2D and 3D X-Ray Structural Microscopy Using Submicron-Resolution Laue Microdiffraction

2004 ◽  
Vol 840 ◽  
Author(s):  
John D. Budai ◽  
Wenge Yang ◽  
Bennett C. Larson ◽  
Jonathan Z. Tischler ◽  
Wenjun Liu ◽  
...  
Keyword(s):  
Strain Tensor ◽  
Polycrystalline Aluminum ◽  
Length Scales ◽  
X Ray ◽  
Area Detector ◽  
Microscopy Technique ◽  
Area Of Interest ◽  
Grain Orientations ◽  
Diffraction Patterns ◽  
2D And 3D

ABSTRACTWe have developed a scanning, polychromatic x-ray microscopy technique with submicron spatial resolution at the Advanced Photon Source. In this technique, white undulator radiation is focused to submicron diameter using elliptical mirrors. Laue diffraction patterns scattered from the sample are collected with an area detector and then analyzed to obtain the local crystal structure, lattice orientation, and strain tensor. These new microdiffraction capabilities have enabled both 2D and 3D structural studies of materials on mesoscopic length-scales of tenths-to-hundreds of microns. For thin samples such as deposited films, 2D structural maps are obtained by step-scanning the area of interest. For example, 2D x-ray microscopy has been applied in studies of the epitaxial growth of oxide films. For bulk samples, a 3D differential-aperture x-ray microscopy technique has been developed that yields the full diffraction information from each submicron volume element. The capabilities of 3D x-ray microscopy are demonstrated here with measurements of grain orientations and grain boundary motion in polycrystalline aluminum during 3D thermal grain growth. X-ray microscopy provides the needed, direct link between the experimentally measured 3D microstructural evolution and the results of theory and modeling of materials processes on mesoscopic length scales.

On the calibration of high-energy X-ray diffraction setups. I. Assessing tilt and spatial distortion of the area detector

2014 ◽  
Vol 47 (3) ◽  
pp. 1042-1053 ◽  
Author(s):  
Andras Borbely ◽  
Loic Renversade ◽  
Peter Kenesei ◽  
Jonathan Wright
Keyword(s):  
Rotation Axis ◽  
Strain Tensor ◽  
Calibration Procedure ◽  
High Energy ◽  
European Synchrotron Radiation Facility ◽  
Data Sets ◽  
X Ray Diffraction ◽  
Spatial Distortion ◽  
X Ray ◽  
Area Detector

The geometry of high-energy X-ray diffraction setups using an area detector and a rotation axis is analysed. The present paper (part 1) describes the methodology for determining continuously varying spatial distortions and tilt of the area detector based on the reference diffraction rings of a certified powder. Analytical expressions describing the degeneration of Debye rings into ellipses are presented and a robust calibration procedure is introduced. It is emphasized that accurate detector calibration requires the introduction of spatial distortion into the equation describing the tilt. The method is applied to data sets measured at the Advanced Photon Source and at the European Synchrotron Radiation Facility using detectors with different physical characteristics, the GE 41RT flat-panel and the FReLoN4M detector, respectively. The spatial distortion of the detectors is compared with regard to their use in structural and strain tensor analysis, a subject treated in part 2 of the calibration work [Borbély, Renversade & Kenesei (2014).J. Appl. Cryst.Submitted].

Rapid small-angle X-ray diffraction of a tonically contracting molluscan smooth muscle recorded with imaging plates

1989 ◽  
Vol 22 (1) ◽  
pp. 72-74 ◽  
Author(s):  
Y. Tajima ◽  
K. Okada ◽  
O. Yoshida ◽  
T. Seto ◽  
Y. Amemiya
Keyword(s):  
Small Angle ◽  
Structural Changes ◽  
High Sensitivity ◽  
Imaging Plate ◽  
Layer Line ◽  
X Ray Diffraction ◽  
Thin Filaments ◽  
X Ray ◽  
Area Detector ◽  
Diffraction Patterns

Small-angle X-ray diffraction patterns from the anterior byssus retractor muscles of Mytilus edulis contracting tonically in response to stimulation with acetylcholine were recorded in a 30 s exposure with synchrotron radiation and a high-sensitivity X-ray area detector called an imaging plate. The 190 Å layer line from the thin filaments increased in intensity with increase in tonic tension up to 6 x 104 kg m−2. Above this value, the layer-line intensity remained almost constant and comparable to that for a contracting skeletal muscle, indicating that the same structural changes of the thin filaments occur in both muscles.

scholarly journals Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector

2017 ◽  
Vol 50 (3) ◽  
pp. 901-908 ◽  
Author(s):  
A. Abboud ◽  
C. Kirchlechner ◽  
J. Keckes ◽  
T. Conka Nurdan ◽  
S. Send ◽  
...  
Keyword(s):  
Elastic Strain ◽  
Strain Tensor ◽  
Energy Dispersive ◽  
Single Shot ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Laue Diffraction ◽  
Experimental Procedure ◽  
X Ray ◽  
Diffraction Patterns

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

On the calibration of high-energy X-ray diffraction setups. II. Assessing the rotation axis and residual strains

2014 ◽  
Vol 47 (5) ◽  
pp. 1585-1595 ◽  
Author(s):  
Andras Borbély ◽  
Loïc Renversade ◽  
Peter Kenesei
Keyword(s):  
Residual Strain ◽  
Rotation Axis ◽  
Strain Tensor ◽  
High Energy ◽  
Laboratory Frame ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Area Detector ◽  
Residual Strains

The calibration of high-energy X-ray diffraction setups using an area detector and a rotation axis is discussed. The characterization of the tilt and spatial distortions of an area detector was discussed in part one of this series [Borbély, Renversade, Kenesei & Wright (2014).J. Appl. Cryst.47, 1042–1053]. Part II links the detector frame to the laboratory frame comprising an additional rotation axis and introduces a general diffractometer equation accounting for all sources of misalignment. Additionally, an independent high-accuracy method for the evaluation of the crystallographic orientation and cell parameters of the undeformed reference crystal is presented. Setup misalignments are mainly described in terms of a residual strain tensor, considered as a quality label of the diffractometer. The method is exemplified using data sets acquired at beamlines ID11 (European Synchrotron Radiation Facility) and 1-ID (Advanced Photon Source) on Al and W single crystals, respectively. The results show that the residual strain tensor is mainly determined by the detector spatial distortion, and values as small as 1–2 × 10−4can be practically achieved.

X-ray Microbeam Diffraction Measurements in Polycrystalline Aluminum and Copper Thin Films

2003 ◽  
Vol 795 ◽  
Author(s):  
L. E. Moyer ◽  
G. S. Cargill ◽  
W. Yang ◽  
B. C. Larson ◽  
G. E. Ice
Keyword(s):  
Thin Films ◽  
Crystallographic Orientation ◽  
Grain Orientation ◽  
Strain Tensor ◽  
Polycrystalline Aluminum ◽  
Thermally Induced ◽  
X Ray ◽  
Glass Substrates ◽  
Orientation Mapping ◽  
Residual Strains

ABSTRACTThermally induced residual strains in polycrystalline Cu and Al films on single crystal Si and glass substrates, respectively, have been examined on a grain-by-grain basis by x-ray microbeam diffraction. The crystallographic orientation and the deviatoric strain tensor, εij*, are determined for each grain by white beam Laue diffraction. From grain orientation mapping and strain tensor measurements, information is obtained about the distributions of strains for similarly oriented grains, about strain variations within single grains, and about grain-to-grain correlations of strains. This type of information may be useful in developing and testing theories for intergrain effects in strain evolution in polycrystals.

scholarly journals Determination of crystal size distribution by two-dimensional X-ray diffraction

2014 ◽  
Vol 70 (a1) ◽  
pp. C1131-C1131
Author(s):  
Alejandro Rodriguez-Navarro ◽  
Krzysztof Kudłacz
Keyword(s):  
Size Distribution ◽  
Crystal Size ◽  
High Sensitivity ◽  
Crystal Size Distribution ◽  
Polycrystalline Materials ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Area Detector ◽  
Diffraction Patterns

Polycrystalline materials properties and behaviour are ultimately determined by their crystallinity, phase composition and microstructure (i.e., crystal size, preferential orientation). Two-dimensional (2D) diffraction patterns collected with an area detector (i.e., CDD), available in modern X-ray diffractometers, contain detailed information about all these important material characteristics. Furthermore, recent advances in detector technologies permits the collection of high resolution diffraction patterns in which the microstructure of the material can be directly imaged. If the size of beam relative to the crystal size in the sample is adequately choosen, the diffraction pattern produced will have spotty rings in which the spots are the diffracted images of individual grains. The resolution of the image is mainly dependent on the characteristics of the X-ray beam (i.e., diameter, angular divergence), which can be modulated by X-ray optics, sample to detector distance, the pixel size of the detector and the sharpness of the point spread function. From these patterns, the crystal size distribution of different crystalline phases present in the sample can be independently determined using specialized software capable of extracting and combining the information contained in these patterns. This technique is applicable to materials with crystal sizes ranging from submicron to mm sizes and is complementary to techniques based on peak profile analyses (i.e., Scherrer method) which are applicable only to nanocrystalline materials. Finally, given the high sensitivity of current detectors, crystal size evolution can be followed in real-time to study important transformation processes such as crystallization, annealing, etc. The use of 2D X-ray diffraction as applied to microstructure characterization will be illustrated through several examples.

XRD2DScan: new software for polycrystalline materials characterization using two-dimensional X-ray diffraction

2006 ◽  
Vol 39 (6) ◽  
pp. 905-909 ◽  
Author(s):  
Alejandro B. Rodriguez-Navarro
Keyword(s):  
Polycrystalline Materials ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Area Detector ◽  
Multiple Data ◽  
Different Types ◽  
Ψ Angle ◽  
Data Files ◽  
Diffraction Patterns

XRD2DScanis a Windows application for displaying and analyzing two-dimensional X-ray diffraction patterns collected with an area detector. This software allows users to take full advantage of diffractometers that are equipped with an area detector but that cannot readily process the information contained in diffraction patterns from polycrystalline materials.XRD2DScanhas many capabilities for generating different types of scans (2θ scan, ψ scan,dspacingversusψ angle), which allows users to extract the maximum amount of information from two-dimensional patterns. Analyses of multiple data files can be fully automated using batch processing. The use of the software is illustrated through several examples.

Assessment of Deformation Behavior of Polycrystalline Aluminum Using Diffraction-Amalgamated Grain-Boundary Tracking (DAGT) Technique

2014 ◽  
Vol 794-796 ◽  
pp. 57-62
Author(s):  
Hiroyuki Toda ◽  
Takanobu Kamiko ◽  
Kentaro Uesugi ◽  
Akihisa Takeuchi ◽  
Yoshio Suzuki ◽  
...  
Keyword(s):  
Grain Boundary ◽  
Deformation Behavior ◽  
Local Strain ◽  
Model Alloy ◽  
Strain Mapping ◽  
Polycrystalline Aluminum ◽  
Boundary Tracking ◽  
X Ray ◽  
Hydrostatic Tension ◽  
Grain Orientations

A novel experimental method has been developed by amalgamating a pencil beam X-Ray diffraction (XRD) technique with the recently developed grain boundary tracking (GBT) technique. XRD and GBT are both non-destructive in-situ analysis techniques for characterizing bulk materials, which can be carried out close to the point of fracture. DAGT provides information about individual grain orientations and 1-micron-level grain morphologies in 3-dimensions (3D) together with high-density local strain mapping. An Al-3 mass % Cu model alloy was used to investigate its deformation behavior under tension. The morphology of the grains was determined by the X-ray microtomography (XMT) imaging and the liquid metal wetting technique, after which GBT provided an accurate description of the position and morphology of all the grains in a region of interests. Diffraction spots in the XRD experiments were related to grains, making it possible to describe crystallographic orientation of all the grains. It has been revealed that deformation is localized at both microscopic and meso-scopic levels. Inhomogeneous deformation was observed in each individual grain. In addition, a group of a few grains coordinately interacts and specific grain boundaries thereby exhibit intense strain localization. Hydrostatic tension was also observed at quadruple junction points and its mechanism was analyzed.

Evaluation of Freezing Methods by Low Temperature X-Ray Diffraction

1977 ◽  
Vol 35 ◽  
pp. 330-333
Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello
Keyword(s):  
Biological Materials ◽  
Molecular Organization ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
X Ray ◽  
Rate Dependent ◽  
Before And After ◽  
Freeze Etching ◽  
Diffraction Patterns ◽  
Set Up

Freeze-etching electron microscopy is currently one of the best methods for studying molecular organization of biological materials. Its application, however, is still limited by our imprecise knowledge about the perturbations of the original organization which may occur during quenching and fracturing of the samples and during the replication of fractured surfaces. Although it is well known that the preservation of the molecular organization of biological materials is critically dependent on the rate of freezing of the samples, little information is presently available concerning the nature and the extent of freezing-rate dependent perturbations of the original organizations. In order to obtain this information, we have developed a method based on the comparison of x-ray diffraction patterns of samples before and after freezing, prior to fracturing and replication.Our experimental set-up is shown in Fig. 1. The sample to be quenched is placed on its holder which is then mounted on a small metal holder (O) fixed on a glass capillary (p), whose position is controlled by a micromanipulator.

Examination of Rabbit Fc Crystals

1968 ◽  
Vol 26 ◽  
pp. 140-141
Author(s):  
J. P. Robinson ◽  
P. G. Lenhert
Keyword(s):  
Molecular Weight ◽  
Flat Plate ◽  
Phosphate Buffer ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Neutral Ph ◽  
Small Crystals ◽  
Carbon Coated ◽  
Diffraction Patterns

Crystallographic studies of rabbit Fc using X-ray diffraction patterns were recently reported. The unit cell constants were reported to be a = 69. 2 A°, b = 73. 1 A°, c = 60. 6 A°, B = 104° 30', space group P21, monoclinic, volume of asymmetric unit V = 148, 000 A°3. The molecular weight of the fragment was determined to be 55, 000 ± 2000 which is in agreement with earlier determinations by other methods.Fc crystals were formed in water or dilute phosphate buffer at neutral pH. The resulting crystal was a flat plate as previously described. Preparations of small crystals were negatively stained by mixing the suspension with equal volumes of 2% silicotungstate at neutral pH. A drop of the mixture was placed on a carbon coated grid and allowed to stand for a few minutes. The excess liquid was removed and the grid was immediately put in the microscope.

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