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

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.

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 ◽  
...  

1996 ◽  
Vol 449 ◽  
Author(s):  
L.J. Lauhon ◽  
S. A. Ustin ◽  
W. Ho

ABSTRACTAlN, GaN, and SiC thin films were grown on 100 mm diameter Si(111) and Si(100) substrates using Supersonic Jet Epitaxy (SJE). Precursor gases were seeded in lighter mass carrier gases and free jets were formed using novel slit-jet apertures. The jet design, combined with substrate rotation, allowed for a uniform flux distribution over a large area of a 100 mm wafer at growth pressures of 1–20 mTorr. Triethylaluminum, triethylgailium, and ammonia were used for nitride growth, while disilane, acetylene, and methylsilane were used for SiC growth. The films were characterized by in situ optical reflectivity, x-ray diffraction (XRD), atomic force microscopy (AFM), and spectroscopic ellipsometry (SE).


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.


2013 ◽  
Vol 46 (4) ◽  
pp. 1151-1161 ◽  
Author(s):  
Pierre Fertey ◽  
Paul Alle ◽  
Emmanuel Wenger ◽  
Bernard Dinkespiler ◽  
Olivier Cambon ◽  
...  

A new experimental approach to perform in situ electric field diffraction on single crystals using an on-then-off pump–probe mode in situ (i.e. the field-switching method) with a synchrotron or a laboratory X-ray source is presented. Taking advantage of the fast readout of the XPAD hybrid pixel two-dimensional detector and its programmable functionalities, the operation mode of the detector has been customized to significantly increase the efficiency of the method. The very weak electric field-induced structural response of a piezoelectric crystal can be accurately measured. This allows the piezoelectric tensor to be precisely obtained from Δθ shifts while the structural variations can be modelled using a full set of ΔI/I data. The experimental method and methodology are detailed and tested as a case study on pure piezoelectric compounds belonging to the α-quartz family (SiO2 and GaAsO4 single crystals). Using the two scan modes developed, it is demonstrated that tiny Bragg angle shifts can be measured as well as small field-induced Bragg intensity variations (<1%). The relevance of measurements performed with an X-ray laboratory source is demonstrated: partial data sets collected at synchrotrons can be completed, but more interestingly, a large part of the study can now be realized in the laboratory (medium to strong intensity reflections) in a comparable data collection time.


Author(s):  
Charline J. J. Gerard ◽  
Gilles Ferry ◽  
Laurent M. Vuillard ◽  
Jean A. Boutin ◽  
Leonard M. G. Chavas ◽  
...  

A microfluidic platform was used to address the problems of obtaining diffraction-quality crystals and crystal handling during transfer to the X-ray diffractometer. Crystallization conditions of a protein of pharmaceutical interest were optimized and X-ray data were collected both in situ and ex situ.


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

2017 ◽  
Vol 905 ◽  
pp. 137-142
Author(s):  
Tatsumi Hirano ◽  
Daiko Takamatsu ◽  
Kosuke Kuwabara ◽  
Shuo Yuan Zhang ◽  
Takahisa Shobu ◽  
...  

Welding technologies are indispensable for fabricating various industrial structures and must be highly reliable. Since tensile residual stresses at surface after welding cause crack progress, it is important to understand how stresses built up during the welding process in order to optimize final residual stresses as reduced tensile or introduced compressive stresses. Therefore, we conducted in-situ measurements of phase transformations, stresses and temperatures during tungsten inert gas (TIG) welding to understand how stresses built up. X-ray diffraction rings were detected per 0.1 sec during TIG welding by using a large-area two-dimensional detector and the accuracy of the stress analysis was estimated to be 8 MPa using the sin2ψ technique. In this paper, we described the phase transformations of ferrite low-carbon rolled steel and the changes in stresses during TIG welding.


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