2D real space visualization of d values in polycrystalline bulk materials of different hardness

2021 ◽  
Vol 54 (2) ◽  
pp. 597-603
Author(s):  
Mari Mizusawa ◽  
Kenji Sakurai
Keyword(s):  
Lattice Distortion ◽  
Structural Information ◽  
Hardness Test ◽  
Real Space ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Imaging ◽  
D Values

Conventional X-ray diffraction measurements provide some average structural information, mainly on the crystal structure of the whole area of the given specimen, which might not be very uniform and may include different crystal structures, such as co-existing crystal phases and/or lattice distortion. The way in which the lattice plane changes due to strain also might depend on the position in the sample, and the average information might have some limits. Therefore, it is important to analyse the sample with good lateral spatial resolution in real space. Although various techniques for diffraction topography have been developed for single crystals, it has not always been easy to image polycrystalline materials. Since the late 1990s, imaging technology for fluorescent X-rays and X-ray absorption fine structure has been developed via a method that does not scan either a sample or an X-ray beam. X-ray diffraction imaging can be performed when this technique is applied to a synchrotron radiation beamline with a variable wavelength. The present paper reports the application of X-ray diffraction imaging to bulk steel materials with varying hardness. In this study, the distribution of lattice distortion of hardness test blocks with different hardness was examined. Via this 2D visualization method, the grains of the crystals with low hardness are large enough to be observed by X-ray diffraction contrast in real space. The change of the d value in the vicinity of the Vickers mark has also been quantitatively evaluated.

Micro Diffraction Imaging of Bulk Polycrystalline Materials

2006 ◽  
Vol 524-525 ◽  
pp. 273-278
Author(s):  
Thomas Wroblewski ◽  
A. Bjeoumikhov ◽  
Bernd Hasse
Keyword(s):  
High Spatial Resolution ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
Short Sample ◽  
X Ray ◽  
Detector Distance ◽  
Transmission Geometry ◽  
Diffraction Imaging ◽  
Position Sensitive

X-ray diffraction imaging applies an array of parallel capillaries in front of a position sensitive detector. Conventional micro channel plates of a few millimetre thickness have successfully been used as collimator arrays but require short sample to detector distances to achieve high spatial resolution. Furthermore, their limited absorption restricts their applications to low energy X-rays of around 10 keV. Progress in the fabrication of long polycapillaries allows an increase in the sample to detector distance without decreasing resolution and the use of high X-ray energies enables bulk investigations in transmission geometry.

scholarly journals Energy Dispersive X-Ray Diffraction Imaging

2013 ◽  
Vol 772 ◽  
pp. 21-25 ◽  
Author(s):  
Jörn Donges ◽  
André Rothkirch ◽  
Thomas Wroblewski ◽  
Aniouar Bjeoumikhov ◽  
Oliver Scharf ◽  
...  
Keyword(s):  
Spatial Information ◽  
Structural Information ◽  
Reciprocal Space ◽  
Energy Dispersive ◽  
Polycrystalline Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Area Detector ◽  
Diffraction Imaging ◽  
Position Sensitive

Position resolved structural information from polycrystalline materials is usually obtained via micro beam techniques illuminating only a single spot of the specimen. Multiplexing in reciprocal space is achieved either by the use of an area detector or an energy dispersive device. Alternatively spatial information may be obtained simultaneously from a large part of the sample by using an array of parallel collimators between the sample and a position sensitive detector which suppresses crossfire of radiation scattered at different positions in the sample. With the introduction of an X-ray camera based on an energy resolving area detector (pnCCD) we could combine this with multiplexing in reciprocal space.

X-Ray Diffraction

2021 ◽  
pp. 408-480
Author(s):  
Kannan M. Krishnan
Keyword(s):  
Point Group ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
Symmetry Point Group ◽  
X Ray ◽  
Atomic Scattering ◽  
Scattering Factor ◽  
Diffraction Patterns ◽  
Lattice Planes

X-rays diffraction is fundamental to understanding the structure and crystallography of biological, geological, or technological materials. X-rays scatter predominantly by the electrons in solids, and have an elastic (coherent, Thompson) and an inelastic (incoherent, Compton) component. The atomic scattering factor is largest (= Z) for forward scattering, and decreases with increasing scattering angle and decreasing wavelength. The amplitude of the diffracted wave is the structure factor, F hkl, and its square gives the intensity. In practice, intensities are modified by temperature (Debye-Waller), absorption, Lorentz-polarization, and the multiplicity of the lattice planes involved in diffraction. Diffraction patterns reflect the symmetry (point group) of the crystal; however, they are centrosymmetric (Friedel law) even if the crystal is not. Systematic absences of reflections in diffraction result from glide planes and screw axes. In polycrystalline materials, the diffracted beam is affected by the lattice strain or grain size (Scherrer equation). Diffraction conditions (Bragg Law) for a given lattice spacing can be satisfied by varying θ or λ — for study of single crystals θ is fixed and λ is varied (Laue), or λ is fixed and θ varied to study powders (Debye-Scherrer), polycrystalline materials (diffractometry), and thin films (reflectivity). X-ray diffraction is widely applied.

Upsampling speckle patterns for coherent X-ray diffraction imaging

2013 ◽  
Vol 46 (2) ◽  
pp. 319-323 ◽  
Author(s):  
Y. Chushkin ◽  
F. Zontone
Keyword(s):  
Diffraction Pattern ◽  
Imaging Technique ◽  
Real Space ◽  
Field Of View ◽  
Combination Method ◽  
Pixel Size ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Imaging ◽  
Diffraction Patterns

Coherent X-ray diffraction imaging is a lensless imaging technique where an iterative phase-retrieval algorithm is applied to the speckle pattern, the far-field diffraction pattern produced by an isolated object. To ensure convergence to a unique solution, the diffraction pattern must be oversampled by a factor of two or more. Since the resolution in real space depends on the maximum wave vector where the intensity is detected,i.e.on the detector field of view, there is a practical limitation on oversampling in reciprocal space and resolution in real space that is ultimately determined by the number of pixels. This work shows that it is possible to reduce the effective pixel size and maintain the detector field of view by applying a linear combination method to shifted diffraction patterns. The feasibility of the method is demonstrated by reconstructing the images of test objects from diffraction patterns oversampled in each dimension by factors of 1.3 and 1.8 only. The described approach can be applied to any diffraction or imaging technique where the resolution is compromised by a large pixel size.

Three-Dimensional Coherent X-Ray Diffraction Microscopy

MRS Bulletin ◽  
2004 ◽  
Vol 29 (3) ◽  
pp. 177-181 ◽  
Author(s):  
Ian K. Robinson ◽  
Jianwei Miao
Keyword(s):  
Electron Microscopy ◽  
Three Dimensional ◽  
Real Space ◽  
Objective Lens ◽  
X Rays ◽  
X Ray Diffraction ◽  
Space Images ◽  
Thin Sections ◽  
X Ray ◽  
Penetration Ability

AbstractX-rays have been widely used in the structural analysis of materials because of their significant penetration ability, at least on the length scale of the granularity of most materials. This allows, in principle, for fully three-dimensional characterization of the bulk properties of a material. One of the main advantages of x-ray diffraction over electron microscopy is that destructive sample preparation to create thin sections is often avoidable. A major disadvantage of x-ray diffraction with respect to electron microscopy is its inability to produce real-space images of the materials under investigation—there are simply no suitable lenses available. There has been significant progress in x-ray microscopy associated with the development of lenses, usually based on zone plates, Kirkpatrick–Baez mirrors, or compound refractive lenses. These technologies are far behind the development of electron optics, particularly for the large magnification ratios needed to attain high resolution. In this article, the authors report progress toward the development of an alternative general approach to imaging, the direct inversion of diffraction patterns by computation methods. By avoiding the use of an objective lens altogether, the technique is free from aberrations that limit the resolution, and it can be highly efficient with respect to radiation damage of the samples. It can take full advantage of the three-dimensional capability that comes from the x-ray penetration. The inversion step employs computational methods based on oversampling to obtain a general solution of the diffraction phase problem.

Atmospheric coherent X-ray diffraction imaging for in situ structural analysis at SPring-8 Hyogo beamline BL24XU

2018 ◽  
Vol 25 (4) ◽  
pp. 1229-1237
Author(s):  
Yuki Takayama ◽  
Yuki Takami ◽  
Keizo Fukuda ◽  
Takamasa Miyagawa ◽  
Yasushi Kagoshima
Keyword(s):  
Structural Analysis ◽  
Control Device ◽  
Photon Flux ◽  
X Rays ◽  
Atmospheric Conditions ◽  
X Ray Diffraction ◽  
Macroporous Silica ◽  
X Ray ◽  
Diffraction Imaging

Coherent X-ray diffraction imaging (CXDI) is a promising technique for non-destructive structural analysis of micrometre-sized non-crystalline samples at nanometre resolutions. This article describes an atmospheric CXDI system developed at SPring-8 Hyogo beamline BL24XU for in situ structural analysis and designed for experiments at a photon energy of 8 keV. This relatively high X-ray energy enables experiments to be conducted under ambient atmospheric conditions, which is advantageous for the visualization of samples in native states. The illumination condition with pinhole-slit optics is optimized according to wave propagation calculations based on the Fresnel–Kirchhoff diffraction formula so that the sample is irradiated by X-rays with a plane wavefront and high photon flux of ∼1 × 1010 photons/16 µmø(FWHM)/s. This work demonstrates the imaging performance of the atmospheric CXDI system by visualizing internal voids of sub-micrometre-sized colloidal gold particles at a resolution of 29.1 nm. A CXDI experiment with a single macroporous silica particle under controlled humidity was also performed by installing a home-made humidity control device in the system. The in situ observation of changes in diffraction patterns according to humidity variation and reconstruction of projected electron-density maps at 5.2% RH (relative humidity) and 82.6% RH at resolutions of 133 and 217 nm, respectively, were accomplished.

Standard Deviations in X-Ray Stress and Elastic Constants Due to Counting Statistics

1988 ◽  
Vol 32 ◽  
pp. 377-388 ◽  
Author(s):  
Masanori Kurita
Keyword(s):  
Elastic Constants ◽  
Stress Measurement ◽  
Steel Specimen ◽  
Polycrystalline Materials ◽  
X Rays ◽  
Confidence Limits ◽  
X Ray Diffraction ◽  
X Ray ◽  
Standard Deviations ◽  
Counting Statistics

AbstractX-ray diffraction can be used to nondestructively measure residual stress of polycrystalline materials. In x-ray stress measurement, it is important to determine a stress constant experimentally in order to measure the stress accurately. However, every value measured by x-ray diffraction has statistical errors arising from counting statistics. The equations for calculating the standard deviations of the stress constant and elastic constants measured by x-rays are derived analytically in order to ascertain the reproducibility of the measured values. These standard deviations represent the size of the variability caused by counting statistics, and can be calculated from a single set of measurements by using these equations. These equations can apply Lu any meuhud for x-ray stress ifiesuremenL. The variances of the x-ray stress and elastic constants are expressed in terms of the linear combinations of the variances of the peak position. The confidence limits of these constants of a quenched and tempered steel specimen were determined by the Gaussian curve method. The 95% confidence limits of the stress constant were -314 ± 25 MFa/deg.

scholarly journals Utilizing broadband X-rays in a Bragg coherent X-ray diffraction imaging experiment

2016 ◽  
Vol 23 (5) ◽  
pp. 1241-1244 ◽  
Author(s):  
Wonsuk Cha ◽  
Wenjun Liu ◽  
Ross Harder ◽  
Ruqing Xu ◽  
Paul H. Fuoss ◽  
...  
Keyword(s):  
Three Dimensional ◽  
Three Dimensions ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Individual Crystal ◽  
Sample Motion ◽  
Diffraction Imaging ◽  
Individual Grains

A method is presented to simplify Bragg coherent X-ray diffraction imaging studies of complex heterogeneous crystalline materials with a two-stage screening/imaging process that utilizes polychromatic and monochromatic coherent X-rays and is compatible within situsample environments. Coherent white-beam diffraction is used to identify an individual crystal particle or grain that displays desired properties within a larger population. A three-dimensional reciprocal-space map suitable for diffraction imaging is then measured for the Bragg peak of interest using a monochromatic beam energy scan that requires no sample motion, thus simplifyingin situchamber design. This approach was demonstrated with Au nanoparticles and will enable, for example, individual grains in a polycrystalline material of specific orientation to be selected, then imaged in three dimensions while under load.

Three-Dimensional X-Ray Diffraction Microscopy Using High-Energy X-Rays

MRS Bulletin ◽  
2004 ◽  
Vol 29 (3) ◽  
pp. 166-169 ◽  
Author(s):  
Henning F. Poulsen ◽  
Dorte Juul Jensen ◽  
Gavin B.M. Vaughan
Keyword(s):  
Materials Science ◽  
Three Dimensional ◽  
High Energy ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Reconstruction Methods ◽  
The Individual ◽  
Individual Grains

AbstractThree-dimensional x-ray diffraction (3DXRD) microscopy is a tool for fast and nondestructive characterization of the individual grains, subgrains, and domains inside bulk materials. The method is based on diffraction with very penetrating hard x-rays (E ≥ 50 keV), enabling 3D studies of millimeter-to-centimeter-thick specimens.The position, volume, orientation, and elastic and plastic strain can be derived for hundreds of grains simultaneously. Furthermore, by applying novel reconstruction methods, 3D maps of the grain boundaries can be generated. The 3DXRD microscope in use at the European Synchrotron Radiation Facility in Grenoble, France, has a spatial resolution of ∼5 μm and can detect grains as small as 150 nm. The technique enables, for the first time, dynamic studies of the individual grains within polycrystalline materials. In this article, some fundamental materials science applications of 3DXRD are reviewed: studies of nucleation and growth kinetics during recrystallization, recovery, and phase transformations, as well as studies of polycrystal deformation.

scholarly journals Cryogenic coherent X-ray diffraction imaging of biological samples at SACLA: a correlative approach with cryo-electron and light microscopy

2016 ◽  
Vol 72 (2) ◽  
pp. 179-189 ◽  
Author(s):  
Yuki Takayama ◽  
Koji Yonekura
Keyword(s):  
Light Microscopy ◽  
Biological Samples ◽  
Free Electron ◽  
Free Electron Laser ◽  
X Rays ◽  
X Ray Diffraction ◽  
Cell Organelles ◽  
X Ray ◽  
Electron And Light Microscopy ◽  
Diffraction Imaging

Coherent X-ray diffraction imaging at cryogenic temperature (cryo-CXDI) allows the analysis of internal structures of unstained, non-crystalline, whole biological samples in micrometre to sub-micrometre dimensions. Targets include cells and cell organelles. This approach involves preparing frozen-hydrated samples under controlled humidity, transferring the samples to a cryo-stage inside a vacuum chamber of a diffractometer, and then exposing the samples to coherent X-rays. Since 2012, cryo-coherent diffraction imaging (CDI) experiments have been carried out with the X-ray free-electron laser (XFEL) at the SPring-8 Ångstrom Compact free-electron LAser (SACLA) facility in Japan. Complementary use of cryo-electron microscopy and/or light microscopy is highly beneficial for both pre-checking samples and studying the integrity or nature of the sample. This article reports the authors' experience in cryo-XFEL-CDI of biological cells and organelles at SACLA, and describes an attempt towards reliable and higher-resolution reconstructions, including signal enhancement with strong scatterers and Patterson-search phasing.

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