A commercial CCD detector for X-ray diffraction fully implemented on a third-generation synchrotron source

In the case of macromolecular crystallography, the measurement of diffracted intensities with monochromatic X-ray radiation is generally performed by the rotation method. A simulation program has been designed and tested by comparison with experimental data to investigate the various factors that are involved in the measurement and to improve collection strategies and tools, especially when using radiation from a third-generation synchrotron source. This program takes into account the main source and detector parameters in a realistic way, together with the possibility of selecting the sample characteristics. This then allows one both to evaluate the performances of existing experimental set-ups and to tailor the characteristics of new instruments,e.g.when designing a new detector or a new source.

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Texture of submicron Ni-Mn-Ga films studied by X-ray diffraction at the ANKA synchrotron source

Zeitschrift für Kristallographie ◽

10.1524/zkri.2007.2007.suppl_26.229 ◽

2007 ◽

Vol 2007 (suppl_26) ◽

pp. 229-234 ◽

Cited By ~ 1

Author(s):

V. A. Chernenko ◽

S. Doyle ◽

M. Kohl ◽

P. Müllner ◽

S. Besseghini ◽

...

Keyword(s):

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray

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Structure Refinements of the Layered Intergrowth Phases SbIIISbV x A 1−x TiO6 (x≃0, A = Ta, Nb) Using Synchrotron X-ray Powder Diffraction Data

Acta Crystallographica Section B Structural Science ◽

10.1107/s0108768197007787 ◽

1997 ◽

Vol 53 (6) ◽

pp. 861-869 ◽

Cited By ~ 2

Author(s):

C. D. Ling ◽

J. G. Thompson ◽

S. Schmid ◽

D. J. Cookson ◽

R. L. Withers

Keyword(s):

Single Crystal ◽

Powder Diffraction ◽

Diffraction Data ◽

Homologous Series ◽

Rietveld Method ◽

Powder Diffraction Data ◽

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray ◽

The Family

The structures of the layered intergrowth phases SbIIISb^{\rm V}_xAl-xTiO6 (x \simeq 0, A = Ta, Nb) have been refined by the Rietveld method, using X-ray diffraction data obtained using a synchrotron source. The starting models for these structures were derived from those of Sb^{\rm III}_3Sb^{\rm V}_xA 3−xTiO14 (x = 1.26, A = Ta and x = 0.89, A = Nb), previously solved by single-crystal X-ray diffraction. There were no significant differences between the derived models and the final structures, validating the approach used to obtain the models and confirming that the n = 1 and n = 3 members of the family, Sb^{\rm III}_nSb^{\rm V}_xA n−xTiO4n+2 are part of a structurally homologous series.

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In Situ Stress Tensor Determination during Phase Transformation of a Metal Matrix Composite by High-Energy X-ray Diffraction

Materials ◽

10.3390/ma11081415 ◽

2018 ◽

Vol 11 (8) ◽

pp. 1415 ◽

Cited By ~ 4

Author(s):

Guillaume Geandier ◽

Lilian Vautrot ◽

Benoît Denand ◽

Sabine Denis

Keyword(s):

Phase Transformation ◽

Stress Tensor ◽

Metal Matrix Composite ◽

Matrix Composite ◽

Metal Matrix ◽

High Energy ◽

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray

In situ high-energy X-ray diffraction using a synchrotron source performed on a steel metal matrix composite reinforced by TiC allows the evolutions of internal stresses during cooling to be followed thanks to the development of a new original experimental device (a transportable radiation furnace with controlled rotation of the specimen). Using the device on a high-energy beamline during in situ thermal treatment, we were able to extract the evolution of the stress tensor components in all phases: austenite, TiC, and even during the martensitic phase transformation of the matrix.

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In Situ X-Ray Diffraction of an Arc Weld Showing the Phase Transformations of Ti and Fe as a Function of Position in the Weld Performed at a Synchrotron

Advances in X-ray Analysis ◽

10.1154/s0376030800016013 ◽

1993 ◽

Vol 37 ◽

pp. 479-482 ◽

Cited By ~ 1

Author(s):

Joe Wong ◽

J. W. Elmer ◽

P. A. Waide ◽

E. M. Larson

Keyword(s):

Combustion Synthesis ◽

Ferroelectric Material ◽

Bragg Diffraction ◽

Intermediate Species ◽

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray ◽

Subsequent Phase ◽

Diffraction Peaks

The synchrotron x-ray source provides a unique opportunity to observe many “in-situ” processes. The formation of the “short-lived” intermediate species, Ta2C, during the combustion synthesis of TaC, has been observed and reported by monitoring the Bragg diffraction peaks of the reactants and products, Similarly, the synthesis of the ferroelectric material, BaTiO3, and subsequent phase transfonnation from cubic to tetragonal have also been investigated. These experiments would not have been possible without the high incident x-ray flux available at a synchrotron source.

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Experiences with CCD detectors on a home X-ray source

Acta Crystallographica Section D Biological Crystallography ◽

10.1107/s0907444999010689 ◽

1999 ◽

Vol 55 (10) ◽

pp. 1669-1671 ◽

Cited By ~ 4

Author(s):

Steven W. Muchmore

Keyword(s):

Small Molecule ◽

High Intensity ◽

Detection System ◽

Large Molecule ◽

Short Exposure ◽

X Ray Diffraction ◽

X Ray ◽

Image Plate ◽

Ccd Detector ◽

Ccd Detectors

Charged-coupled device (CCD) detectors have been widely accepted as detectors for collecting X-ray diffraction images. The CCD detector offers a sensitive detection system well suited for diffraction analysis and, compared with other detectors on the market, a relatively rapid system for read-out of the collected image. The two predominant markets for the CCD detector have been those in which relatively short exposure times are used,i.e.small-molecule X-ray diffraction and large-molecule crystallography at high-intensity synchrotron sources. CCD detectors have not been commonly used on rotating-anode X-ray sources for large-molecule crystallography. Comparison of the performance of the CCD detectors with commercially available image-plate detectors shows that the CCD detectors function in a similar fashion to image-plate-based detectors.

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X-ray laser–induced electron dynamics observed by femtosecond diffraction from nanocrystals of Buckminsterfullerene

Science Advances ◽

10.1126/sciadv.1601186 ◽

2016 ◽

Vol 2 (9) ◽

pp. e1601186 ◽

Cited By ~ 11

Author(s):

Brian Abbey ◽

Ruben A. Dilanian ◽

Connie Darmanin ◽

Rebecca A. Ryan ◽

Corey T. Putkunz ◽

...

Keyword(s):

Diffraction Pattern ◽

Molecular Targets ◽

Third Generation ◽

Free Electron Lasers ◽

Electron Dynamics ◽

Incident Power ◽

Synchrotron Source ◽

High Brightness ◽

X Ray ◽

The One

X-ray free-electron lasers (XFELs) deliver x-ray pulses with a coherent flux that is approximately eight orders of magnitude greater than that available from a modern third-generation synchrotron source. The power density of an XFEL pulse may be so high that it can modify the electronic properties of a sample on a femtosecond time scale. Exploration of the interaction of intense coherent x-ray pulses and matter is both of intrinsic scientific interest and of critical importance to the interpretation of experiments that probe the structures of materials using high-brightness femtosecond XFEL pulses. We report observations of the diffraction of extremely intense 32-fs nanofocused x-ray pulses by a powder sample of crystalline C60. We find that the diffraction pattern at the highest available incident power significantly differs from the one obtained using either third-generation synchrotron sources or XFEL sources operating at low output power and does not correspond to the diffraction pattern expected from any known phase of crystalline C60. We interpret these data as evidence of a long-range, coherent dynamic electronic distortion that is driven by the interaction of the periodic array of C60 molecular targets with intense x-ray pulses of femtosecond duration.

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A system for doing low temperature-high pressure single crystal X-ray diffraction with a synchrotron source

High Pressure Research ◽

10.1080/08957959208201046 ◽

1991 ◽

Vol 6 (6) ◽

pp. 379-388 ◽

Cited By ~ 14

Author(s):

R. LeToullec ◽

P. Loubeyre ◽

J. P. Pinceaux ◽

H. K. Mao ◽

J. Hu

Keyword(s):

High Pressure ◽

Low Temperature ◽

Single Crystal ◽

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray

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Changing the game of time resolved X-ray diffraction on the mechanochemistry playground by downsizing

Nature Communications ◽

10.1038/s41467-021-26264-1 ◽

2021 ◽

Vol 12 (1) ◽

Author(s):

Giulio I. Lampronti ◽

Adam A. L. Michalchuk ◽

Paolo P. Mazzeo ◽

Ana M. Belenguer ◽

Jeremy K. M. Sanders ◽

...

Keyword(s):

Diffraction Data ◽

Small Sample ◽

Model Systems ◽

Ex Situ ◽

X Ray Diffraction ◽

Time Resolved ◽

Synchrotron Source ◽

X Ray ◽

Microstructural Parameters ◽

Metal Organic

AbstractTime resolved in situ (TRIS) monitoring has revolutionised the study of mechanochemical transformations but has been limited by available data quality. Here we report how a combination of miniaturised grinding jars together with innovations in X-ray powder diffraction data collection and state-of-the-art analysis strategies transform the power of TRIS synchrotron mechanochemical experiments. Accurate phase compositions, comparable to those obtained by ex situ measurements, can be obtained with small sample loadings. Moreover, microstructural parameters (crystal size and microstrain) can be also determined with high confidence. This strategy applies to all chemistries, is readily implemented, and yields high-quality diffraction data even using a low energy synchrotron source. This offers a direct avenue towards the mechanochemical investigation of reactions comprising scarce, expensive, or toxic compounds. Our strategy is applied to model systems, including inorganic, metal-organic, and organic mechanosyntheses, resolves previously misinterpreted mechanisms in mechanochemical syntheses, and promises broad, new directions for mechanochemical research.

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Evaluation of grain-average stress tensor in a tensile-deformed Al–Mn polycrystal by high-energy X-ray diffraction

Journal of Applied Crystallography ◽

10.1107/s1600576717008238 ◽

2017 ◽

Vol 50 (4) ◽

pp. 1144-1157 ◽

Cited By ~ 3

Author(s):

Loïc Renversade ◽

András Borbély

Keyword(s):

Rotation Axis ◽

Three Dimensional ◽

Calibration Method ◽

High Energy ◽

Normal Strain ◽

X Ray Diffraction ◽

Synchrotron Source ◽

X Ray ◽

Strain Stress ◽

Individual Grains

Three-dimensional X-ray diffraction was applied to characterize the strain/stress evolution in individual grains of an Al–0.3 wt% Mn polycrystal deformedin situat a synchrotron source. Methodological aspects concerning the calibration of the geometrical setup and the evaluation of the strain/stress tensors are discussed. A two-step calibration method separately treating the detector and the rotation axis allows one to determine the centre-of-mass position and crystallographic orientation of grains with standard errors of about 1.5 µm and 0.02°, respectively. Numerical simulations indicate that the error of normal strain components (about 1 × 10−4) is mainly caused by calibration errors, while the error of shear components (about 0.5 × 10−4) is largely influenced by counting statistics and random spot-centre errors due to detector distortion. The importance of monitoring the beam energy is emphasized.

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