Selective imaging of nano-particle contrast agents by a single-shot x-ray diffraction technique

This article describes a single-shot methodology to derive an average coating thickness in multi-particle core–shell systems exhibiting high X-ray absorption. Powder composed of U–Mo alloy particles surrounded by a micrometre-thick UO2protective layer has been used as a test sample. Combining high-energy X-ray diffraction and laser granulometry, the average shell thickness could be accurately characterized. These results have been validated by additional measurements on single particles by two techniques: X-ray nanotomography and high-energy X-ray diffraction. The presented single-shot approach gives rise to many potential applications on core–shell systems and in particular on as-fabricated heterogeneous nuclear fuels.

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Single-shot structural analysis by high-energy X-ray diffraction using an ultrashort all-optical source

Scientific Reports ◽

10.1038/s41598-017-16477-0 ◽

2017 ◽

Vol 7 (1) ◽

Cited By ~ 2

Author(s):

R. Rakowski ◽

G. Golovin ◽

J. O’Neal ◽

J. Zhang ◽

P. Zhang ◽

...

Keyword(s):

Structural Analysis ◽

High Energy ◽

Single Shot ◽

X Ray Diffraction ◽

Optical Source ◽

X Ray ◽

All Optical

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Coherent convergent-beam time-resolved X-ray diffraction

Philosophical Transactions of the Royal Society B Biological Sciences ◽

10.1098/rstb.2013.0325 ◽

2014 ◽

Vol 369 (1647) ◽

pp. 20130325 ◽

Cited By ~ 12

Author(s):

John C. H. Spence ◽

Nadia A. Zatsepin ◽

Chufeng Li

Keyword(s):

Single Shot ◽

Beam Diameter ◽

X Ray Diffraction ◽

Single Particles ◽

Time Resolved ◽

X Ray ◽

Challenges And Opportunities ◽

Phase Sensitive ◽

Diffraction Patterns ◽

Convergent Beam

The use of coherent X-ray lasers for structural biology allows the use of nanometre diameter X-ray beams with large beam divergence. Their application to the structure analysis of protein nanocrystals and single particles raises new challenges and opportunities. We discuss the form of these coherent convergent-beam (CCB) hard X-ray diffraction patterns and their potential use for time-resolved crystallography, normally achieved by Laue (polychromatic) diffraction, for which the monochromatic laser radiation of a free-electron X-ray laser is unsuitable. We discuss the possibility of obtaining single-shot, angle-integrated rocking curves from CCB patterns, and the dependence of the resulting patterns on the focused beam coordinate when the beam diameter is larger or smaller than a nanocrystal, or smaller than one unit cell. We show how structure factor phase information is provided at overlapping interfering orders and how a common phase origin between different shots may be obtained. Their use in refinement of the phase-sensitive intensity between overlapping orders is suggested.

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The Effect of Thickness on the Physical Properties of Fe2O3 Thin Films Prepared by DC Magnetron Sputtering

Al-Mustansiriyah Journal of Science ◽

10.23851/mjs.v28i1.325 ◽

2017 ◽

Vol 28 (1) ◽

pp. 149

Author(s):

Baha'a A. Al-Hilli

Keyword(s):

Film Thickness ◽

Physical Properties ◽

Room Temperature ◽

Optical Constants ◽

Energy Gap ◽

Nano Particle ◽

X Ray Diffraction ◽

Thin Film Thickness ◽

X Ray ◽

Deposition Parameters

The objective of this study is to assess the influence of nano-particle Fe2O3 thin film thickness on some physical properties which were prepared by magnetron DC- sputtering on glass substrate at room temperature. The structure was tested with X-Ray diffraction and it was to be amorphous and to become single crystal with recognized peak in (003) after annealing at temperature 500oC. The physical properties as a function of deposition parameters and then film thickness were studied. The optical properties such as absorbance, energy gap and some optical constants are measured and found that of about (3eV) energy gap.

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Data processing software suiteSITENNOfor coherent X-ray diffraction imaging using the X-ray free-electron laser SACLA

Journal of Synchrotron Radiation ◽

10.1107/s1600577514003439 ◽

2014 ◽

Vol 21 (3) ◽

pp. 600-612 ◽

Cited By ~ 25

Author(s):

Yuki Sekiguchi ◽

Tomotaka Oroguchi ◽

Yuki Takayama ◽

Masayoshi Nakasako

Keyword(s):

Data Processing ◽

Free Electron ◽

Free Electron Laser ◽

Single Shot ◽

X Ray Diffraction ◽

X Ray ◽

Custom Made ◽

Diffraction Imaging ◽

Diffraction Patterns ◽

Ccd Detectors

Coherent X-ray diffraction imaging is a promising technique for visualizing the structures of non-crystalline particles with dimensions of micrometers to sub-micrometers. Recently, X-ray free-electron laser sources have enabled efficient experiments in the `diffraction before destruction' scheme. Diffraction experiments have been conducted at SPring-8 Angstrom Compact free-electron LAser (SACLA) using the custom-made diffraction apparatus KOTOBUKI-1 and two multiport CCD detectors. In the experiments, ten thousands of single-shot diffraction patterns can be collected within several hours. Then, diffraction patterns with significant levels of intensity suitable for structural analysis must be found, direct-beam positions in diffraction patterns determined, diffraction patterns from the two CCD detectors merged, and phase-retrieval calculations for structural analyses performed. A software suite namedSITENNOhas been developed to semi-automatically apply the four-step processing to a huge number of diffraction data. Here, details of the algorithm used in the suite are described and the performance for approximately 9000 diffraction patterns collected from cuboid-shaped copper oxide particles reported. Using theSITENNOsuite, it is possible to conduct experiments with data processing immediately after the data collection, and to characterize the size distribution and internal structures of the non-crystalline particles.

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Recrystallization Investigated by X- Ray Diffraction Imaging

Materials Science Forum ◽

10.4028/www.scientific.net/msf.550.631 ◽

2007 ◽

Vol 550 ◽

pp. 631-636 ◽

Cited By ~ 2

Author(s):

Thomas Wroblewski ◽

Adeline Buffet

Keyword(s):

Nucleation And Growth ◽

Single Shot ◽

X Ray Diffraction ◽

Growth Behaviour ◽

Large Area ◽

Polycrystalline Specimen ◽

X Ray ◽

Classical Models ◽

Diffraction Imaging ◽

Cold Rolled

X-ray diffraction imaging allows the investigation of a large area of a polycrystalline specimen in a single shot. Dynamic processes like recystallization can, therefore, be studied without prior knowledge of where they occur. Even early stages of nucleation can be traced back using the information from images taken from the fully recrystallized specimen. Experiments performed at HASYLAB beamline G3 on cold rolled Cu and Al showed nucleation and growth behaviour that cannot be explained by classical models.

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Improved crystal orientation and physical properties from single-shot XFEL stills

Acta Crystallographica Section D Biological Crystallography ◽

10.1107/s1399004714024134 ◽

2014 ◽

Vol 70 (12) ◽

pp. 3299-3309 ◽

Cited By ~ 32

Author(s):

Nicholas K. Sauter ◽

Johan Hattne ◽

Aaron S. Brewster ◽

Nathaniel Echols ◽

Petrus H. Zwart ◽

...

Keyword(s):

Crystal Orientation ◽

Degrees Of Freedom ◽

Reciprocal Lattice ◽

Single Shot ◽

X Ray Diffraction ◽

Reciprocal Lattice Point ◽

X Ray ◽

Structure Factors ◽

Rotational Degrees Of Freedom ◽

Diffraction Patterns

X-ray diffraction patterns from still crystals are inherently difficult to process because the crystal orientation is not uniquely determined by measuring the Bragg spot positions. Only one of the three rotational degrees of freedom is directly coupled to spot positions; the other two rotations move Bragg spots in and out of the reflecting condition but do not change the direction of the diffracted rays. This hinders the ability to recover accurate structure factors from experiments that are dependent on single-shot exposures, such as femtosecond diffract-and-destroy protocols at X-ray free-electron lasers (XFELs). Here, additional methods are introduced to optimally model the diffraction. The best orientation is obtained by requiring, for the brightest observed spots, that each reciprocal-lattice point be placed into the exact reflecting condition implied by Bragg's law with a minimal rotation. This approach reduces the experimental uncertainties in noisy XFEL data, improving the crystallographicRfactors and sharpening anomalous differences that are near the level of the noise.

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Single-shot full strain tensor determination with microbeam X-ray Laue diffraction and a two-dimensional energy-dispersive detector

Journal of Applied Crystallography ◽

10.1107/s1600576717005581 ◽

2017 ◽

Vol 50 (3) ◽

pp. 901-908 ◽

Cited By ~ 9

Author(s):

A. Abboud ◽

C. Kirchlechner ◽

J. Keckes ◽

T. Conka Nurdan ◽

S. Send ◽

...

Keyword(s):

Elastic Strain ◽

Strain Tensor ◽

Energy Dispersive ◽

Single Shot ◽

Two Dimensional ◽

X Ray Diffraction ◽

Laue Diffraction ◽

Experimental Procedure ◽

X Ray ◽

Diffraction Patterns

The full strain and stress tensor determination in a triaxially stressed single crystal using X-ray diffraction requires a series of lattice spacing measurements at different crystal orientations. This can be achieved using a tunable X-ray source. This article reports on a novel experimental procedure for single-shot full strain tensor determination using polychromatic synchrotron radiation with an energy range from 5 to 23 keV. Microbeam X-ray Laue diffraction patterns were collected from a copper micro-bending beam along the central axis (centroid of the cross section). Taking advantage of a two-dimensional energy-dispersive X-ray detector (pnCCD), the position and energy of the collected Laue spots were measured for multiple positions on the sample, allowing the measurement of variations in the local microstructure. At the same time, both the deviatoric and hydrostatic components of the elastic strain and stress tensors were calculated.

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Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays

IUCrJ ◽

10.1107/s205225252000144x ◽

2020 ◽

Vol 7 (2) ◽

pp. 276-286 ◽

Cited By ~ 1

Author(s):

Akinobu Niozu ◽

Yoshiaki Kumagai ◽

Toshiyuki Nishiyama ◽

Hironobu Fukuzawa ◽

Koji Motomura ◽

...

Keyword(s):

Free Electron ◽

Structural Information ◽

Single Shot ◽

X Ray Diffraction ◽

X Ray ◽

Angular Correlations ◽

Crystalline Defects ◽

X Ray Scattering ◽

Diffraction Patterns ◽

Ray Scattering

Characterizing and controlling the uniformity of nanoparticles is crucial for their application in science and technology because crystalline defects in the nanoparticles strongly affect their unique properties. Recently, ultra-short and ultra-bright X-ray pulses provided by X-ray free-electron lasers (XFELs) opened up the possibility of structure determination of nanometre-scale matter with Å spatial resolution. However, it is often difficult to reconstruct the 3D structural information from single-shot X-ray diffraction patterns owing to the random orientation of the particles. This report proposes an analysis approach for characterizing defects in nanoparticles using wide-angle X-ray scattering (WAXS) data from free-flying single nanoparticles. The analysis method is based on the concept of correlated X-ray scattering, in which correlations of scattered X-ray are used to recover detailed structural information. WAXS experiments of xenon nanoparticles, or clusters, were conducted at an XFEL facility in Japan by using the SPring-8 Ångstrom compact free-electron laser (SACLA). Bragg spots in the recorded single-shot X-ray diffraction patterns showed clear angular correlations, which offered significant structural information on the nanoparticles. The experimental angular correlations were reproduced by numerical simulation in which kinematical theory of diffraction was combined with geometric calculations. We also explain the diffuse scattering intensity as being due to the stacking faults in the xenon clusters.

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