A method for in-situ measurements of the growth in the bulk of deformed single crystals at the 3DXRD microscope

2004 ◽  
Vol 819 ◽  
Author(s):  
S. Schmidt ◽  
D. Juul Jensen
Keyword(s):  
Spatial Information ◽  
Boundary Migration ◽  
Three Dimensional ◽  
European Synchrotron Radiation Facility ◽  
X Ray Diffraction ◽  
X Ray ◽  
Local Boundary ◽  
Migration Rates ◽  
Spatial Grain

AbstractWith the Three Dimensional X-ray Diffraction microscope (3DXRD) located at the European Synchrotron Radiation Facility (ESRF) full 3D spatial information of grains in the interior of a sample can be measured non-destructively. In this paper we discuss the possibility of an extension to this scenario, namely in-situ annealing studies, where the 3D spatial grain shape can be monitored as function of time. Consequently, local boundary migration rates can be estimated and compared to the deformed microstructure. Such information may reveal to what extend the deformed microstructure influences the growth of a grain during recrystallization.

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.

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

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.

The Application of In Situ 3D X-Ray Diffraction in Annealing Experiments: First Interpretation of Substructure Development in Deformed NaCl

2012 ◽  
Vol 715-716 ◽  
pp. 461-466 ◽  
Author(s):  
Verity Borthwick ◽  
Søren Schmidt ◽  
Sandra Piazolo ◽  
Carsten Gundlach ◽  
Albert Griera ◽  
...  
Keyword(s):  
Subgrain Boundary ◽  
Surface Effects ◽  
Sample Volume ◽  
European Synchrotron Radiation Facility ◽  
X Ray Diffraction ◽  
Boundary Misorientation ◽  
X Ray ◽  
Before And After ◽  
Annealing Experiments

n-situ 3D X-ray diffraction (3DXRD) annealing experiments were conducted at the ID-11 beamline at the European Synchrotron Radiation Facility in Grenoble. This allowed us to non-destructively document and subsequently analyse the development of substructures during heating, without the influence of surface effects. A sample of deformed single crystal halite was heated to between 260-400 °C. Before and after heating a volume of 500 by 500 by 300 μm was mapped using a planar beam, which was translated over the sample volume at intervals of 5-10 µm in the vertical dimension. In the following we present partially reconstructed orientation maps over one layer before and after heating for 240min at 260 °C. Additional small syn-heating maps over a constrained sample rotation of 12-30º. The purpose of this was to illuminate a few reflections from 1 or 2 subgrains and follow their evolution during heating. Preliminary results show that significant changes occurred within the sample volume, for which, surface effects can be excluded. Results show a number of processes, including: i) change in subgrain boundary misorientation angle and ii) subgrain subdivision into areas of similar lattice orientation with new subgrain boundary formation. These results demonstrate that 3DXRD coupled with in-situ heating is a successful non-destructive technique for examining real-time post-deformational annealing in strongly deformed crystalline materials with complicated microstructures.

Orientations of Recrystallization Nuclei Studied by 3DXRD

2005 ◽  
Vol 495-497 ◽  
pp. 1285-1290 ◽  
Author(s):  
Dorte Juul Jensen ◽  
A.W. Larsen
Keyword(s):  
Critical Point ◽  
Boundary Migration ◽  
X Ray Diffraction ◽  
X Ray ◽  
Deformation Microstructure ◽  
3 Dimensional ◽  
Nucleation Mechanisms ◽  
Crystallographic Orientations

A critical point in the understanding of recrystallization textures is the development of crystallographic orientations of the nuclei. Here an issue, which has been debated much recently [eg. 1], is if nuclei have orientations identical to those of the deformation microstructures from which they originate or not. Traditional nucleation mechanisms like strain induced boundary migration [2] and particle stimulated nucleation [3] operate with nuclei orientations identical to the “parent”deformation microstructure. This is also what is commonly incorporated in recrystallization modeling. However, a number of studies have found recrystallization nuclei in orientations that were not expected from measurements on deformed structures. Some of these results are reviewed and discussed in this paper, and new in-situ results obtained by the 3 dimensional X-ray diffraction (3DXR) method are presented.

scholarly journals Determination of Residual Stresses in an Oxidized Metallic Alloy under Thermal Loadings

Metals ◽  
2018 ◽  
Vol 8 (11) ◽  
pp. 913
Author(s):  
Zhimao Wang ◽  
Jean-Luc Grosseau-Poussard ◽  
Benoît Panicaud ◽  
Guillaume Geandier ◽  
Pierre-Olivier Renault ◽  
...  
Keyword(s):  
Residual Stresses ◽  
Correction Method ◽  
Lattice Parameter ◽  
European Synchrotron Radiation Facility ◽  
X Ray Diffraction ◽  
Synchrotron Diffraction ◽  
X Ray ◽  
Crystallographic Planes

In order to clarify the mechanical features of a metal under thermal cyclic loading for the system Ni30Cr-Cr2O3, a specific study has been carried out. In the present work, the residual stresses in both the metal and the oxide layer have been investigated. An adapted method is applied to process the experimental results that were obtained by using in-situ high temperature synchrotron diffraction at European Synchrotron Radiation Facility. The sin2ψ analysis provides information about the stress in metal and oxide. X-ray diffraction provides also the lattice parameter between crystallographic planes in the metal. To obtain correct stress values, a correction method is also proposed taking into account different discrepancies sources to ensure the equation of mechanical balance.

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.

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