Current developments in time-resolved X-ray diffraction

Techert, Simone

doi:10.1080/08893110600688873

Cited by 6 publications

(6 citation statements)

References 33 publications

(46 reference statements)

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“…26 The 2-aminobiphenyl derivatives were converted to the corresponding azides using standard diazotization conditions. 27 The identity of all compounds was established by 1 H NMR, 13 C NMR, and Fourier transfrom infrared spectra, which matched reported data from all the known compounds. Subsequent recrystallization from acetonitrile yielded crystalline solids in all cases except for 1D, which is a liquid at ambient temperature (Table 1).…”

mentioning

confidence: 72%

Photochemistry and Transmission Pump–Probe Spectroscopy of 2-Azidobiphenyls in Aqueous Nanocrystalline Suspensions: Simplified Kinetics in Crystalline Solids

Chung

Ayitou

Park

et al. 2017

J. Phys. Chem. Lett.

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Aqueous nanocrystalline suspensions provide a simple and efficient medium for performing transmission spectroscopy measurements in the solid state. In this Letter we describe the use of laser flash photolysis methods to analyze the photochemistry of 2-azidobiphenyl and several aryl-substituted derivatives. We show that all the crystalline compounds analyzed in this study transform quantitatively into carbazole products via a crystal-to-crystal reconstructive phase transition. While the initial steps of the reaction cannot be followed within the time resolution of our instrument (ca. 8 ns), we detected the primary isocarbazole photoproducts and analyzed the kinetics of their formal 1,5-H shift reactions, which take place in time scales that range from a few nanoseconds to several microseconds. It is worth noting that the high reaction selectivity observed in the crystalline state translates into a clean and simple kinetic process compared to that in solution.

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confidence: 72%

Photochemistry and Transmission Pump–Probe Spectroscopy of 2-Azidobiphenyls in Aqueous Nanocrystalline Suspensions: Simplified Kinetics in Crystalline Solids

Chung

Ayitou

Park

et al. 2017

J. Phys. Chem. Lett.

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“…Area detectors are currently in use at the majority of X-ray diffraction instruments implemented at synchrotron sources, with applications ranging from protein crystallography to materials science. Owing to the availability of high-brilliance X-ray beams and short acquisition times, the utilization of area detectors has become state-of-the-art in crystallography (Helliwell, 2012), structural characterization of polycrystals (Poulsen, 2004;Sørensen et al, 2012), time-resolved diffraction (Techert, 2006), and various X-ray and neutron scattering techniques (Ilavsky, 2012). The aim of each experiment is the measurement of the scattered or diffracted intensity as a function of the reciprocal space vector Q, the accuracy of which is a prerequisite for obtaining physically meaningful results.…”

Section: Introductionmentioning

confidence: 99%

On the calibration of high-energy X-ray diffraction setups. I. Assessing tilt and spatial distortion of the area detector

et al. 2014

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International audienceThe geometry of high-energy X-ray diffraction setups using an area detector and a rotation axis is analysed. The present paper (part 1) describes the methodology for determining continuously varying spatial distortions and tilt of the area detector based on the reference diffraction rings of a certified powder. Analytical expressions describing the degeneration of Debye rings into ellipses are presented and a robust calibration procedure is introduced. It is emphasized that accurate detector calibration requires the introduction of spatial distortion into the equation describing the tilt. The method is applied to data sets measured at the Advanced Photon Source and at the European Synchrotron Radiation Facility using detectors with different physical characteristics, the GE 41RT flat-panel and the FReLoN4M detector, respectively. The spatial distortion of the detectors is compared with regard to their use in structural and strain tensor analysis, a subject treated in part 2 of the calibration work [Borbely, Renversade & Kenesei (2014). J. Appl. Cryst. Submitted]

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“…This interest relates to the increasing requirement of getting a deeper insight into the changes that occur when a chemical or physical transformation or reaction takes place in the sample under investigation. Time-resolved structural characterization is a valuable tool in this respect, and usually such techniques are used to study the reaction kinetics at a defined reaction temperature, [1][2][3] mainly by means of X-ray diffraction (XRD). On the other hand, neutron diffraction (ND) is a valuable tool to investigate oxides owing to the sensitivity of neutrons to light atoms such as oxygen and to the possibility of revealing superstructure peaks.…”

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confidence: 99%

In Situ Time‐Resolved Neutron Diffraction Investigation during Oxygen Exchange in Layered Cobaltite Cathode Materials

Malavasi¹,

Tealdi²,

Ritter³

2009

Angew Chem Int Ed

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The development of in situ techniques for the characterization of solid phases is becoming one of the major issues in current research on materials. This interest relates to the increasing requirement of getting a deeper insight into the changes that occur when a chemical or physical transformation or reaction takes place in the sample under investigation. Time-resolved structural characterization is a valuable tool in this respect, and usually such techniques are used to study the reaction kinetics at a defined reaction temperature, [1][2][3] mainly by means of X-ray diffraction (XRD). On the other hand, neutron diffraction (ND) is a valuable tool to investigate oxides owing to the sensitivity of neutrons to light atoms such as oxygen and to the possibility of revealing superstructure peaks. Highly studied materials which benefit from the investigation through ND are solid-state ionic (SSI) materials (mainly electrolytes and mixed ionic-electronic materials) for which, for example, the study of oxygen-exchange processes are of great importance to test their performance and define the temperature range for their potential application. To date, to the best of our knowledge, there are no available experimental probes to study the structural evolution of a crystalline solid during oxygen-exchange processes. As the investigated material undergoes a structural change during the diffusion of oxygen into or out of it, it would be highly desirable to develop a method able to simultaneously study the oxygen content variation profile and the structural variation occurring in the sample. This technique could pave the way for extraction of new and essential information on the phenomena occurring during oxygen exchange and can be of relevance for the comprehension of the oxygen migration mechanism and, therefore, could guide the design of optimized compositions.In view of these relevant applications, we have devised and carried out time-resolved in situ neutron diffraction (ND) measurements under isothermal conditions and with varied oxygen partial pressure p(O 2 ) inside the measurement apparatus. By recording neutron patterns at proper time intervals it is possible, through the refinement of oxygen occupancies, to determine the concentration profile during oxygen exchange and, at the same time, to have a clear insight into the structural changes occurring in the sample when oxygen is introduced or removed. To our knowledge, our experiment is the first of this kind carried out on any material. Herein we present the result of the experimental work, thus showing the feasibility of this approach to the study of SSI materials and, in general, of any nonstoichiometric oxygencontaining compound. It is clear that this method can also be applied to the in situ time-resolved study of any species that can be easily probed by neutrons, such as hydrogen and deuterium, thus opening new possibilities, for example in the field of hydrogen storage materials.The compound investigated herein is the HoBaCo 2 O 5+d layered cobaltite. Recently t...

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Current developments in time-resolved X-ray diffraction

Cited by 6 publications

References 33 publications

Photochemistry and Transmission Pump–Probe Spectroscopy of 2-Azidobiphenyls in Aqueous Nanocrystalline Suspensions: Simplified Kinetics in Crystalline Solids

Photochemistry and Transmission Pump–Probe Spectroscopy of 2-Azidobiphenyls in Aqueous Nanocrystalline Suspensions: Simplified Kinetics in Crystalline Solids

On the calibration of high-energy X-ray diffraction setups. I. Assessing tilt and spatial distortion of the area detector

In Situ Time‐Resolved Neutron Diffraction Investigation during Oxygen Exchange in Layered Cobaltite Cathode Materials

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