Hard X-ray diffraction scanning tomography with sub-micrometre spatial resolution: application to an annealed γ-U0.85Mo0.15particle

2011 ◽  
Vol 44 (5) ◽  
pp. 1111-1119 ◽  
Author(s):  
Hervé Palancher ◽  
Rémi Tucoulou ◽  
Pierre Bleuet ◽  
Anne Bonnin ◽  
Eléonore Welcomme ◽  
...  
Keyword(s):  
Spatial Resolution ◽  
Structural Information ◽  
Three Dimensional ◽  
Real Space ◽  
Protective Role ◽  
Diffraction Tomography ◽  
X Ray Diffraction ◽  
X Ray ◽  
Thermally Activated

It is demonstrated that scanning X-ray diffraction tomography of heterogeneous and polycrystalline samples can provide real-space semi-quantitative three-dimensional structural information at a submicrometre spatial resolution. The capabilities of this technique are illustrated by the study of a slice of a spherical particle consisting of a UMo core (about 37 µm in diameter) surrounded by a UMoAl shell (5 µm thick). The technique allows precise characterization of the embedded UMo/UMoAl interface where the phases α-U (in the core), UAl2and U6Mo4Al43(in the shell) are found. Moreover, an unexpected phase (UC) is detected at a trace level. It is shown that the thickness of the UMoAl shell is locally anticorrelated with the amount of UC, suggesting that this phase plays a protective role in inhibiting thermally activated Al diffusion in UMo.

2D real space visualization of d values in polycrystalline bulk materials of different hardness

2021 ◽  
Vol 54 (2) ◽  
pp. 597-603
Author(s):  
Mari Mizusawa ◽  
Kenji Sakurai
Keyword(s):  
Lattice Distortion ◽  
Structural Information ◽  
Hardness Test ◽  
Real Space ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diffraction Imaging ◽  
D Values

Conventional X-ray diffraction measurements provide some average structural information, mainly on the crystal structure of the whole area of the given specimen, which might not be very uniform and may include different crystal structures, such as co-existing crystal phases and/or lattice distortion. The way in which the lattice plane changes due to strain also might depend on the position in the sample, and the average information might have some limits. Therefore, it is important to analyse the sample with good lateral spatial resolution in real space. Although various techniques for diffraction topography have been developed for single crystals, it has not always been easy to image polycrystalline materials. Since the late 1990s, imaging technology for fluorescent X-rays and X-ray absorption fine structure has been developed via a method that does not scan either a sample or an X-ray beam. X-ray diffraction imaging can be performed when this technique is applied to a synchrotron radiation beamline with a variable wavelength. The present paper reports the application of X-ray diffraction imaging to bulk steel materials with varying hardness. In this study, the distribution of lattice distortion of hardness test blocks with different hardness was examined. Via this 2D visualization method, the grains of the crystals with low hardness are large enough to be observed by X-ray diffraction contrast in real space. The change of the d value in the vicinity of the Vickers mark has also been quantitatively evaluated.

scholarly journals PolyProc: A Modular Processing Pipeline for X-ray Diffraction Tomography

2019 ◽  
Vol 8 (3) ◽  
pp. 388-399 ◽  
Author(s):  
Jiwoong Kang ◽  
Ning Lu ◽  
Issac Loo ◽  
Nancy Senabulya ◽  
Ashwin J. Shahani
Keyword(s):  
Three Dimensional ◽  
Valuable Insight ◽  
Diffraction Tomography ◽  
Computationally Efficient ◽  
X Ray Diffraction ◽  
Orientation Data ◽  
Bulk Specimen ◽  
X Ray ◽  
Data Alignment ◽  
And Performance

Abstract Direct imaging of three-dimensional microstructure via X-ray diffraction-based techniques gives valuable insight into the crystallographic features that influence materials properties and performance. For instance, X-ray diffraction tomography provides information on grain orientation, position, size, and shape in a bulk specimen. As such techniques become more accessible to researchers, demands are placed on processing the datasets that are inherently “noisy,” multi-dimensional, and multimodal. To fulfill this need, we have developed a one-of-a-kind function package, PolyProc, that is compatible with a range of data shapes, from planar sections to time-evolving and three-dimensional orientation data. Our package comprises functions to import, filter, analyze, and visualize the reconstructed grain maps. To accelerate the computations in our pipeline, we harness computationally efficient approaches: for instance, data alignment is done via genetic optimization; grain tracking through the Hungarian method; and feature-to-feature correlation through k-nearest neighbors algorithm. As a proof-of-concept, we test our approach in characterizing the grain texture, topology, and evolution in a polycrystalline Al–Cu alloy undergoing coarsening.

scholarly journals Crystallization and preliminary X-ray diffraction analysis of a single variable domain of the immunoglobulin superfamily in amphioxus,Amphi-IgSF-V

2014 ◽  
Vol 70 (8) ◽  
pp. 1072-1075 ◽  
Author(s):  
Bo Jiang ◽  
Yanjie Liu ◽  
Rong Chen ◽  
Zhenbao Wang ◽  
Mansoor Tariq ◽  
...  
Keyword(s):  
Immune System ◽  
Structural Information ◽  
Three Dimensional ◽  
Dimensional Structure ◽  
Immunoglobulin Superfamily ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
System A ◽  
Human Immunoglobulins

Amphioxus is regarded as an essential animal model for the study of immune evolution. Discovery of new molecules with the immunoglobulin superfamily (IgSF) variable (V) domain in amphioxus would help in studying the evolution of IgSF V molecules in the immune system. A protein was found which just contains only one IgSF V domain in amphioxus, termedAmphi-IgSF-V; it has over 30% sequence identity to the V domains of human immunoglobulins and mammalian T-cell receptors. In order to clarify the three-dimensional structure of this new molecule in amphioxus,Amphi-IgSF-V was expressed, purified and crystallized, and diffraction data were collected to a resolution of 1.95 Å. The crystal belonged to space groupP3221, with unit-cell parametersa=b= 53.9,c= 135.5 Å. The Matthews coefficient and solvent content were calculated to be 2.58 Å3 Da−1and 52.38%, respectively. The results will provide structural information to study the evolution of IgSF V molecules in the immune system.

High Resolution Synchrotron X-Ray Diffraction Tomography Of Large-Grained Samples

1996 ◽  
Vol 437 ◽  
Author(s):  
D.P. Piotrowski ◽  
S.R. Stock ◽  
A. Guvenilir ◽  
J.D. Haase ◽  
Z.U. Rek
Keyword(s):  
Spatial Distribution ◽  
High Resolution ◽  
Three Dimensional ◽  
Polycrystalline Materials ◽  
Diffraction Tomography ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
Image Storage ◽  
X Ray ◽  
Dimensional Distribution

AbstractIn order to understand the macroscopic response of polycrystalline structural materials to loading, it is frequently essential to know the spatial distribution of strain as well as the variation of micro-texture on the scale of 100 μm. The methods must be nondestructive, however, if the three-dimensional evolution of strain is to be studied. This paper describes an approach to high resolution synchrotron x-ray diffraction tomography of polycrystalline materials. Results from model samples of randomly-packed, millimeter-sized pieces of Si wafers and of similarly sized single-crystal Al blocks have been obtained which indicate that polychromatic beams collimated to 30 μm diameter can be used to determine the depth of diffracting volume elements within ± 70 μm. The variation in the two-dimensional distribution of diffracted intensity with changing sample to detector separation is recorded on image storage plates and used to infer the depth of diffracting volume elements.

scholarly journals Maximum a posteriori estimation of crystallographic phases in X-ray diffraction tomography

2015 ◽  
Vol 373 (2043) ◽  
pp. 20140392 ◽  
Author(s):  
Doĝa Gürsoy ◽  
Tekin Biçer ◽  
Jonathan D. Almer ◽  
Raj Kettimuthu ◽  
Stuart R. Stock ◽  
...  
Keyword(s):  
National Laboratory ◽  
Spinous Process ◽  
Argonne National Laboratory ◽  
Three Dimensional ◽  
Polycrystalline Materials ◽  
Reconstruction Method ◽  
Diffraction Tomography ◽  
A Posteriori ◽  
X Ray Diffraction ◽  
X Ray

A maximum a posteriori approach is proposed for X-ray diffraction tomography for reconstructing three-dimensional spatial distribution of crystallographic phases and orientations of polycrystalline materials. The approach maximizes the a posteriori density which includes a Poisson log-likelihood and an a priori term that reinforces expected solution properties such as smoothness or local continuity. The reconstruction method is validated with experimental data acquired from a section of the spinous process of a porcine vertebra collected at the 1-ID-C beamline of the Advanced Photon Source, at Argonne National Laboratory. The reconstruction results show significant improvement in the reduction of aliasing and streaking artefacts, and improved robustness to noise and undersampling compared to conventional analytical inversion approaches. The approach has the potential to reduce data acquisition times, and significantly improve beamtime efficiency.

High Resolution Synchrotron X-Ray Diffraction Tomography of Polycrystalline Samples

1994 ◽  
Vol 375 ◽  
Author(s):  
S. R. Stock ◽  
A. Guvenilir ◽  
D. P. Piotrowski ◽  
Z. U. Rek
Keyword(s):  
Spatial Distribution ◽  
High Resolution ◽  
Three Dimensional ◽  
Compact Tension ◽  
Polycrystalline Materials ◽  
Diffraction Tomography ◽  
X Ray Diffraction ◽  
Image Storage ◽  
X Ray ◽  
Nondestructive Measurements

AbstractThe macroscopic response of polycrystalline materials to loading depends on both the spatial distribution of strain and the variation of microtexture on the scale of 100 μm. Nondestructive measurements are needed if the three-dimensional evolution of strain is to be studied. This paper describes approaches for high resolution synchrotron polychromatic x-ray diffraction tomography of polycrystalline materials. Preliminary experiments are reported on partially cracked compact tension samples of Al-Li 2090 and on model samples of randomly-packed, millimeter-sized pieces of Si wafers. Polychromatic beams collimated to 100 μm diameter have been used, and the distribution of diffracted intensity has been collected on high resolution x-ray film as well as on image storage plates. The depths of diffracting volume elements are determined from the changes in the spatial distribution of diffracted intensity with varying sample to detector separation.

Structural characterization of self-assembled semiconductor islands by three-dimensional X-ray diffraction mapping in reciprocal space

2008 ◽  
Vol 516 (22) ◽  
pp. 8022-8028 ◽  
Author(s):  
V. Holý ◽  
K. Mundboth ◽  
C. Mokuta ◽  
T.H. Metzger ◽  
J. Stangl ◽  
...  
Keyword(s):  
Structural Characterization ◽  
Three Dimensional ◽  
Reciprocal Space ◽  
X Ray Diffraction ◽  
X Ray ◽  
Self Assembled

Hydroxyapatite/Biopolymers Composite Scaffolds for Bone Tissue Engineering

2011 ◽  
Vol 493-494 ◽  
pp. 826-831
Author(s):  
A.C.B.M. Fook ◽  
Thiago Bizerra Fideles ◽  
R.C. Barbosa ◽  
G.T.F.S. Furtado ◽  
G.Y.H. Sampaio ◽  
...  
Keyword(s):  
Tissue Engineering ◽  
Bone Tissue Engineering ◽  
Bone Tissue ◽  
Freeze Drying ◽  
Three Dimensional ◽  
Porous Scaffolds ◽  
X Ray Diffraction ◽  
X Ray ◽  
Interconnected Pores

The application of a hybrid composite consisting of biopolymer and calcium phosphate, similar morphology and properties of natural bone, may be a way to solve the problem of the fragility of ceramics without reducing its mechanical properties, retaining the properties of biocompatibility and high bioactivity. This work aims at the preparation and characterization of three-dimensional scaffolds composite HA / biopolymers (chitosan and gelatin). The freeze-drying technique was employed in this study to obtain these frameworks and partial results showed the effectiveness of this method. This involved the study of structural, chemical and morphological frameworks, in order to direct the research suggested the application. The X Ray Diffraction (XRD) and infrared spectroscopy and Fourier transform (FTIR) results confirmed the formation of hydroxyapatite (HA) phase and the presence of characteristic bands of HA and biopolymers in all compositions. The microstructure of the scaffolds study conducted by Scanning Electron Microscopy (SEM) revealed the formation of longitudinally oriented microchannels with interconnected pores. In all compositions the porous scaffolds showed varying sizes and mostly larger than 100μm, and is therefore considered materials with potential for application in bone tissue engineering.

scholarly journals Structure of Carbon Materials Explored by Local Transmission Electron Microscopy and Global Powder Diffraction Probes

2018 ◽  
Vol 4 (4) ◽  
pp. 68 ◽  
Author(s):  
Karolina Jurkiewicz ◽  
Mirosława Pawlyta ◽  
Andrzej Burian
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Neutron Diffraction ◽  
Carbon Materials ◽  
Structural Information ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Local Transmission

Transmission electron microscopy and neutron or X-ray diffraction are powerful techniques available today for characterization of the structure of various carbon materials at nano and atomic levels. They provide complementary information but each one has advantages and limitations. Powder X-ray or neutron diffraction measurements provide structural information representative for the whole volume of a material under probe but features of singular nano-objects cannot be identified. Transmission electron microscopy, in turn, is able to probe single nanoscale objects. In this review, it is demonstrated how transmission electron microscopy and powder X-ray and neutron diffraction methods complement each other by providing consistent structural models for different types of carbons such as carbon blacks, glass-like carbons, graphene, nanotubes, nanodiamonds, and nanoonions.

Synthesis and Characterization of a Three-dimensional Porous Compound: [Cu(H2O)6][{Cu(H2O)2}2{Cu(H2O)4H4W12O42}] · 12H2O

2008 ◽  
Vol 63 (2) ◽  
pp. 187-192 ◽  
Author(s):  
Chun-jing Zhang ◽  
Ya-guang Chen ◽  
Dong-mei Shi ◽  
Hai-jun Pang
Keyword(s):  
Aqueous Solution ◽  
Magnetic Susceptibility ◽  
Elemental Analysis ◽  
3D Structure ◽  
Three Dimensional ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Vis Spectroscopy

A novel transition metal polyoxotungstate, [Cu(H2O)6][{Cu(H2O)2}2{Cu(H2O)4H4W12O42}] · 12H2O (1), has been synthesized in aqueous solution and characterized by single-crystal X-ray diffraction, elemental analysis, IR and UV/vis spectroscopy, and TG analysis. The paradodecatungstate anions [H2W12O42]10− are linked by CuO6 octahedra, forming a three-dimensional (3D) structure. The magnetic susceptibility of compound 1 in the temperature range 2 - 300 K shows the presence of antiferromagnetic interactions within the uniform Cu2・ ・ ・Cu3 chains

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