Observation of non-basal slip in Mg-Y by in situ three-dimensional X-ray diffraction

2018 ◽  
Vol 143 ◽  
pp. 44-48 ◽  
Author(s):  
Zhonghe Huang ◽  
Leyun Wang ◽  
Bijin Zhou ◽  
Torben Fischer ◽  
Sangbong Yi ◽  
...  
Keyword(s):  
Basal Slip ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray

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

2018 ◽  
Vol 2 (4) ◽  
pp. 24 ◽  
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.

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

Nano Energy ◽  
2016 ◽  
Vol 27 ◽  
pp. 147-156 ◽  
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

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.

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

2014 ◽  
Vol 777 ◽  
pp. 118-123 ◽  
Author(s):  
Yujiro Hayashi ◽  
Yoshiharu Hirose ◽  
Daigo Setoyama
Keyword(s):  
Three Dimensional ◽  
Diffraction Method ◽  
Inverse Pole Figure ◽  
Coarse Grained ◽  
Uniaxial Tensile ◽  
X Ray Diffraction ◽  
Polycrystalline Iron ◽  
X Ray ◽  
Orientation Mapping

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.

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.

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

1998 ◽  
Vol 547 ◽  
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.

scholarly journals Formation and annihilation of stressed deformation twins in magnesium

2021 ◽  
Vol 2 (1) ◽  
Author(s):  
Karim Louca ◽  
Hamidreza Abdolvand ◽  
Charles Mareau ◽  
Marta Majkut ◽  
Jonathan Wright
Keyword(s):  
Mechanical Response ◽  
Axial Stress ◽  
Three Dimensional ◽  
Service Performance ◽  
Polycrystalline Materials ◽  
X Ray Diffraction ◽  
Sign Reversal ◽  
X Ray ◽  
Hexagonal Close Packed

AbstractThe mechanical response of polycrystalline materials to an externally applied load and their in-service performance depend on the local load partitioning among the constituent crystals. In hexagonal close-packed polycrystals such load partitioning is significantly affected by deformation twinning. Here we report in-situ compression-tension experiments conducted on magnesium specimens to measure the evolution of grain resolved tensorial stresses and formation and annihilation of twins. More than 13000 grains and 1300 twin-parent pairs are studied individually using three-dimensional synchrotron X-ray diffraction. It is shown that at the early stages of plasticity, the axial stress in twins is higher than that of parents, yet twins relax with further loading. While a sign reversal is observed for the resolved shear stress (RSS) acting on the twin habit plane in the parent, the sign of RSS within the majority of twins stays unchanged until twin annihilation during the load reversal. The variations of measured average stresses across parents and twins are also investigated.

A new ZnII coordination polymer based on 4-(pyridin-4-yl)benzoic and formic acids: in-situ synthesis, crystal structure and luminescence properties

2018 ◽  
Vol 74 (10) ◽  
pp. 1133-1137 ◽  
Author(s):  
Fuming Luo ◽  
Guodong Tang ◽  
Jinfang Zhang
Keyword(s):  
Three Dimensional ◽  
Luminescence Properties ◽  
Supramolecular Framework ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Structural Units ◽  
X Ray ◽  
Layer Structures ◽  
State Luminescence

The title compound, poly[(μ2-formato-κ3 O,O′:O)[μ2-4-(pyridin-4-yl)benzoato-κ3 N:O,O′]zinc(II)], [Zn(C12H8NO2)(HCOO)] n , has been synthesized in situ and characterized by thermogravimetric analysis (TGA) and single-crystal and powder X-ray diffraction analyses. The polymer contains two independent structural units in the asymmetric unit. These are constructed from Zn2+ ions, 4-(pyridin-4-yl)benzoate (4-pbc) bridges and in-situ-generated formate ligands, forming two similar two-dimensional (2D) layer structures. These similar 2D layers are arranged alternately and are linked with each other by dense C—H...O hydrogen bonds to generate a three-dimensional (3D) supramolecular framework. The crystal is pseudomerohedrally twinned about [201]. Compared with free 4-Hpbc, the polymer exhibits a red shift and significantly enhanced solid-state luminescence properties.

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