Measuring Techniques of Parallel Beam-Diffraction Micrography

1966 ◽  
Vol 10 ◽  
pp. 80-90
Author(s):  
H. Barth
Keyword(s):  
Resolving Power ◽  
X Rays ◽  
X Ray Diffraction ◽  
Crystal Surfaces ◽  
Parallel Beam ◽  
X Ray ◽  
Fixed Sample ◽  
Independent Field ◽  
Measuring Techniques ◽  
Beam Method

AbstractExamination of the substructure of crystalline solids by diffractographic methods has recently developed into an independent field of work alongside atomicstructure analysis. Diffraction micrography with electrons is characterized by the small size of the distortion fields and the high resolving power in small crystal ranges (1000-3000Å thickness). X-ray diffraction micrography is characterized by great reciprocation between wave field and distortion field and by undisturbed preparation and undisturbed testing in the large crystal ranges (up to 15 cm2). There are two groups of examination methods for diffraction micrography with X-rays: (1) Examination with a finely limited, polychromatic or monochromatic X-ray source and moving sample, according to A. R. Lang et al. (2) Examination with a parallel-ray beam of polychromatic or monochromatic X-rays with fixed sample, in accordance with Berg-Barrett et al. For the examination of coarse defects in single-crystalline and poly crystalline matter, the parallel-beam method offers a wide scope for studies in the physics and applications of single-crystal line and polycrystalline solids. This paper therefore includes a summary of the methods using collimation systems and grating diaphragms. Measuring techniques and results are illustrated with the help of reflection and transmission pictures on various crystals. The various methods and refined measuring technique of the parallel-beam method enable the following to be defined: (1) Localization of crystallites from 20 μ diam. upward in a surface up to 15 cm2. (2) Determination of the faces of averted crystallites from 20 µ diam. upward in crystal surfaces. (3) Angle of avertence of crystallites or curvature angles of net faces from 1 to 3° in crystal surfaces up to 15 cm2. (4) Subangle grain boundaries, slip bands, and dislocation lines; also distortion fields (from 20 μ upward) resulting from mechanical, thermal, and radiation damage.

X-Ray Diffraction Contrast from Impurity Precipitates in CdS Single Crystals

1966 ◽  
Vol 10 ◽  
pp. 153-158 ◽  
Author(s):  
Jun-ichi Chikawa
Keyword(s):  
Strain Field ◽  
Crystal Surface ◽  
Bragg Angle ◽  
X Rays ◽  
Bragg Condition ◽  
X Ray Diffraction ◽  
Crystal Surfaces ◽  
X Ray ◽  
Impurity Doped ◽  
Free Plane

AbstractImpurity-doped crystals CdS(GaGl3) have been studied by X-ray topography. Some large precipitates are formed close to the crystal surfaces by annealing at 300°C. In the symmetrical Laue case, the precipitates show circular images (30-60 μ in diameter) due to the radial strains around the precipitates which consist of two semicircles separated by a contrast-free plane parallel to the reflecting plane. The observations indicate that the strain field between the crystal surface and precipitate is not responsible for the contrast, and that the images are formed by X-rays which are deviated from the Bragg condition for the perfect region and satisfy the Bragg condition in the strain field on the inside of the precipitate. One of the semicircles is formed by the incident X-rays with larger glancing angles than the Bragg angle and the other with smaller ones. It is concluded that this contrast is due to the strain around a convex lens shaped precipitate.

Parallel-beam X-ray diffractometry using X-ray guide tubes

2000 ◽  
Vol 33 (2) ◽  
pp. 389-391 ◽  
Author(s):  
Toyoko Yamanoi ◽  
Hiromoto Nakazawa
Keyword(s):  
Large Diameter ◽  
Preferred Orientation ◽  
X Rays ◽  
X Ray Diffraction ◽  
Parallel Beam ◽  
X Ray ◽  
Orientation Effects ◽  
Powder Samples ◽  
Xrd Patterns ◽  
Integrated Intensities

A parallel-beam X-ray diffraction geometry using X-ray guide tubes is proposed to eliminate preferred-orientation effects in powder X-ray diffraction (XRD) patterns and for new applications of XRD. A bundle of X-ray guide tubes (polycapillaries) is used to provide an intense quasi-parallel (approximately 0.2° divergence) and large-diameter (approximately 20 mm) beam of X-rays needed for parallel-beam diffractometry. Mica and silicon particles were agitated inside a cylindrical chamber by a steady flow of N2gas so that they were randomly oriented. The quasi-parallel incident X-ray beam passed through the cloud of floating particles. The diffracted X-rays were detected using a standard 2θ diffractometer. The integrated intensities observed agree well with those calculated from the known model of the crystal structure. This result demonstrates that this type of diffractometry is capable of avoiding preferred-orientation effects and of collecting XRD data for moving powder samples.

X-ray diffraction properties of curved crystal diffractors

1992 ◽  
Vol 50 (2) ◽  
pp. 1734-1735
Author(s):  
W. Z. Chang ◽  
D. B. Wittry
Keyword(s):  
Diffraction Theory ◽  
X Rays ◽  
Diffraction Image ◽  
X Ray Diffraction ◽  
Rocking Curve ◽  
X Ray ◽  
Bent Crystal ◽  
Diffraction Geometry ◽  
Crystal Parameter ◽  
Quantitative Procedure

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.

Investigation of the phase shift in X-ray forward diffraction using an X-ray interferometer

1998 ◽  
Vol 5 (3) ◽  
pp. 967-968 ◽  
Author(s):  
Keiichi Hirano ◽  
Atsushi Momose
Keyword(s):  
Phase Shift ◽  
Silicon Crystal ◽  
Dynamical Theory ◽  
Perfect Crystal ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bragg Geometry

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.

scholarly journals X-ray crystal structure of a malonate-semialdehyde dehydrogenase fromPseudomonassp. strain AAC

2017 ◽  
Vol 73 (1) ◽  
pp. 24-28 ◽  
Author(s):  
Matthew Wilding ◽  
Colin Scott ◽  
Thomas S. Peat ◽  
Janet Newman
Keyword(s):  
Crystal Structure ◽  
Search Model ◽  
Molecular Replacement ◽  
X Rays ◽  
X Ray Diffraction ◽  
Acetyl Coa ◽  
Space Group ◽  
X Ray ◽  
Semialdehyde Dehydrogenase

The NAD-dependent malonate-semialdehyde dehydrogenase KES23460 fromPseudomonassp. strain AAC makes up half of a bicistronic operon responsible for β-alanine catabolism to produce acetyl-CoA. The KES23460 protein has been heterologously expressed, purified and used to generate crystals suitable for X-ray diffraction studies. The crystals belonged to space groupP212121and diffracted X-rays to beyond 3 Å resolution using the microfocus beamline of the Australian Synchrotron. The structure was solved using molecular replacement, with a monomer from PDB entry 4zz7 as the search model.

scholarly journals Electronic Excitations and Radiation Damage in Macromolecular Crystallography

Crystals ◽  
2018 ◽  
Vol 8 (7) ◽  
pp. 273 ◽  
Author(s):  
José Brandão-Neto ◽  
Leonardo Bernasconi
Keyword(s):  
Chemical Information ◽  
X Rays ◽  
Electronic Excitations ◽  
Macromolecular Crystallography ◽  
X Ray Diffraction ◽  
X Ray ◽  
Atomic Structures ◽  
Successful Approach ◽  
Structural Research

Macromolecular crystallography at cryogenic temperatures has so far provided the majority of the experimental evidence that underpins the determination of the atomic structures of proteins and other biomolecular assemblies by means of single crystal X-ray diffraction experiments. One of the core limitations of the current methods is that crystal samples degrade as they are subject to X-rays, and two broad groups of effects are observed: global and specific damage. While the currently successful approach is to operate outside the range where global damage is observed, specific damage is not well understood and may lead to poor interpretation of the chemistry and biology of the system under study. In this work, we present a phenomenological model in which specific damage is understood as the result of a single process, the steady excitation of crystal electrons caused by X-ray absorption, which acts as a trigger for the bulk effects that manifest themselves in the form of global damage and obscure the interpretation of chemical information from XFEL and synchrotron structural research.

Applications of High-Resolution Powder X-Ray Diffraction

2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch
Keyword(s):  
High Resolution ◽  
Synchrotron Radiation ◽  
Powder Diffraction ◽  
X Rays ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Structural Characterisation ◽  
Pdf Analysis

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.

scholarly journals Synchrotron Nano-Diffraction Study of Thermally Treated Asbestos Tremolite from Val d’Ala, Turin (Italy)

Minerals ◽  
2018 ◽  
Vol 8 (8) ◽  
pp. 311 ◽  
Author(s):  
Carlotta Giacobbe ◽  
Jonathan Wright ◽  
Dario Di Giuseppe ◽  
Alessandro Zoboli ◽  
Mauro Zapparoli ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Heat Treatment ◽  
Risk Management ◽  
Structure Analysis ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Adverse Health Effects ◽  
Nano Crystalline ◽  
Original Fibre

Nowadays, due to the adverse health effects associated with exposure to asbestos, its removal and thermal inertization has become one of the most promising ways for reducing waste risk management. Despite all the advances in structure analysis of fibers and characterization, some problems still remain that are very hard to solve. One challenge is the structure analysis of natural micro- and nano-crystalline samples, which do not form crystals large enough for single-crystal X-ray diffraction (SC-XRD), and their analysis is often hampered by reflection overlap and the coexistence of multiple fibres linked together. In this paper, we have used nano-focused synchrotron X-rays to refine the crystal structure of a micrometric tremolite fibres from Val d’Ala, Turin (Italy) after various heat treatment. The structure of the original fibre and after heating to 800 °C show minor differences, while the fibre that was heated at 1000 °C is recrystallized into pyroxene phases and cristobalite.

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