scholarly journals Laue diffraction and time-resolved crystallography: a personal history

2019 ◽  
Vol 377 (2147) ◽  
pp. 20180243 ◽  
Author(s):  
Keith Moffat
Keyword(s):  
Storage Ring ◽  
Structural Changes ◽  
X Ray Diffraction ◽  
Laue Diffraction ◽  
Time Resolved ◽  
Pump Probe ◽  
X Ray ◽  
Historical View ◽  
Laser Sources ◽  
Diffraction Patterns

A personal, historical view is presented of Laue X-ray diffraction and its application to time-resolved studies of dynamic processes, largely in light-sensitive biological systems. In Laue diffraction, a stationary crystal is illuminated by a polychromatic X-ray source. Laue diffraction has inherent complications largely absent in monochromatic diffraction, and consequently fell into disuse for quantitative structure determination. However, the advent of naturally polychromatic, intense, pulsed storage ring X-ray sources in the 1970s led to re-examination at Daresbury and elsewhere of its underlying principles. Laue diffraction has been successfully applied at storage ring sources to time-resolved, pump–probe crystallographic studies, whose exposure time and time resolution were progressively reduced from minutes to seconds, milliseconds, nanoseconds and 100 ps. Most recently, hard X-ray free electron laser sources have been used to generate narrow bandpass Laue diffraction patterns. The femtosecond X-ray pulses from such sources are completely destructive, generate only one diffraction pattern per tiny crystal and have unusual properties. However, they too are being applied to time-resolved crystallography to explore, for example, isomerization and rapid tertiary structural changes on the chemical, femtosecond timescale. This article is part of the theme issue ‘Fifty years of synchrotron science: achievements and opportunities’.

First-, second- and third-order correlation function in time-resolved X-ray diffraction experiments

2004 ◽  
Vol 37 (3) ◽  
pp. 445-450 ◽  
Author(s):  
Simone Techert
Keyword(s):  
Structural Changes ◽  
X Rays ◽  
X Ray Diffraction ◽  
Structural Reorganization ◽  
Third Order ◽  
Time Resolved ◽  
Pump Probe ◽  
X Ray ◽  
Laser Systems ◽  
Laser Sources

In the past decade, sustained progress has been made in the field of time-resolved X-ray diffraction and photocrystallography. Laser systems have been developed rapidly, and the combination of pulsed laser sources with pulsed X-ray sources, particularly by using synchrotron X-ray radiation and X-rays generated by plasma sources, has made the application of pump-probe schemes routine. So far, however, most studies have been focused on two questions: (i) the refinement of structural changes during the course of a reaction, and (ii) possible relations between transient structural changes and the intermediates found by optical spectroscopy. In this work, a kinetic description for different time laws in time-resolved X-ray diffraction experiments is derived in the framework of time-dependent correlation functions. The derived time laws were applied to time-resolved studies on a [2+2] photodimerization and a reversible reaction undergoing structural reorganization.

scholarly journals The time-resolved hard X-ray diffraction endstation KMC-3 XPP at BESSY II

2021 ◽  
Vol 28 (3) ◽  
Author(s):  
Matthias Rössle ◽  
Wolfram Leitenberger ◽  
Matthias Reinhardt ◽  
Azize Koç ◽  
Jan Pudell ◽  
...  
Keyword(s):  
Storage Ring ◽  
Single Photon ◽  
Laser System ◽  
High Vacuum ◽  
Laser Pulses ◽  
Pixel Detector ◽  
X Ray Diffraction ◽  
Optical Pump ◽  
Time Resolved ◽  
X Ray

The time-resolved hard X-ray diffraction endstation KMC-3 XPP for optical pump/X-ray probe experiments at the electron storage ring BESSY II is dedicated to investigating the structural response of thin film samples and heterostructures after their excitation with ultrashort laser pulses and/or electric field pulses. It enables experiments with access to symmetric and asymmetric Bragg reflections via a four-circle diffractometer and it is possible to keep the sample in high vacuum and vary the sample temperature between ∼15 K and 350 K. The femtosecond laser system permanently installed at the beamline allows for optical excitation of the sample at 1028 nm. A non-linear optical setup enables the sample excitation also at 514 nm and 343 nm. A time-resolution of 17 ps is achieved with the `low-α' operation mode of the storage ring and an electronic variation of the delay between optical pump and hard X-ray probe pulse conveniently accesses picosecond to microsecond timescales. Direct time-resolved detection of the diffracted hard X-ray synchrotron pulses use a gated area pixel detector or a fast point detector in single photon counting mode. The range of experiments that are reliably conducted at the endstation and that detect structural dynamics of samples excited by laser pulses or electric fields are presented.

Influence of Aging Time on the Structural Changes of Cassava Thermoplastic Starch

2012 ◽  
Vol 1372 ◽  
Author(s):  
José H. Mina ◽  
Alex Valadez ◽  
Pedro J. Herrera-Franco ◽  
Tanit Toledano
Keyword(s):  
Yield Stress ◽  
Amorphous Phase ◽  
Structural Changes ◽  
Thermoplastic Starch ◽  
X Ray Diffraction ◽  
X Ray ◽  
Second Stage ◽  
Diffraction Patterns ◽  
Type V ◽  
Stress Drops

ABSTRACTIn this work the change in the structural properties of cassava (manihot sculenta Crantz) thermoplastic starch (TPS) under controlled environment (humidity and temperature) was studied. Fourier Transform Infrared spectroscopy (FTIR) and X-ray diffraction (XRD) results showed an evident increasing in the amorphous phase of the TPS regarding the native starch. There was a relative decrease of the band at 1047 cm-1 associated to crystalline structure of starch compared to the amorphous peak at 1022 cm-1. The X-ray diffraction patterns confirmed the increment of the amorphous phase in the TPS samples. Likewise the X-ray diffraction patterns shows evidence of residual type C crystallinity and the formation of a new crystalline phase type VH due to the orientation induced in plasticization process. In first stage of conditioning the tensile yield stress drops from 7.5 drops to 0.5 MPa and the break strain increases 1000%. At the same time it seems that the crystallinity of the samples increases as was evidenced by the gradually increasing of the FTIR band at 1047 cm-1. In a second stage, the yield stress increases, the break strain drops and the crystallinity continue growing steadily. These findings suggest that coexist two phenomena simultaneously in the samples. A phenomenon of re-crystallization (retrogradation) that tends to make the material more stiff and a process of plasticization that tends to softening it. It seems that the latter mechanism predominates in the first stage, at short times, and the former in the second stage, at older times.

scholarly journals First steps towards time-resolved 'in-house' X-ray diffraction experiments

2014 ◽  
Vol 70 (a1) ◽  
pp. C775-C775 ◽  
Author(s):  
Radoslaw Kaminski ◽  
Jason Benedict ◽  
Elzbieta Trzop ◽  
Katarzyna Jarzembska ◽  
Bertrand Fournier ◽  
...  
Keyword(s):  
Excited State ◽  
Time Resolution ◽  
Structural Changes ◽  
Laser Pulses ◽  
High Repetition Rate ◽  
X Ray Diffraction ◽  
Laboratory Equipment ◽  
Time Resolved ◽  
X Ray ◽  
Ligand Charge Transfer

High-intensity X-ray sources, such as synchrotrons or X-ray free electron lasers, providing up to 100 ps time-resolution allow for studying very short-lived excited electronic states in molecular crystals. Some recent examples constitute investigations of Rh...Rh bond shortening,[1] or metal-to-ligand charge transfer processes in CuI complexes.[2] Nevertheless, in cases in which the lifetime of excited state species exceeds 10 μs it is now possible, due to the dramatic increase in the brightness of X-ray sources and the sensitivity of detectors, to use laboratory equipment to explore structural changes upon excitation. Consequently, in this contribution we present detailed technical description of the 'in-house' X-ray diffraction setup allowing for the laser-pump X-ray-probe experiments within the time-resolution at the order of 10 μs or larger. The experimental setup consists of a modified Bruker Mo-rotating-anode diffractometer, coupled with the high-frequency Nd:YAG laser (λ = 355 nm). The required synchronization of the laser pulses and the X-ray beam is realized via the optical chopper mounted across the beam-path. Chopper and laser capabilities enable high-repetition-rate experiments reaching up to 100 kHz. In addition, the laser shutter is being directly controlled though the original diffractometer software, allowing for collection of the data in a similar manner as done at the synchrotron (alternating light-ON & light-OFF frames). The laser beam itself is split into two allowing for improved uniform light delivery onto the crystal specimen. The designed setup was tested on the chosen set of crystals exhibiting rather long-lived excited state, such as, the Cu2Br2L2 (L = C5H4N-NMe2) complex, for which the determined lifetime is about 100 μs at 90 K. The results shall be presented. Research is funded by the National Science Foundation (CHE1213223). KNJ is supported by the Polish Ministry of Science and Higher Education through the "Mobility Plus" program.

scholarly journals A Flow-Through Reaction Cell for Studying Minerals Leaching by In-Situ Synchrotron Powder X-ray Diffraction

Minerals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 990
Author(s):  
Fatemeh Nikkhou ◽  
Fang Xia ◽  
Xizhi Yao ◽  
Idowu A. Adegoke ◽  
Qinfen Gu ◽  
...  
Keyword(s):  
Flow Rate ◽  
Pressure Leaching ◽  
X Ray Diffraction ◽  
Reaction Cell ◽  
Time Resolved ◽  
X Ray ◽  
Ore Minerals ◽  
Flow Through ◽  
Diffraction Patterns

A flow-through reaction cell has been developed for studying minerals leaching by in-situ time-resolved powder X-ray diffraction, allowing for a better understanding of the leaching mechanisms and kinetics. The cell has the capability of independent control of temperature (up to 95 °C) and flow rate (>0.5 mL min−1) for atmospheric pressure leaching. It was successfully tested at the powder diffraction beamline at the Australian Synchrotron. Galena powder was leached in a citrate solution under flow-through condition at a flow rate of 0.5 mL min−1, while diffraction patterns were collected during the entire leaching process, showing rapid galena dissolution without the formation of secondary mineral phases. The flow-through cell can be used to study leaching processes of other ore minerals.

scholarly journals Time-resolved X-ray diffraction study of structural changes associated with the photocycle of bacteriorhodopsin.

1991 ◽  
Vol 10 (3) ◽  
pp. 521-526 ◽  
Author(s):  
M. H. Koch ◽  
N. A. Dencher ◽  
D. Oesterhelt ◽  
H. J. Plöhn ◽  
G. Rapp ◽  
...  
Keyword(s):  
Diffraction Study ◽  
Structural Changes ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray

scholarly journals Observation of Transient Structural Changes on Hydrogen Absorption Process of LaNi4.75Sn0.25 by Time Resolved X-Ray Diffraction

2015 ◽  
Vol 79 (3) ◽  
pp. 124-130 ◽  
Author(s):  
Akihiko Machida ◽  
Kensuke Higuchi ◽  
Yoshinori Katayama ◽  
Kouji Sakaki ◽  
Hyunjeong Kim ◽  
...  
Keyword(s):  
Hydrogen Absorption ◽  
Structural Changes ◽  
Absorption Process ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray

scholarly journals Coherent convergent-beam time-resolved X-ray diffraction

2014 ◽  
Vol 369 (1647) ◽  
pp. 20130325 ◽  
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.

Structural changes during activation of frog muscle studied by time-resolved X-ray diffraction

1986 ◽  
Vol 188 (3) ◽  
pp. 325-342 ◽  
Author(s):  
M. Kress ◽  
H.E. Huxley ◽  
A.R. Faruqi ◽  
J. Hendrix
Keyword(s):  
Structural Changes ◽  
Frog Muscle ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray
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