scholarly journals Quantitative powder diffraction using a (2 + 3) surface diffractometer and an area detector

2021 ◽  
Vol 54 (4) ◽  
Author(s):  
Giuseppe Abbondanza ◽  
Alfred Larsson ◽  
Francesco Carlá ◽  
Edvin Lundgren ◽  
Gary S. Harlow
Keyword(s):  
Powder Diffraction ◽  
High Energy ◽  
Fiber Texture ◽  
X Ray Diffraction ◽  
Measured Intensity ◽  
X Ray ◽  
Area Detector ◽  
Sample Orientation ◽  
Instrumental Resolution ◽  
Textured Materials

X-ray diffractometers primarily designed for surface X-ray diffraction are often used to measure the diffraction from powders, textured materials and fiber-texture samples in 2θ scans. Unlike in high-energy powder diffraction, only a fraction of the powder rings is typically measured, and the data consist of many detector images across the 2θ range. Such diffractometers typically scan in directions not possible on a conventional laboratory diffractometer, which gives enhanced control of the scattering vector relative to the sample orientation. There are, however, very few examples where the measured intensity is directly used, such as for profile/Rietveld refinement, as is common with other powder diffraction data. Although the underlying physics is known, converting the data is time consuming and the appropriate corrections are dispersed across several publications, often not with powder diffraction in mind. This paper presents the angle calculations and correction factors required to calculate meaningful intensities for 2θ scans with a (2 + 3)-type diffractometer and an area detector. Some of the limitations with respect to texture, refraction and instrumental resolution are also discussed, as is the kind of information that one can hope to obtain.

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].

The In Situ Study on the Micro-Structural Characters of IF Steel at Early Stage of Recrystallization Using High-Energy X-Ray

2008 ◽  
Vol 575-578 ◽  
pp. 972-977
Author(s):  
He Tong ◽  
Yan Dong Liu ◽  
Q.W. Jiang ◽  
Y. Ren ◽  
G. Wang ◽  
...  
Keyword(s):  
Annealing Temperature ◽  
Early Stage ◽  
High Energy ◽  
Fiber Texture ◽  
Interstitial Free ◽  
If Steel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cold Rolled

High-energy synchrotron diffraction offers great potential for experimental study of recrystallization kinetics. A fine experimental design to study the recrystallization mechanism of Interstitial Free (IF) steel was implemented in this work. In-situ annealing process of cold-rolled IF steel with 80% reduction was observed using high-energy X-ray diffraction. Results show that, the diffraction intensity of {001}<110> and {112}<110> belong to α-fiber texture component decreased with the annealing temperature increased while {111}<110> did nearly not change and {111}<112> increased; the FMTH decreasing and d-space changing with annealing temperature increasing indicated that the residual stress relaxed completely during recovery.

scholarly journals Powder crystallography on macromolecules

2007 ◽  
Vol 64 (1) ◽  
pp. 169-180 ◽  
Author(s):  
I. Margiolaki ◽  
J. P. Wright
Keyword(s):  
Powder Diffraction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Small Proteins ◽  
Synchrotron Powder Diffraction ◽  
Wide Range ◽  
Instrumental Resolution ◽  
Rich Information ◽  
The Rich ◽  
Peak Widths

Following the seminal work of Von Dreele, powder X-ray diffraction studies on proteins are being established as a valuable complementary technique to single-crystal measurements. A wide range of small proteins have been found to give synchrotron powder diffraction profiles where the peak widths are essentially limited only by the instrumental resolution. The rich information contained in these profiles, combined with developments in data analysis, has stimulated research and development to apply the powder technique to microcrystalline protein samples. In the present work, progress in using powder diffraction for macromolecular crystallography is reported.

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.

A novel approach to micro-sample X-ray powder diffraction using nylon loops

2003 ◽  
Vol 36 (6) ◽  
pp. 1480-1481 ◽  
Author(s):  
Nattamai S. P. Bhuvanesh ◽  
Joseph H. Reibenspies
Keyword(s):  
Single Crystal ◽  
Diffraction Pattern ◽  
Powder Diffraction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Area Detector ◽  
Novel Approach ◽  
Novel Method

A novel method for sample mounting to obtain powder diffraction from very small amounts of samples (ranging from micrograms down to a few nanograms), by using a combination of multiwire area detector, three-circle diffractometer, monochromatic CuKα radiation and 10 µm nylon loops, has been developed. This method exploits customary single-crystal approaches to collect the powder diffraction pattern, which overcomes many of the limitations of conventional powder X-ray diffraction.

Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis

2016 ◽  
Vol 52 (96) ◽  
pp. 13865-13868 ◽  
Author(s):  
Saul J. Moorhouse ◽  
Yue Wu ◽  
Hannah C. Buckley ◽  
Dermot O'Hare
Keyword(s):  
High Temperature ◽  
Molten Salt ◽  
Powder Diffraction ◽  
High Energy ◽  
Chemical Processes ◽  
Molten Salt Synthesis ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray

We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses.

A versatile X-ray diffraction station at LNLS (Brazil)

1998 ◽  
Vol 5 (3) ◽  
pp. 491-493 ◽  
Author(s):  
Cesar Cusatis ◽  
Margareth Kobayashi Franco ◽  
Edson Kakuno ◽  
Carlos Giles ◽  
Sergio Morelhão ◽  
...  
Keyword(s):  
Single Crystal ◽  
Powder Diffraction ◽  
High Energy ◽  
High Energy Resolution ◽  
High Angular Resolution ◽  
X Ray Diffraction ◽  
Double Crystal ◽  
X Ray ◽  
And Control ◽  
Imaging Plates

Versatility was a major consideration in the project to provide an X-ray diffraction station at LNLS. At least two techniques are possible at the station: powder diffraction and multiple single-crystal diffraction. A two-crystal monochromator based on monolithic elastic translators, developed at LNLS, with sagittal focusing by the second crystal, allows 10 mrad of a ≥2 keV monochromatic beam to be used on the diffractometer. The station is equipped with a fast scintillation detector, imaging plates, a high-energy-resolution pin-diode detector, an ionization chamber and a high-angular-resolution soller slit. The data collection and control hardware and software were also developed at LNLS. The θ–2θ goniometry for powder diffraction on this 1 m-diameter diffractometer is based on commercial rotation tables. The multiple single-crystal goniometry is realized by an independent elastic axis driven by differential micrometers for both high- and low-resolution angular movements. At least four independent axes can be positioned as necessary on the diffractometer table. Powder diffractograms and double-crystal rocking curves collected with the synchrotron beam show the expected quality.

Determination of directionally dependent structural and microstructural information using high-energy X-ray diffraction

2008 ◽  
Vol 41 (6) ◽  
pp. 1109-1114 ◽  
Author(s):  
J. E. Daniels
Keyword(s):  
Zirconium Alloys ◽  
High Energy ◽  
Ferroelectric Ceramics ◽  
X Ray Diffraction ◽  
Large Area ◽  
X Ray ◽  
Area Detector ◽  
Profile Fitting ◽  
Multiple Data Sets ◽  
Dependent Sample

High-energy synchrotron X-ray diffraction using a monochromatic beam and large area detector offers a unique method for the study of directionally dependent sample information. The very short wavelengths and subsequent low scattering angles mean that scattering vectors at all angles approximately perpendicular to the beam direction are sampled simultaneously. Here a method is proposed and demonstrated in which the magnitude and directions of structural and microstructural changes can be determined with higher resolution than was possible with previously used techniques. The method takes advantage of parametric refinements over multiple data sets using the profile fitting packageTOPAS. Examples of the technique applied to the study of strains in multiphase zirconium alloys and microstructural texture in ferroelastic/ferroelectric ceramics are given. The angular precision in lattice strain for a diffraction image with good statistics is found to be below 0.1°.

scholarly journals The Extreme Conditions Beamline P02.2 and the Extreme Conditions Science Infrastructure at PETRA III

2015 ◽  
Vol 22 (4) ◽  
pp. 908-924 ◽  
Author(s):  
H.-P. Liermann ◽  
Z. Konôpková ◽  
W. Morgenroth ◽  
K. Glazyrin ◽  
J. Bednarčik ◽  
...  
Keyword(s):  
High Pressure ◽  
High Energy ◽  
Extreme Conditions ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
High Pressure Studies ◽  
Time Regime ◽  
Diamond Anvil ◽  
Instrumental Resolution

A detailed description is presented of the Extreme Conditions Beamline P02.2 for micro X-ray diffraction studies of matter at simultaneous high pressure and high/low temperatures at PETRA III, in Hamburg, Germany. This includes performance of the X-ray optics and instrumental resolution as well as an overview of the different sample environments available for high-pressure studies in the diamond anvil cell. Particularly emphasized are the high-brilliance and high-energy X-ray diffraction capabilities of the beamline in conjunction with the use of fast area detectors to conduct time-resolved compression studies in the millisecond time regime. Finally, the current capability of the Extreme Conditions Science Infrastructure to support high-pressure research at the Extreme Conditions Beamline and other PETRA III beamlines is described.

Characterizations of Synthetic 8mol% YSZ with Comparison to 3mol %YSZ for HT-SOFC

2020 ◽  
Vol 38 (4A) ◽  
pp. 491-500
Author(s):  
Abeer F. Al-Attar ◽  
Saad B. H. Farid ◽  
Fadhil A. Hashim
Keyword(s):  
Ionic Conductivity ◽  
Electrochemical Impedance ◽  
Structural Information ◽  
Impedance Analysis ◽  
High Energy ◽  
Yttria Stabilized Zirconia ◽  
X Ray Diffraction ◽  
Stabilized Zirconia ◽  
Powder Morphology ◽  
X Ray

In this work, Yttria (Y2O3) was successfully doped into tetragonal 3mol% yttria stabilized Zirconia (3YSZ) by high energy-mechanical milling to synthesize 8mol% yttria stabilized Zirconia (8YSZ) used as an electrolyte for high temperature solid oxide fuel cells (HT-SOFC). This work aims to evaluate the densification and ionic conductivity of the sintered electrolytes at 1650°C. The bulk density was measured according to ASTM C373-17. The powder morphology and the microstructure of the sintered electrolytes were analyzed via Field Emission Scanning Electron Microscopy (FESEM). The chemical analysis was obtained with Energy-dispersive X-ray spectroscopy (EDS). Also, X-ray diffraction (XRD) was used to obtain structural information of the starting materials and the sintered electrolytes. The ionic conductivity was obtained through electrochemical impedance spectroscopy (EIS) in the air as a function of temperatures at a frequency range of 100(mHz)-100(kHz). It is found that the 3YSZ has a higher density than the 8YSZ. The impedance analysis showed that the ionic conductivity of the prepared 8YSZ at 800°C is0.906 (S.cm) and it was 0.214(S.cm) of the 3YSZ. Besides, 8YSZ has a lower activation energy 0.774(eV) than that of the 3YSZ 0.901(eV). Thus, the prepared 8YSZ can be nominated as an electrolyte for the HT-SOFC.

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