X-ray diffraction study of lithium hydrazinium sulfate and lithium ammonium sulfate crystals under a static electric field

1991 ◽  
Vol 24 (6) ◽  
pp. 1015-1022 ◽  
Author(s):  
M. T. Sebastian ◽  
R. A. Becker ◽  
H. Klapper

X-ray diffraction studies are made on proton conducting polar lithium hydrazinium sulfate and ferroelectric lithium ammonium sulfate. The X-ray rocking curves recorded with in situ electric field along the polar b axis of lithium hydrazinium sulfate (direction of proton conductivity) show a strong enhancement of the 0k0 diffraction intensity. The corresponding 0k0 X-ray topographs reveal extinction contrast consisting of striations parallel to the polar axis. They disappear when the electric field is switched off. The effect is very strong in 0k0 but invisible in h0l reflections. It is present only if the electric field is parallel to the polar axis b. This unusual X-ray topographic contrast is correlated with the proton conduction. It is supposed that, under electric field, an inhomogeneous charge distribution develops, distorting the crystal lattice. Similar experiments on lithium ammonium sulfate also show contrast variations, but of quite different behaviour than before. In this case they result from changes of the ferroelectric domain configuration under electric field.

1992 ◽  
Vol 25 (2) ◽  
pp. 274-280 ◽  
Author(s):  
M. T. Sebastian ◽  
H. Klapper ◽  
R. J. Bolt

X-ray diffraction studies are made on ion-conducting potassium titanyl phosphate (KTP) crystals with in situ DC electric field along different crystallographic directions. The X-ray rocking curves recorded with an electric field along the polar b axis (which is the direction of ion conduction) show a strong enhancement of the 040 reflection intensity (reflecting planes normal to the b axis) whereas the h0l reflections (reflecting planes parallel to the polar axis) do not show any intensity change. For an electric field normal to the polar axis no intensity change, either in 040 or in h0l reflections, occurs. This observation is supplemented by X-ray topography. The 040 X-ray topographs recorded with in situ electric field along b exhibit strong extinction contrast in the form of striations parallel to the polar (ion-conduction) axis. The 040 intensity increase and the striation contrast are attributed to lattice deformation by the space-charge polarization due to the movement of the K+ ions under the influence of the electric field.


2021 ◽  
Vol 118 (13) ◽  
pp. 132903
Author(s):  
Mao-Hua Zhang ◽  
Changhao Zhao ◽  
Lovro Fulanović ◽  
Jürgen Rödel ◽  
Nikola Novak ◽  
...  

2017 ◽  
Vol 111 (8) ◽  
pp. 082907 ◽  
Author(s):  
Seiji Nakashima ◽  
Osami Sakata ◽  
Hiroshi Funakubo ◽  
Takao Shimizu ◽  
Daichi Ichinose ◽  
...  

2021 ◽  
Vol 54 (3) ◽  
Author(s):  
Semën Gorfman ◽  
David Spirito ◽  
Netanela Cohen ◽  
Peter Siffalovic ◽  
Peter Nadazdy ◽  
...  

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.


2018 ◽  
Vol 537 (1) ◽  
pp. 20-26 ◽  
Author(s):  
Henrik Hovde Sønsteby ◽  
Julia Wind ◽  
Martin Jensen ◽  
Thomas Aarflot Storaas ◽  
Dmitry Chernyshov ◽  
...  

Crystals ◽  
2018 ◽  
Vol 8 (2) ◽  
pp. 76 ◽  
Author(s):  
Shuo Sui ◽  
Yuxi Wang ◽  
Christos Dimitrakopoulos ◽  
Sarah Perry

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.


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