scholarly journals In-house-built single-crystal anomalous X-ray diffraction measurement system using white X-rays and an energy dispersive detector

2021 ◽  
Vol 129 (9) ◽  
pp. 594-600
Author(s):  
Rayko SIMURA ◽  
Hisanori YAMANE ◽  
Terutoshi SAKAKURA ◽  
Kazumasa SUGIYAMA
Keyword(s):  
Single Crystal ◽  
Measurement System ◽  
Energy Dispersive ◽  
Diffraction Measurement ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

scholarly journals Influence of Layer Removal Methods in Residual Stress Profiling of a Shot Peened Steel Using X-Ray Diffraction

2014 ◽  
Vol 996 ◽  
pp. 175-180 ◽  
Author(s):  
Rasha Alkaisee ◽  
Ru Lin Peng
Keyword(s):  
Residual Stress ◽  
Chemical Etching ◽  
Stress Measurement ◽  
Diffraction Measurement ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Layer Removal ◽  
Compressive Stresses ◽  
The Difference

For X-Ray Diffraction Measurement of Depth Profiles of Residual Stress, Step-Wise Removal of Materials has to be Done to Expose the Underneath Layers to the X-Rays. this Paper Investigates the Influence of Layer Removal Methods, Including Electro-Polishing in Two Different Electrolytes and Chemical Etching, on the Accuracy of Residual Stress Measurement. Measurements on Two Shot-Peened Steels Revealed Large Discrepancy in Subsurface Distributions of Residual Stress Obtained with the Respective Methods. Especially, the Chemical Etching Yielded much Lower Subsurface Compressive Stresses than the Electro-Polishing Using a so Called AII Electrolyte. the Difference was Explained by the Influence of the Different Layer Removal Methods on the Microscopic Roughness.

A Re-investigation of the Crystal Structure of the Perovskite PbZrO3 by X-ray and Neutron Diffraction

1997 ◽  
Vol 53 (1) ◽  
pp. 135-142 ◽  
Author(s):  
D. L. Corker ◽  
A. M. Glazer ◽  
J. Dec ◽  
K. Roleder ◽  
R. W. Whatmore
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Neutron Diffraction ◽  
Single Crystal ◽  
Lead Zirconate ◽  
Conclusive Evidence ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure Investigations

The crystal structure of the perovskite lead zirconate PbZrO3 has been redetermined using single-crystal X-ray diffraction (Mo Kα radiation, λ = 0.71069 Å). Single-crystal data at 100 K: space group. Pbam, a = 5.884 (1), b = 11.787 (3), c = 8.231 (2) Å, V = 570.85 Å3 with Z = 8, μ = 612.6 cm−1, D x = 8.06 Mg m−3, F(000) = 1168, final R = 0.033, wR = 0.061 over 555 reflections with I > 2σ(I). An investigation is made into previous contradicting reports of a possible disorder in the O atoms and their origin by examining the crystal pseudo-symmetry. Information distinguishing an ordered and disordered oxygen substructure is shown to reside in weak l odd reflections. Because of their extremely low intensities these reflections have not contributed sufficiently in previous X-ray structure investigations and hence, to date, conclusive evidence differentiating between ordered and disordered models has not been possible. By collecting single-crystal X-ray data at low temperature and by using exceptionally long scans on selected hkl, l odd, reflections, a new accurate structure determination is presented and discussed, showing the true ordered oxygen positions. Because of the large difference in scattering factors between lead and oxygen when using X-rays, a neutron diffraction Rietveld refinement using polycrystalline samples (D1A instrument, ILL, λ = 1.90788 Å) is also reported as further evidence to support the true ordered oxygen structure revealed by the low-temperature X-ray analysis.

X-rays Powder Diffraction Measurement in Reactive Atmospheres at 1000 °C and 7 MPa (1000 PSIG)

1978 ◽  
Vol 22 ◽  
pp. 19-30
Author(s):  
F. A. Mauer ◽  
C. R. Robbins
Keyword(s):  
Phase Composition ◽  
Flexural Strength ◽  
Powder Diffraction ◽  
Pressure Vessel ◽  
Coal Gasification ◽  
Energy Dispersive ◽  
Diffraction Measurement ◽  
X Rays ◽  
X Ray

Studies of changes in the flexural strength and phase composition of castable refractories are being carried out in simulated coal gasification reactor environments. This paper describes a pressure vessel in which x-ray powder diffraction measurements can be made by an energy dispersive method while the specimen is being heated to temperatures as high as 1000°C in atmospheres containing H2O, CO2, CO, H2, CH4, NH3 , and H2S at pressures up to 7 MPa (1000 psig).

Evaluation of Tri-Axial Magnetostriction in Cube-Oriented Fe-Ga Single Crystal by Using X-Ray Diffraction Method

2017 ◽  
Vol 909 ◽  
pp. 300-305 ◽  
Author(s):  
Takehito Ikeuchi ◽  
Akihiro Koyama ◽  
Muneyuki Imafuku ◽  
Shun Fujieda ◽  
Yusuke Onuki ◽  
...  
Keyword(s):  
Magnetic Field ◽  
Single Crystal ◽  
Volume Fraction ◽  
Diffraction Method ◽  
Diffraction Measurement ◽  
Magnetic Field Direction ◽  
Magnetic Domains ◽  
X Ray Diffraction ◽  
X Ray

We carried out in situ tri-axial magnetostriction analysis for cube-oriented Fe-18%Ga single crystal by X-ray diffraction measurement under magnetic field. Periodic change in tri-axial magnetostriction with applied magnetic field direction was clearly observed. However, those values in [100] and [010] directions were not equivalent. Theoretical calculation of magnetostriction considering domain structure revealed this is caused by the non-equivalent volume fraction of initial magnetic domains.

scholarly journals X-Ray Diffraction of Magnetically Oriented Microcrystals of Protein

2014 ◽  
Vol 70 (a1) ◽  
pp. C349-C349
Author(s):  
Shu Tsukui ◽  
Fumiko Kimura ◽  
Kimihiko Mizutani ◽  
Bunzo Mikami ◽  
Tsunehisa Kimura
Keyword(s):  
Single Crystal ◽  
Three Dimensional ◽  
Water Soluble ◽  
Dimensional Structure ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Consolidation Process ◽  
X Ray ◽  
Three Dimensional Structure

Elucidation of the three-dimensional structure of biomolecules is of great importance because the three-dimensional structure is closely related to biological functions. X-ray single-crystal analysis is powerful method to analyze the structure, but it is sometimes difficult to grow a crystal sufficiently large for conventional or even synchrotron single-crystal X-ray measurement. We recently reported on a magnetically oriented microcrystal array (MOMA) [1] that is a composite in which microcrystals are aligned three-dimensionally in polymer matrix. Microcrystals are suspended in an ultraviolet-curable monomer and rotated non-uniformly in a static magnetic field to achieve three dimensional crystal alignment. Then, the monomer is photopolymerized to maintain the achieved alignment. We have successfully demonstrated that X-ray single crystal structure determinations through MOMA are possible for low molecular weight compounds [2] as well as protein. [3] However, the method with MOMA has two drawbacks: (i) the sample microcrystals cannot be recovered from a MOMA, which is especially serious problem in case of proteins, and (ii) the alignment is deteriorated during the consolidation process, causing low resolution. In this study, we attempt to solve these problems. First, we use a water-soluble sol as microcrystalline media and consolidate the alignment by gelation, which makes the recovery of microcrystals possible. Second, a magnetically oriented microcrystal suspension (MOMS) is used for in-situ X-ray diffraction measurement, which makes the sample recovery possible and enhances the resolution. We use lysozyme as a model protein for both cases. The in-situ method with in-house X-ray diffractometer gave diffraction spots about 3.0 Å resolutions. We plan to perform the same experiment at SPring-8.

Oxford HEXameter: Laboratory High Energy X-Ray Diffractometer for Bulk Residual Stress Analysis

2006 ◽  
Vol 524-525 ◽  
pp. 743-748 ◽  
Author(s):  
Alexander M. Korsunsky ◽  
Shu Yan Zhang ◽  
Daniele Dini ◽  
Willem J.J. Vorster ◽  
Jian Liu
Keyword(s):  
Accurate Determination ◽  
High Energy ◽  
Energy Dispersive ◽  
Detector Response ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
New Instrument ◽  
Synchrotron Beamlines

Diffraction of penetrating radiation such as neutrons or high energy X-rays provides a powerful non-destructive method for the evaluation of residual stresses in engineering components. In particular, strain scanning using synchrotron energy-dispersive X-ray diffraction has been shown to offer a fast and highly spatially resolving measurement technique. Synchrotron beamlines provide best available instruments in terms of flux and low beam divergence, and hence spatial and measurement resolution and data collection rate. However, despite the rapidly growing number of facilities becoming available in Europe and across the world, access to synchrotron beamlines for routine industrial and research use remains regulated, comparatively slow and expensive. A laboratory high energy X-ray diffractometer for bulk residual strain evaluation (HEXameter) has been developed and built at Oxford University. It uses a twin-detector setup first proposed by one of the authors in the energy dispersive X-ray diffraction mode and allows simultaneous determination of macroscopic and microscopic strains in two mutually orthogonal directions that lie approximately within the plane normal to the incident beam. A careful procedure for detector response calibration is used in order to facilitate accurate determination of lattice parameters by pattern refinement. The results of HEXameter measurements are compared with synchrotron X-ray data for several samples e.g. made from a titanium alloy and a particulate composite with an aluminium alloy matrix. Experimental results are found to be consistent with synchrotron measurements and strain resolution close to 2×10-4 is routinely achieved by the new instrument.

scholarly journals Detailed single crystal studies on silicates using neutron diffraction

2014 ◽  
Vol 70 (a1) ◽  
pp. C1110-C1110
Author(s):  
Martin Meven ◽  
G. Gatta
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Room Temperature ◽  
Structural Features ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Order And Disorder ◽  
Structural Details ◽  
Displacement Regime

Up to now minerals of the silicate family are an interesting and versatile topic of research. Different members of the epidote, lithium tourmaline and beryl groups with very different structural features were studied on the single crystal diffractometer HEIDI at the hot source of the Heinz Maier-Leibnitz Zentrum in Garching (MLZ) in the recent past. The combination of neutron and X-ray diffraction in combination with other methods revealed for each of the studied minerals valuable information about their structural details. Epidote, an important mineral for metamorphic or magmatic petrology was studied with neutrons at room temperature and at 1070 K. The results confirm the high structural stability with no dehydration and only slight thermal expansion [1]. A combined study with x-ray and neutron diffraction on the complex boro-cyclo-silicate elbaite give insight to the displacement regime and H and O order and disorder respectively [2]. Combined single crystal diffraction with x-rays at room temperature and with neutrons at 2.3 K on pezzottaite, an obverse/reverse twin of the beryl family reveals a complex displacement regime with possible partial H2O replacement [3].

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