In Situ Three-Dimensional Orientation Mapping in Plastically-Deformed Polycrystalline Iron by Three-Dimensional X-Ray Diffraction

In situ three-dimensional crystallographic orientation mapping in plastically-deformed polycrystalline iron is demonstrated using a modified three-dimensional x-ray diffraction method. This voxel-by-voxel measurement method enables the observation of intragranular orientation distribution. The experiment is performed using coarse-grained ferrite with a mean grain size of ~ 60 μm and an incident x-ray beam with a beam size of 20 μm × 20 μm. Grains averagely rotate approximately toward the <110> preferred orientation of body-centered cubic uniaxial tensile texture. Intragranular orientation distributions are spread as the tensile strain increases to 10.7 %. Furthermore, intragranular multidirectional rotations are observed in grains near the <100> and <111> corners in the inverse pole figure.

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Study of The Hydrothermal Synthesis of Gallium Phosphates Using in Situ Time-Resolved X-Ray Diffraction

MRS Proceedings ◽

10.1557/proc-547-63 ◽

1998 ◽

Vol 547 ◽

Cited By ~ 1

Author(s):

R.I. Walton ◽

T. Loiseau ◽

R.J. Francis ◽

D. O'Hare ◽

G. Férey

Keyword(s):

Kinetic Data ◽

Three Dimensional ◽

Diffraction Method ◽

Effect Of Temperature ◽

X Ray Diffraction ◽

Hydrothermal Conditions ◽

Time Resolved ◽

X Ray ◽

Phosphorus Source

AbstractThe hydrothermal crystallisation (130-180 °C) of three-dimensional open-framework gallium and aluminium oxyfluoro-phosphates with the ULM-3 and ULM-4 structures have been studied in situ for the first time. The in situ energy-dispersive X-ray diffraction method has allowed the formation of the crystalline products to be observed under hydrothermal conditions The integrated areas of the strongest Bragg reflections has allowed quantitative kinetic data to be extracted. The effect of temperature, phosphorus source, templating agent have been investigated. The nature of phosphorus source in the reaction mixture has been found to affect dramatically the course of reaction for certain combinations of amine and temperature. Previously unobserved transient crystalline phases have been seen during the production of ULM-3 gallium phosphates when P2O5 or polyphosphoric acid are used. The formation of these intermediates affects the kinetics of product growth. In the case of the aluminium ULM-3 materials reaction always proceeds via a crystalline intermediate whatever phosphorus source is used. The ULM-4 framework materials are found to always crystallise directly with no evidence for any intermediates. Kinetic data for each system have been modelled using standard solid-state chemistry expressions, and these calculations indicate the reactions to be diffusion controlled.

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In Situ Coherent X-ray Diffraction during Three-Point Bending of a Au Nanowire: Visualization and Quantification

Quantum Beam Science ◽

10.3390/qubs2040024 ◽

2018 ◽

Vol 2 (4) ◽

pp. 24 ◽

Cited By ~ 4

Author(s):

Anton Davydok ◽

Thomas Cornelius ◽

Zhe Ren ◽

Cedric Leclere ◽

Gilbert Chahine ◽

...

Keyword(s):

Three Dimensional ◽

Reciprocal Space ◽

X Ray Diffraction ◽

Complex Deformation ◽

X Ray ◽

Three Point Bending ◽

Atomic Force ◽

Au Nanowire ◽

Before And After

The three-point bending behavior of a single Au nanowire deformed by an atomic force microscope was monitored by coherent X-ray diffraction using a sub-micrometer sized hard X-ray beam. Three-dimensional reciprocal-space maps were recorded before and after deformation by standard rocking curves and were measured by scanning the energy of the incident X-ray beam during deformation at different loading stages. The mechanical behavior of the nanowire was visualized in reciprocal space and a complex deformation mechanism is described. In addition to the expected bending of the nanowire, torsion was detected. Bending and torsion angles were quantified from the high-resolution diffraction data.

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Three dimensional V2O5/NaV6O15 hierarchical heterostructures: Controlled synthesis and synergistic effect investigated by in situ X-ray diffraction

Nano Energy ◽

10.1016/j.nanoen.2016.06.057 ◽

2016 ◽

Vol 27 ◽

pp. 147-156 ◽

Cited By ~ 38

Author(s):

Chaojiang Niu ◽

Xiong Liu ◽

Jiashen Meng ◽

Lin Xu ◽

Mengyu Yan ◽

...

Keyword(s):

Synergistic Effect ◽

Three Dimensional ◽

Controlled Synthesis ◽

X Ray Diffraction ◽

X Ray

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X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

Acta Crystallographica Section A Foundations and Advances ◽

10.1107/s2053273314088615 ◽

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.

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