Direct observation of active material interactions in flowable electrodes using X-ray tomography

2017 ◽  
Vol 199 ◽  
pp. 511-524 ◽  
Author(s):  
Kelsey B. Hatzell ◽  
Jens Eller ◽  
Samantha L. Morelly ◽  
Maureen H. Tang ◽  
Nicolas J. Alvarez ◽  
...  
Keyword(s):  
Structural Properties ◽  
Structural Changes ◽  
Solid Phase ◽  
Active Material ◽  
Carbon Particle ◽  
Three Dimensional ◽  
Static Structure ◽  
Flow Process ◽  
X Ray ◽  
Biphasic Systems

Understanding electrical percolation and charging mechanisms in electrochemically active biphasic flowable electrodes is critical for enabling scalable deionization (desalination) and energy storage. Flowable electrodes are dynamic material systems which store charge (remove ions) and have the ability to flow. This flow process can induce structural changes in the underlying material arrangement and result in transient and non-uniform material properties. Carbon-based suspensions are opaque, multi-phase, and three dimensional, and thus prior characterization of the structural properties has been limited to indirect methods (electrochemical and rheology). Herein, a range of mixed electronic and ionically conducting suspensions are evaluated to determine their static structure, function, and properties, utilizing synchrotron radiation X-ray tomographic microscopy (SRXTM). The high brilliance of the synchrotron light enables deconvolution of the liquid and solid phases. Reconstruction of the solid phase reveals agglomeration cluster volumes between 10 μm3 and 103 μm3 (1 pL) for low loaded samples (5 wt% carbon). The largest agglomeration cluster in the low loaded sample (5 wt%) occupied only 3% of the reconstructed volume whereas samples loaded with 10 wt% activated carbon demonstrated electrically connected clusters that occupied 22% of the imaged region. The highly loaded samples (20 wt%) demonstrated clusters of the order of a microliter, which accounted for 63–85% of the imaged region. These results demonstrate a capability for discerning the structural properties of biphasic systems utilizing SRXTM techniques, and show that discontinuity in the carbon particle networks induces decreased material utilization in low-loaded flowable electrodes.

scholarly journals X-ray tracking of structural changes during a subnanosecond solid-solid phase transition in cobalt nanoparticles

2019 ◽  
Vol 100 (24) ◽  
Author(s):  
Peter Vester ◽  
Morten Christensen ◽  
Elisa Biasin ◽  
Simon O. Mariager ◽  
Gemma Newby ◽  
...  
Keyword(s):  
Phase Transition ◽  
Structural Changes ◽  
Solid Phase ◽  
Cobalt Nanoparticles ◽  
X Ray ◽  
Solid Phase Transition

scholarly journals Photocrystallography

2007 ◽  
Vol 64 (1) ◽  
pp. 259-271 ◽  
Author(s):  
Jacqueline M. Cole
Keyword(s):  
Structural Changes ◽  
Three Dimensional ◽  
Research Area ◽  
Active Species ◽  
X Ray Diffraction ◽  
X Ray ◽  
Future Possibility ◽  
New Research ◽  
Exciting Area

This review describes the development and application of a new crystallographic technique that is starting to enable the three-dimensional structural determination of molecules in their photo-activated states. So called `photocrystallography' has wide applicability, particularly in the currently exciting area of photonics, and a discussion of this applied potential is put into context in this article. Studies are classified into four groups: photo-structural changes that are (i) irreversible; (ii) long-lived but reversible under certain conditions; (iii) transient with photo-active lifetimes of the order of microseconds; (iv) very short lived, existing at the nanosecond or even picosecond level. As photo-structural changes relative to the `ground state' can be subtle, this article necessarily concentrates on small-molecule single-crystal X-ray diffraction given that high atomic resolution is possible. That said, where it is pertinent, references are also made to related major advances in photo-induced macromolecular crystallography. The review concludes with an outlook on this new research area, including the future possibility of studying even more ephemeral, femtosecond-lived, photo-active species.

scholarly journals Recent innovations in membrane-protein structural biology

F1000Research ◽  
2019 ◽  
Vol 8 ◽  
pp. 211 ◽  
Author(s):  
James P Allen
Keyword(s):  
Membrane Proteins ◽  
Structural Properties ◽  
Protein Function ◽  
Three Dimensional ◽  
Protein Crystals ◽  
Experimental Investigations ◽  
X Ray Diffraction ◽  
Single Particles ◽  
X Ray ◽  
New Instrumentation

Innovations are expanding the capabilities of experimental investigations of the structural properties of membrane proteins. Traditionally, three-dimensional structures have been determined by measuring x-ray diffraction using protein crystals with a size of least 100 μm. For membrane proteins, achieving crystals suitable for these measurements has been a significant challenge. The availabilities of micro-focus x-ray beams and the new instrumentation of x-ray free-electron lasers have opened up the possibility of using submicrometer-sized crystals. In addition, advances in cryo-electron microscopy have expanded the use of this technique for studies of protein crystals as well as studies of individual proteins as single particles. Together, these approaches provide unprecedented opportunities for the exploration of structural properties of membrane proteins, including dynamical changes during protein function.

The antigenic structure of poliovirus

1989 ◽  
Vol 323 (1217) ◽  
pp. 467-478 ◽  
Keyword(s):  
Monoclonal Antibodies ◽  
Virus Particle ◽  
Structural Changes ◽  
Three Dimensional ◽  
Antigenic Structure ◽  
X Ray ◽  
Antigenic Sites ◽  
Type 3 ◽  
Insight Into

We have solved the structure of the Mahoney strain of type 1 and the Sabin (attenuated vaccine) strain of type 3 poliovirus by X -ray crystallographic methods. By providing a three-dimensional framework for the interpretation of a wealth of experimental data, the structures have yielded insight into the architecture and assembly of the virus particle, have provided information regarding the entry of virus into susceptible cells, and defined the sites on the virus particle that are recognized by neutralizing monoclonal antibodies. Thus locating mutations in variants selected for resistance to neutralizing monoclonal antibodies has defined three antigenic sites of the surface of the virion, and provided clues as to the mechanisms by which viruses escape neutralization. Finally, comparison of the structures of the two strains, together with analysis of sequences of many poliovirus strains, have begun to define the structural changes associated with serotypic differences between polioviruses.

THERMALLY-DRIVEN STRUCTURAL CHANGES OF SPUTTERED COPPER ALUMINUM OXIDE FILMS (Cu–Al2O3) GROWN BY LAYER STACKING METHOD

2017 ◽  
Vol 24 (Supp01) ◽  
pp. 1850002
Author(s):  
WEI QIANG LIM ◽  
SHANMUGAN SUBRAMANI ◽  
MUTHARASU DEVARAJAN
Keyword(s):  
Crystallite Size ◽  
Structural Properties ◽  
Structural Changes ◽  
Annealing Temperature ◽  
Compressive Strain ◽  
Rf Magnetron Sputtering ◽  
Xrd Analysis ◽  
X Ray ◽  
Layer Stacking ◽  
Deposited Films

Copper aluminium oxide (Cu–Al2O3) films were synthesized on Si(111) substrates through RF magnetron sputtering by using the layer stacking technique. Cu and Al2O3 targets were used to deposit Cu and Al2O3 thin films under Ar atmosphere, respectively and the deposited films were then annealed under N2 environment at 350[Formula: see text]C, 450[Formula: see text]C and 550[Formula: see text]C for 6[Formula: see text]h. The structural properties of the films were investigated by using X-ray diffraction (XRD) while the surface morphology and topography of the deposited films were examined through Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersive X-ray (EDX) and Atomic Force Microscopy (AFM). XRD analysis revealed the existence of multiple phases of CuO, Al2O3 and CuAl2O4 in the deposited films on Si(111) substrates. As a result of the annealing effect, the peak intensities of CuO, Al2O3 and CuAl2O4 were found to be increased along with the shifting of peak positions. Williamson–Hall (WH) analysis was also implemented to analyze the structural properties such as crystallite size, stress, strain, and energy density. Based on the three models used in WH analysis, the changes in the crystallite size and strain of the films were indicated to be anomalous with the changes in the annealing temperature. Moreover, the strain of films was also showed to be changed from compressive strain into tensile strain. The FESEM results also indicated the formation of various surface morphologies under various annealing temperatures whereas EDX analysis showed an increased atomic percentage of Cu, Al, and O due to the effect of increase in annealing temperature. The AFM analysis showed that the surface roughness of the deposited films increased with the increase in the annealing temperature.

scholarly journals Three dimensional soil organic matter distribution, accessibility and microbial respiration in macro-aggregates using osmium staining and synchrotron X-ray CT

2016 ◽  
Author(s):  
Barry G Rawlins ◽  
Joanna Wragg ◽  
Christina Rheinhard ◽  
Robert C Atwood ◽  
Alasdair Houston ◽  
...  
Keyword(s):  
Organic Matter ◽  
Transition Probabilities ◽  
Solid Phase ◽  
Pore Space ◽  
Three Dimensional ◽  
Soil Core ◽  
Length Scales ◽  
X Ray ◽  
Mineral Phases ◽  
Indicator Variograms

Abstract. The spatial distribution and accessibility of organic matter (OM) to soil microbes in aggregates – determined by the fine-scale, 3-D distribution of organic matter, pores and mineral phases – may be an important control on the magnitude of soil heterotrophic respiration (SHR). Attempts to model SHR at fine scales requires data on the transition probabilities between adjacent pore space and soil OM, a measure of microbial accessibility to the latter. We used a combination of osmium staining and synchrotron X-ray CT to determine the 3-D (voxel) distribution of these three phases (scale 6.6 μm) throughout nine aggregates taken from a single soil core (range of organic carbon (OC) concentrations 4.2–7.7 %). Prior to the synchrotron analyses we had measured the magnitude of SHR for each aggregate over 24 hours under controlled conditions (moisture content and temperature). We test the hypothesis that larger magnitudes of SHR will be observed in aggregates with shorter length scales of OM variation (i.e. more frequent, and possibly more finely disseminated, OM and a larger number of aerobic microsites). After scaling to their OC concentrations, there was a six-fold variation in the magnitude of SHR for the nine aggregates. The distribution of pore volumes, pore shape and volume normalised surface area were similar for each of the nine aggregates. The overall transition probabilities between OM and pore voxels were between 0.02 and 0.03, significantly smaller than those used in previous simulation studies. We computed the length scales over which OM, pore and mineral phases vary within each aggregate using indicator variograms. The median range of models fitted to variograms of OM varied between 178 and 487 μm. The linear correlation between these median length scales of OM variation and the magnitudes of SHR for each aggregate was −0.42, providing some evidence to support our hypothesis. We require a larger number of observations to make a statistical inference. There was no evidence to suggest a statistical relationship between OM:pore transition probabilities and the magnitudes of aggregate SHR. The solid-phase volume proportions (45–63 %) of OM we report for our aggregates were surprisingly large by comparison to those assumed in previous modelling approaches. We suggest this requires further assessment using accurate measurements of OM bulk density in a range of soil types.

3-D Imaging of Deep-Fat Fried Chicken Nuggets Breading Coating Using X-Ray Micro-CT

2009 ◽  
Vol 5 (4) ◽  
Author(s):  
Akinbode A. Adedeji ◽  
Michael O. Ngadi
Keyword(s):  
Mass Transfer ◽  
Structural Properties ◽  
Structural Changes ◽  
Imaging Techniques ◽  
Micro Ct ◽  
Microstructural Properties ◽  
Chicken Nuggets ◽  
Frying Time ◽  
X Ray ◽  
Fried Foods

Food coatings are used to add value to deep-fat fried foods and to control heat and mass transfer during frying. They impart special characteristics such as crispiness and flavor to fried products while they also form a barrier to moisture and fat transfer during frying. Development of structure during frying plays an important role in defining the performance of batter/bread coatings. Food structural properties such as porosity have been associated with fat uptake in fried foods. A good understanding of the microstructural properties is necessary in order to produce high quality fried foods. X-ray micro-computed tomography (X-ray micro-CT) is a unique technique for imaging food non-invasively, requiring no or minimal sample preparation and 3-D rendition of high resolution images. The technique is capable of providing morphological details under a natural environment, which gives some advantages over the conventional imaging techniques such as microscopy. Study on chicken nuggets provided useful information relating frying conditions to structural changes in the breading-batter coating using X-ray micro-CT technique. Chicken nuggets were fried at 180°C for different frying durations after which the products were scanned using X-ray micro-CT. Images were reconstructed and analyzed, and 2-D and 3-D renditions of the coating images confirmed porosity changes with frying time. Numerical slicing of the 3-D images with image analysis software showed the degree of interconnectivity of pores, pore shape and pore count under different conditions of frying. The effect of frying time on microstructural parameters is significant. X-ray micro-CT shows great prospect in characterizing microstructural properties of foods especially coated fried products. This technique could be used in optimizing mass transfer during deep-fat frying by providing quantitative information on structural properties such as porosity, pore size distribution and pore connectivity.

scholarly journals USE OF DUST X-RAY DIFFRACTION IN THE CHARACTERIZATION OF PEROVSKITAS TYPE FERRITES

2008 ◽  
Vol 05 (9) ◽  
pp. 23-30
Author(s):  
Márcio DE PAULA ◽  
Regina Helena Porto FRANCISCO
Keyword(s):  
Solid State ◽  
Powder Diffraction ◽  
Structural Changes ◽  
Solid Phase ◽  
Orthorhombic Phase ◽  
Polycrystalline Sample ◽  
Cubic Phase ◽  
X Ray Diffraction ◽  
X Ray

The X-ray diffraction is one experimental method very important on characterization solids compounds. In the case of polycrystalline samples, the x-ray powder diffraction allows for the identification of the solid phase and the characterization of structural changes. The present paper was prepared any antiferromagnetic ceramic phases, bicalcic ferrite derivate (Ca2Fe2O5) by solid state reaction from pulverized reagents and mixed manually. These were heated in the Pt melting pan, in air oven at temperature between 1000 and 1450oC for 12h. The occurrence of reaction with reagents and the products obtained were identified and structurally characterized by X-ray diffraction by polycrystalline sample. Mixtures of regents CaCO3, SrCO3, BaCO3, Fe2O3, Nb2O5, Have been made with various symmetries: a) Ba2Fe2O5, b) CaBaFe2O5, c) Ba2FeNbO6, d) Ca2Fe2O5, (e) Ba2Nb2O7, (f) Ca2Nb2O7, (g) Sr2Nb2O7, (h) CaBaFeNbO6. The products obtained showed that O2 of the air participated of reactions by providing the anions oxides required for obtaining the cubic phase. The formation of this phase was also helped by the presence of barium and niobium, since in the absence of these elements, can be seen the formation of orthorhombic phase, characteristic of Ca2Fe2O5.

scholarly journals X-ray Computed Tomography Method for Macroscopic Structural Property Evaluation of Active Twist Composite Blades

Aerospace ◽  
2021 ◽  
Vol 8 (12) ◽  
pp. 370
Author(s):  
Joon H. Ahn ◽  
Hyun J. Hwang ◽  
Sehoon Chang ◽  
Sung Nam Jung ◽  
Steffen Kalow ◽  
...  
Keyword(s):  
Computed Tomography ◽  
Structural Properties ◽  
Digital Image ◽  
Torsional Rigidity ◽  
Three Dimensional ◽  
Measured Data ◽  
X Ray ◽  
X Ray Computed ◽  
Active Twist ◽  
The Impact

This paper describes an evaluation of the structural properties of the next-generation active twist blade using X-ray computed tomography (CT) combined with digital image processing. This non-destructive testing technique avoids the costly demolition of the blade structure. The CT scan covers the whole blade region, including the root, transition, and tip regions, as well as the airfoil blade regions, in which there are spanwise variations in the interior structural layout due to the existence of heavy instrumentation. The three-dimensional digital image data are processed at selected radial stations, and finite element beam cross-section analyses are conducted to evaluate the structural properties of the blade at the macroscopic level. The fidelity of the digital blade model is first assessed by correlating the estimated blade mass with the measured data. A separate mechanical measurement is then carried out to determine the representative elastic properties of the blade and to verify the predicted results. The agreement is found to be good to excellent for the mass, elastic axis, flap bending, and torsional rigidity. The discrepancies are less than 2.0% for the mass and elastic axis locations, and about 8.1% for the blade stiffness properties, as compared with the measured data. Finally, a sensitivity analysis is conducted to clarify the impact of modeling the sensor and actuator cables, nose weight, and manufacturing imperfections on the structural properties of the blade.

scholarly journals Resolution extension by image summing in serial femtosecond crystallography of two-dimensional membrane-protein crystals

IUCrJ ◽  
2018 ◽  
Vol 5 (1) ◽  
pp. 103-117 ◽  
Author(s):  
Cecilia M. Casadei ◽  
Ching-Ju Tsai ◽  
Anton Barty ◽  
Mark S. Hunter ◽  
Nadia A. Zatsepin ◽  
...  
Keyword(s):  
Membrane Protein ◽  
Large Scale ◽  
Structural Changes ◽  
Signal To Noise Ratio ◽  
Three Dimensional ◽  
Single Layer ◽  
Protein Crystals ◽  
Single Shot ◽  
Two Dimensional ◽  
X Ray

Previous proof-of-concept measurements on single-layer two-dimensional membrane-protein crystals performed at X-ray free-electron lasers (FELs) have demonstrated that the collection of meaningful diffraction patterns, which is not possible at synchrotrons because of radiation-damage issues, is feasible. Here, the results obtained from the analysis of a thousand single-shot, room-temperature X-ray FEL diffraction images from two-dimensional crystals of a bacteriorhodopsin mutant are reported in detail. The high redundancy in the measurements boosts the intensity signal-to-noise ratio, so that the values of the diffracted intensities can be reliably determined down to the detector-edge resolution of 4 Å. The results show that two-dimensional serial crystallography at X-ray FELs is a suitable method to study membrane proteins to near-atomic length scales at ambient temperature. The method presented here can be extended to pump–probe studies of optically triggered structural changes on submillisecond timescales in two-dimensional crystals, which allow functionally relevant large-scale motions that may be quenched in three-dimensional crystals.

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