Multipurpose diffractometer for in situ X-ray crystallography of functional materials

2021 ◽  
Vol 54 (3) ◽  
Author(s):  
Semën Gorfman ◽  
David Spirito ◽  
Netanela Cohen ◽  
Peter Siffalovic ◽  
Peter Nadazdy ◽  
...  
Keyword(s):  
Electric Field ◽  
Materials Science ◽  
Functional Materials ◽  
X Ray Diffraction ◽  
Reciprocal Space Mapping ◽  
X Ray ◽  
X Ray Crystallography ◽  
Area Detector ◽  
Characterization Of Materials

Laboratory X-ray diffractometers play a crucial role in X-ray crystallography and materials science. Such instruments still vastly outnumber synchrotron facilities and are responsible for most of the X-ray characterization of materials around the world. The efforts to enhance the design and performance of in-house X-ray diffraction instruments benefit a broad research community. Here, the realization of a custom-built multipurpose four-circle diffractometer in the laboratory for X-ray crystallography of functional materials at Tel Aviv University, Israel, is reported. The instrument is equipped with a microfocus Cu-based X-ray source, collimating X-ray optics, four-bounce monochromator, four-circle goniometer, large (PILATUS3 R 1M) pixel area detector, analyser crystal and scintillating counter. It is suitable for a broad range of tasks in X-ray crystallography/structure analysis and materials science. All the relevant X-ray beam parameters (total flux, flux density, beam divergence, monochromaticity) are reported and several applications such as determination of the crystal orientation matrix and high-resolution reciprocal-space mapping are demonstrated. The diffractometer is suitable for measuring X-ray diffraction in situ under an external electric field, as demonstrated by the measurement of electric-field-dependent rocking curves of a quartz single crystal. The diffractometer can be used as an independent research instrument, but also as a training platform and for preparation for synchrotron experiments.

scholarly journals In situ X-ray diffraction investigation of electric-field-induced switching in a hybrid improper ferroelectric

2021 ◽  
Vol 54 (2) ◽  
pp. 533-540
Author(s):  
Gabriel Clarke ◽  
Chris Ablitt ◽  
John Daniels ◽  
Stefano Checchia ◽  
Mark S. Senn
Keyword(s):  
Electric Field ◽  
Simulated Data ◽  
Functional Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Switching Mechanism ◽  
One Step ◽  
Diffraction Patterns ◽  
Ferroelectric Switching

Improper ferroelectric mechanisms are increasingly under investigation for their potential to expand the current catalogue of functional materials whilst promoting couplings between ferroelectricity and other technologically desirable properties such as ferromagnetism. This work presents the results of an in situ synchrotron X-ray diffraction experiment performed on samples of Ca2.15Sr0.85Ti2O7 in an effort to elucidate the mechanism of hybrid improper ferroelectric switching in this compound. By simultaneously applying an electric field and recording diffraction patterns, shifts in the intensity of superstructure peaks consistent with one of the switching mechanisms proposed by Nowadnick & Fennie [Phys. Rev. B, (2016), 94, 104105] are observed. While the experiment only achieves a partial response, comparison with simulated data demonstrates a preference for a one-step switching mechanism involving an unwinding of the octahedral rotation mode in the initial stages of switching. These results represent some of the first reported experimental diffraction-based evidence for a switching mechanism in an improper ferroelectric.

scholarly journals Revealing the mechanism of electric-field-induced phase transition in antiferroelectric NaNbO3 by in situ high-energy x-ray diffraction

2021 ◽  
Vol 118 (13) ◽  
pp. 132903
Author(s):  
Mao-Hua Zhang ◽  
Changhao Zhao ◽  
Lovro Fulanović ◽  
Jürgen Rödel ◽  
Nikola Novak ◽  
...  
Keyword(s):  
Phase Transition ◽  
Electric Field ◽  
High Energy ◽  
X Ray Diffraction ◽  
X Ray

Electric-field-induced lattice distortion in epitaxial BiFeO3 thin films as determined by in situ time-resolved x-ray diffraction

2017 ◽  
Vol 111 (8) ◽  
pp. 082907 ◽  
Author(s):  
Seiji Nakashima ◽  
Osami Sakata ◽  
Hiroshi Funakubo ◽  
Takao Shimizu ◽  
Daichi Ichinose ◽  
...  
Keyword(s):  
Thin Films ◽  
Electric Field ◽  
Lattice Distortion ◽  
X Ray Diffraction ◽  
Time Resolved ◽  
X Ray ◽  
Bifeo3 Thin Films

Phase Transformations in the Brazing Joint during Transient Liquid Phase Bonding of a γ-TiAl Alloy Studied with In Situ High-Energy X-Ray Diffraction

2018 ◽  
Vol 941 ◽  
pp. 943-948
Author(s):  
Katja Hauschildt ◽  
Andreas Stark ◽  
Hilmar Burmester ◽  
Ursula Tietze ◽  
Norbert Schell ◽  
...  
Keyword(s):  
Liquid Phase ◽  
Materials Science ◽  
Transient Liquid Phase ◽  
High Energy ◽  
Transient Liquid Phase Bonding ◽  
X Ray Diffraction ◽  
Energy Materials ◽  
Joint Region ◽  
X Ray

TiAl alloys are increasingly used as a lightweight material, for example in aero engines, which also leads to the requirement for suitable repair techniques. Transient liquid phase bonding is a promising method for the closure of cracks (in non-critical or non-highly loaded areas). The brazing solder Ti-24Ni was investigated for brazing the alloy Ti-45Al-5Nb-0.2B-0.2C (in at. %). After brazing, the joint exhibits different microstructures and phase compositions. The transient liquid phase bonding process was investigated in the middle of the joint region in situ to acquire time resolved information of the phases, their development, and thus the brazing process. These investigations were performed using high-energy X-ray diffraction at the “High-Energy Materials Science” beamline HEMS, located at the synchrotron radiation facility PETRA III at DESY in Hamburg, Germany. For this, we used an induction furnace, which is briefly described here. During the analysis of the diffraction data with Rietveld refinement, the amount of liquid was refined with Gaussian peaks and thus could be quantified. Furthermore, while brazing four different phases occurred in the middle of the joint region over time. Additionally, the degree of ordering of the βo phase was determined with two ideal stoichiometric phases (completely ordered and disordered). Altogether, the phase composition changed clearly over the first six hours of the brazing process.

A furnace and environmental cell for thein situinvestigation of molten salt electrolysis using high-energy X-ray diffraction

2011 ◽  
Vol 19 (1) ◽  
pp. 39-47 ◽  
Author(s):  
Mark J. Styles ◽  
Matthew R. Rowles ◽  
Ian C. Madsen ◽  
Katherine McGregor ◽  
Andrew J. Urban ◽  
...  
Keyword(s):  
Molten Salt ◽  
Inert Anode ◽  
High Energy ◽  
X Ray Diffraction ◽  
Molten Salt Electrolysis ◽  
X Ray ◽  
Quantitative Measurements ◽  
Materials Used ◽  
Characterization Of Materials

This paper describes the design, construction and implementation of a relatively large controlled-atmosphere cell and furnace arrangement. The purpose of this equipment is to facilitate thein situcharacterization of materials used in molten salt electrowinning cells, using high-energy X-ray scattering techniques such as synchrotron-based energy-dispersive X-ray diffraction. The applicability of this equipment is demonstrated by quantitative measurements of the phase composition of a model inert anode material, which were taken during anin situstudy of an operational Fray–Farthing–Chen Cambridge electrowinning cell, featuring molten CaCl2as the electrolyte. The feasibility of adapting the cell design to investigate materials in other high-temperature environments is also discussed.

In situ synchrotron X-ray diffraction of thin films under perturbation by an electric field

2018 ◽  
Vol 537 (1) ◽  
pp. 20-26 ◽  
Author(s):  
Henrik Hovde Sønsteby ◽  
Julia Wind ◽  
Martin Jensen ◽  
Thomas Aarflot Storaas ◽  
Dmitry Chernyshov ◽  
...  
Keyword(s):  
Thin Films ◽  
Electric Field ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals A Graphene-Based Microfluidic Platform for Electrocrystallization and In Situ X-ray Diffraction

Crystals ◽  
2018 ◽  
Vol 8 (2) ◽  
pp. 76 ◽  
Author(s):  
Shuo Sui ◽  
Yuxi Wang ◽  
Christos Dimitrakopoulos ◽  
Sarah Perry
Keyword(s):  
Electric Field ◽  
Internal Electric Field ◽  
X Ray Diffraction ◽  
Large Area ◽  
Microfluidic Platform ◽  
X Ray ◽  
Egg White Lysozyme ◽  
Constant Potential ◽  
Transparent Windows

Here, we describe a novel microfluidic platform for use in electrocrystallization experiments. The device incorporates ultra-thin graphene-based films as electrodes and as X-ray transparent windows to enable in situ X-ray diffraction analysis. Furthermore, large-area graphene films serve as a gas barrier, creating a stable sample environment over time. We characterize different methods for fabricating graphene electrodes, and validate the electrical capabilities of our device through the use of methyl viologen, a redox-sensitive dye. Proof-of-concept electrocrystallization experiments using an internal electric field at constant potential were performed using hen egg-white lysozyme (HEWL) as a model system. We observed faster nucleation and crystal growth, as well as a higher signal-to-noise for diffraction data obtained from crystals prepared in the presence of an applied electric field. Although this work is focused on the electrocrystallization of proteins for structural biology, we anticipate that this technology should also find utility in a broad range of both X-ray technologies and other applications of microfluidic technology.

Combining `dry' co-crystallization andin situdiffraction to facilitate ligand screening by X-ray crystallography

2015 ◽  
Vol 71 (8) ◽  
pp. 1777-1787 ◽  
Author(s):  
Muriel Gelin ◽  
Vanessa Delfosse ◽  
Frédéric Allemand ◽  
François Hoh ◽  
Yoann Sallaz-Damaz ◽  
...  
Keyword(s):  
Protein Crystallization ◽  
X Ray Diffraction ◽  
X Ray ◽  
X Ray Crystallography ◽  
Ligand Screening ◽  
Alternative Approach ◽  
Manual Handling ◽  
Stock Solutions ◽  
Established Technique

X-ray crystallography is an established technique for ligand screening in fragment-based drug-design projects, but the required manual handling steps – soaking crystals with ligand and the subsequent harvesting – are tedious and limit the throughput of the process. Here, an alternative approach is reported: crystallization plates are pre-coated with potential binders prior to protein crystallization and X-ray diffraction is performed directly `in situ' (or in-plate). Its performance is demonstrated on distinct and relevant therapeutic targets currently being studied for ligand screening by X-ray crystallography using either a bending-magnet beamline or a rotating-anode generator. The possibility of using DMSO stock solutions of the ligands to be coated opens up a route to screening most chemical libraries.

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