt and calcium showed single bands associated with unique crystallographic positions. The oxygen 1s spectrum displayed two bands associated with the arsenate group and crystal water. Arsenic 3d exhibited bands with a ratio close to that of the cobalt to magnesium ratio, indicative of the local arsenic environment being sensitive to the substitution of magnesium for cobalt. The Raman arsenate symmetric and antisymmetric modes were all split with the antisymmetric modes observed around 865 and 818 cm−1, while the symmetric modes were found around 980 and 709 cm−1. An overlapping water-libration mode was observed at 709 cm−1. The region at 400–500 cm−1 showed splitting of the arsenate antisymmetric mode with bands at 499, 475, 450 and 425 cm−1. The 300–400 cm−1 region showed the corresponding symmetric bending modes at 377, 353, 336 and 304 cm−1. The bands below 300 cm−1 were assigned to lattice modes. Full article
(This article belongs to the Special Issue Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials)
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14 pages, 5759 KiB  
Article
X-ray Natural Circular Dichroism Imaging of Multiferroic Crystals
by Mikhail S. Platunov, Irina A. Gudim, Elena N. Ovchinnikova, Ksenia A. Kozlovskaya, Fabrice Wilhelm, Andrei Rogalev, Amir Hen, Vsevolod Y. Ivanov, Alexander A. Mukhin and Vladimir E. Dmitrienko
Crystals 2021, 11(5), 531; https://doi.org/10.3390/cryst11050531 - 11 May 2021
Cited by 10 | Viewed by 3649
Abstract
The polarizing spectroscopy techniques in visible range optics have been used since the beginning of the 20th century to study the anisotropy of crystals based on birefringence and optical activity phenomena. On the other hand, the phenomenon of X-ray optical activity has been [...] Read more.
The polarizing spectroscopy techniques in visible range optics have been used since the beginning of the 20th century to study the anisotropy of crystals based on birefringence and optical activity phenomena. On the other hand, the phenomenon of X-ray optical activity has been demonstrated only relatively recently. It is a selective probe for the element-specific properties of individual atoms in non-centrosymmetric materials. We report the X-ray Natural Circular Dichroism (XNCD) imaging technique which enables spatially resolved mapping of X-ray optical activity in non-centrosymmetric materials. As an example, we present the results of combining micro-focusing X-ray optics with circularly polarized hard X-rays to make a map of enantiomorphous twinning in a multiferroic SmFe3(BO3)4 crystal. Our results demonstrate the utility and potential of polarization-contrast imaging with XNCD as a sensitive technique for multiferroic crystals where the local enantiomorphous properties are especially important. In perspective, this brings a novel high-performance method for the characterization of structural changes associated with phase transitions and identification of the size and spatial distribution of twin domains. Full article
(This article belongs to the Special Issue Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials)
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15 pages, 4582 KiB  
Article
Determination of the Exact Orientation of Single-Crystal X-ray Optics from Its Glitch Spectrum and Modeling of Glitches for an Arbitrary Configuration
by Nataliya Klimova, Oleksandr Yefanov, Irina Snigireva and Anatoly Snigirev
Crystals 2021, 11(5), 504; https://doi.org/10.3390/cryst11050504 - 2 May 2021
Cited by 6 | Viewed by 3057
Abstract
X-ray optics made of single-crystal materials are widely used at most of the X-ray sources due to the outstanding properties. The main drawback of such optics—the diffraction losses, also known as glitches of intensity in the energy spectrum of the transmitted/diffracted beam. To [...] Read more.
X-ray optics made of single-crystal materials are widely used at most of the X-ray sources due to the outstanding properties. The main drawback of such optics—the diffraction losses, also known as glitches of intensity in the energy spectrum of the transmitted/diffracted beam. To be able to handle this negative effect, one needs a reliable way to simulate the glitch spectrum in any configuration. Here, we demonstrate the way of precisely determining the crystallographic orientation and unit cell parameters of optical elements just from a small glitch spectrum with the consequent possibility of simulating glitches for any energy. Full article
(This article belongs to the Special Issue Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials)
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14 pages, 1107 KiB  
Article
Forbidden Reflections in TeO2 in the Vicinity of the Te L1 Absorption Edge
by Elena Ovchinnikova, Dmitri Novikov, Matthias Zschornak, Anton Kulikov, Ksenia Kozlovskaya, Vladimir Dmitrienko, Alexey Oreshko, Alexander Blagov, Enver Mukhamedzhanov, Nikita Marchenkov, Mickhail Borisov, Azat Khadiev, Arsen Petrenko and Yury Pisarevsky
Crystals 2020, 10(9), 719; https://doi.org/10.3390/cryst10090719 - 19 Aug 2020
Cited by 7 | Viewed by 3445
Abstract
Examining forbidden reflections provides valuable information on electronic states and the local environment of resonant atoms in crystals. Experimental studies of two forbidden reflections 002 and 100 in TeO2 single crystals were performed at photon energies close to the L1 tellurium [...] Read more.
Examining forbidden reflections provides valuable information on electronic states and the local environment of resonant atoms in crystals. Experimental studies of two forbidden reflections 002 and 100 in TeO2 single crystals were performed at photon energies close to the L1 tellurium absorption edge. It was found that the spectral form corresponding to these two reflections looks almost identical, which is completely unexpected for a highly anisotropic material. Theoretical consideration shows that only one component fxy of the tensor describing dipole-dipole resonance scattering contributes to the 002 reflection, while two components fxy and fxz correspond to the 100 reflection. Numerical calculations show that the latter tensor component is comparable to the first one, but the combination of several geometric factors leads to the fact that its contribution to the spectrum is negligible. This explains the experimentally observed results. The finding shows a way for targeted investigation of single tensor components and makes it possible to compare different spectra and use them the study the physical phenomena in functional materials. Full article
(This article belongs to the Special Issue Synchrotron-Based X-Ray Techniques for the Study of New Crystalline Materials)
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