Structural information of long-chain fatty material obtained rapidly and conveniently by the use of X-ray diffraction studies of single crystals of urea and thiourea adducts

Bragg coherent X-ray diffraction imaging has become valuable for visualization of the structural, morphological and strain evolution of crystals in operando electrode materials. As the electrode material particles (either in a single-crystal form or an aggregation form of single crystals) are evenly dispersed and randomly oriented in the electrode laminate, the submicrometer-sized coherentX-ray beam can be used to probe the local properties of electrode material crystals using two approaches. Coherent multi-crystal diffraction provides collective structural information of phase transitions in tens of crystals simultaneously as well as the individual behavior from single crystals, which are oriented at the Bragg condition in the X-ray illumination volume. Bragg coherent diffractive imaging enables one to monitor the evolution of the morphology and strain in individual crystals. This work explores and highlights the Bragg coherent X-ray diffraction measurements of battery electrode materials in operando conditions at the 34-ID-C beamline at the Advanced Photon Source. The experiment is demonstrated with NaNi1/3Fe1/3Mn1/3O2, a sodium-ion cathode material loaded in a half cell. The paper will discuss, in detail, the beamline setup, sample mounting and handling, alignment strategies and the data acquisition protocols.

Download Full-text

X-Ray Diffraction from a 28 Attoliter Crystal Volume

Advances in X-ray Analysis ◽

10.1154/s0376030800009332 ◽

1991 ◽

Vol 35 (A) ◽

pp. 617-621

Author(s):

E.F. Skelton ◽

J.D. Ayers ◽

S.B. Qadri ◽

J.Z. Hu ◽

L.W. Finger ◽

...

Keyword(s):

Synchrotron Radiation ◽

Single Crystals ◽

Diffraction Data ◽

Structural Information ◽

Beam Line ◽

X Ray Diffraction ◽

Single Crystal Diffraction ◽

X Ray ◽

Diffraction Peaks ◽

Crystal Volume

AbstractMetallic filaments with sub-micrometer diameters have recently been fabricated using novel materials fabrication techniques at NRL. The specimens are enshrouded in a glass sheath and all efforts to obtain structural information from these samples with conventional x-ray sources have been negative. By using synchrotron radiation on a wiggler beam line, x-ray diffraction data have been obtained from samples with diameters of 0.22, 0.09, 0.07, and 0.04 μm. The two thicker samples were found to be single crystals with a structure consistent with that of normal Bi. Single crystal diffraction peaks obtained from the 0.07 μm sample are incompatible with the Bi-1 or any other known structure of Bi. We have provisionally identified this as Bi-X.

Download Full-text

Direct visualization of phase-separated domains in lipid membranes

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100082315 ◽

1978 ◽

Vol 36 (2) ◽

pp. 290-291

Author(s):

S. W. Hui ◽

T. P. Stewart

Keyword(s):

Lipid Membranes ◽

Structural Information ◽

Freeze Fracture ◽

Biological Molecules ◽

Vacuum Drying ◽

Direct Visualization ◽

X Ray Diffraction ◽

Electron Microscopic ◽

X Ray ◽

Hydrocarbon Chains

Direct electron microscopic study of biological molecules has been hampered by such factors as radiation damage, lack of contrast and vacuum drying. In certain cases, however, the difficulties may be overcome by using redundent structural information from repeating units and by various specimen preservation methods. With bilayers of phospholipids in which both the solid and fluid phases co-exist, the ordering of the hydrocarbon chains may be utilized to form diffraction contrast images. Domains of different molecular packings may be recgnizable by placing properly chosen filters in the diffraction plane. These domains would correspond to those observed by freeze fracture, if certain distinctive undulating patterns are associated with certain molecular packing, as suggested by X-ray diffraction studies. By using an environmental stage, we were able to directly observe these domains in bilayers of mixed phospholipids at various temperatures at which their phases change from misible to inmissible states.

Download Full-text

Characterizations of Synthetic 8mol% YSZ with Comparison to 3mol %YSZ for HT-SOFC

Engineering and Technology Journal ◽

10.30684/etj.v38i4a.351 ◽

2020 ◽

Vol 38 (4A) ◽

pp. 491-500

Author(s):

Abeer F. Al-Attar ◽

Saad B. H. Farid ◽

Fadhil A. Hashim

Keyword(s):

Ionic Conductivity ◽

Electrochemical Impedance ◽

Structural Information ◽

Impedance Analysis ◽

High Energy ◽

Yttria Stabilized Zirconia ◽

X Ray Diffraction ◽

Stabilized Zirconia ◽

Powder Morphology ◽

X Ray

In this work, Yttria (Y2O3) was successfully doped into tetragonal 3mol% yttria stabilized Zirconia (3YSZ) by high energy-mechanical milling to synthesize 8mol% yttria stabilized Zirconia (8YSZ) used as an electrolyte for high temperature solid oxide fuel cells (HT-SOFC). This work aims to evaluate the densification and ionic conductivity of the sintered electrolytes at 1650°C. The bulk density was measured according to ASTM C373-17. The powder morphology and the microstructure of the sintered electrolytes were analyzed via Field Emission Scanning Electron Microscopy (FESEM). The chemical analysis was obtained with Energy-dispersive X-ray spectroscopy (EDS). Also, X-ray diffraction (XRD) was used to obtain structural information of the starting materials and the sintered electrolytes. The ionic conductivity was obtained through electrochemical impedance spectroscopy (EIS) in the air as a function of temperatures at a frequency range of 100(mHz)-100(kHz). It is found that the 3YSZ has a higher density than the 8YSZ. The impedance analysis showed that the ionic conductivity of the prepared 8YSZ at 800°C is0.906 (S.cm) and it was 0.214(S.cm) of the 3YSZ. Besides, 8YSZ has a lower activation energy 0.774(eV) than that of the 3YSZ 0.901(eV). Thus, the prepared 8YSZ can be nominated as an electrolyte for the HT-SOFC.

Download Full-text

Effect of trytophan as dopant on potassium acid phthalate single crystals

10.31221/osf.io/cn28k ◽

2019 ◽

Author(s):

Chem Int

Keyword(s):

Single Crystals ◽

Room Temperature ◽

Visible Region ◽

X Ray Diffraction ◽

X Ray ◽

Slow Evaporation Technique ◽

Absorption Studies ◽

Evaporation Technique ◽

Potassium Acid Phthalate ◽

Acid Phthalate

Optically transparent single crystals of potassium acid phthalate (KAP, 0.5 g) 0.05 g and 0.1 g (1 and 2 mol %) trytophan were grown in aqueous solution by slow evaporation technique at room temperature. Single crystal X- ray diffraction analysis confirmed the changes in the lattice parameters of the doped crystals. The presence of functional groups in the crystal lattice has been determined qualitatively by FTIR analysis. Optical absorption studies revealed that the doped crystals possess very low absorption in the entire visible region. The dielectric constant has been studied as a function of frequency for the doped crystals. The thermal stability was evaluated by TG-DSC analysis.

Download Full-text

Some Novel Cobalt Diphenylphosphine Complexes: Synthesis, Characterization, and Behavior in the Polymerization of 1,3-Butadiene

Molecules ◽

10.3390/molecules26134067 ◽

2021 ◽

Vol 26 (13) ◽

pp. 4067

Author(s):

Giovanni Ricci ◽

Giuseppe Leone ◽

Giorgia Zanchin ◽

Benedetta Palucci ◽

Alessandra Forni ◽

...

Keyword(s):

Crystal Structure ◽

Single Crystals ◽

The Novel ◽

X Ray Diffraction ◽

X Ray ◽

And Behavior

Some novel cobalt diphenylphosphine complexes were synthesized by reacting cobalt(II) chloride with (2-methoxyethyl)diphenylphosphine, (2-methoxyphenyl)diphenylphosphine, and 2-(1,1-dimethylpropyl)-6-(diphenylphosphino)pyridine. Single crystals suitable for X-ray diffraction studies were obtained for the first two complexes, and their crystal structure was determined. The novel compounds were then used in association with methylaluminoxane (MAO) for the polymerization of 1,3-butadiene, and their behavior was compared with that exhibited in the polymerization of the same monomer by the systems CoCl2(PnPrPh2)2/MAO and CoCl2(PPh3)2/MAO. Some significant differences were observed depending on the MAO/Co ratio used, and a plausible interpretation for such a different behavior is proposed.

Download Full-text

Growth of sillenite Bi12FeO20 single crystals: structural, thermal, optical, photocatalytic features and first principle calculations

Scientific Reports ◽

10.1038/s41598-020-78598-3 ◽

2020 ◽

Vol 10 (1) ◽

Author(s):

Durga Sankar Vavilapalli ◽

Ambrose A. Melvin ◽

F. Bellarmine ◽

Ramanjaneyulu Mannam ◽

Srihari Velaga ◽

...

Keyword(s):

Single Crystal ◽

Single Crystals ◽

Photoelectron Spectroscopy ◽

Diffraction Method ◽

Lattice Parameter ◽

First Principle ◽

X Ray Diffraction ◽

X Ray ◽

First Principle Calculations ◽

Photodegradation Efficiency

AbstractIdeal sillenite type Bi12FeO20 (BFO) micron sized single crystals have been successfully grown via inexpensive hydrothermal method. The refined single crystal X-ray diffraction data reveals cubic Bi12FeO20 structure with single crystal parameters. Occurrence of rare Fe4+ state is identified via X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS). The lattice parameter (a) and corresponding molar volume (Vm) of Bi12FeO20 have been measured in the temperature range of 30–700 °C by the X-ray diffraction method. The thermal expansion coefficient (α) 3.93 × 10–5 K−1 was calculated from the measured values of the parameters. Electronic structure and density of states are investigated by first principle calculations. Photoelectrochemical measurements on single crystals with bandgap of 2 eV reveal significant photo response. The photoactivity of as grown crystals were further investigated by degrading organic effluents such as Methylene blue (MB) and Congo red (CR) under natural sunlight. BFO showed photodegradation efficiency about 74.23% and 32.10% for degrading MB and CR respectively. Interesting morphology and microstructure of pointed spearhead like BFO crystals provide a new insight in designing and synthesizing multifunctional single crystals.

Download Full-text

Modeling of magneto-conductivity of bismuth selenide: a topological insulator

SN Applied Sciences ◽

10.1007/s42452-021-04397-8 ◽

2021 ◽

Vol 3 (4) ◽

Author(s):

Yogesh Kumar ◽

Rabia Sultana ◽

Prince Sharma ◽

V. P. S. Awana

Keyword(s):

Magnetic Field ◽

Magnetic Fields ◽

Single Crystal ◽

Single Crystals ◽

X Ray Diffraction ◽

Field Range ◽

X Ray ◽

Bulk Carriers ◽

Different Temperatures

AbstractWe report the magneto-conductivity analysis of Bi2Se3 single crystal at different temperatures in a magnetic field range of ± 14 T. The single crystals are grown by the self-flux method and characterized through X-ray diffraction, Scanning Electron Microscopy, and Raman Spectroscopy. The single crystals show magnetoresistance (MR%) of around 380% at a magnetic field of 14 T and a temperature of 5 K. The Hikami–Larkin–Nagaoka (HLN) equation has been used to fit the magneto-conductivity (MC) data. However, the HLN fitted curve deviates at higher magnetic fields above 1 T, suggesting that the role of surface-driven conductivity suppresses with an increasing magnetic field. This article proposes a speculative model comprising of surface-driven HLN and added quantum diffusive and bulk carriers-driven classical terms. The model successfully explains the MC of the Bi2Se3 single crystal at various temperatures (5–200 K) and applied magnetic fields (up to 14 T).

Download Full-text

Crystallization and preliminary X-ray analysis of thePlasmodium falciparumapicoplast DNA polymerase

Acta Crystallographica Section F Structural Biology Communications ◽

10.1107/s2053230x15002423 ◽

2015 ◽

Vol 71 (3) ◽

pp. 333-337 ◽

Cited By ~ 2

Author(s):

Morgan E. Milton ◽

Jun-yong Choe ◽

Richard B. Honzatko ◽

Scott W. Nelson

Keyword(s):

Dna Polymerase ◽

Structural Information ◽

Klenow Fragment ◽

X Ray Diffraction ◽

Dna Polymerase I ◽

X Ray ◽

Cell Parameters ◽

A Genome ◽

Reported Data ◽

Polymerase I

Infection by the parasitePlasmodium falciparumis the leading cause of malaria in humans. The parasite has a unique and essential plastid-like organelle called the apicoplast. The apicoplast contains a genome that undergoes replication and repair through the action of a replicative polymerase (apPOL). apPOL has no direct orthologs in mammalian polymerases and is therefore an attractive antimalarial drug target. No structural information exists for apPOL, and the Klenow fragment ofEscherichia coliDNA polymerase I, which is its closest structural homolog, shares only 28% sequence identity. Here, conditions for the crystallization of and preliminary X-ray diffraction data from crystals ofP. falciparumapPOL are reported. Data complete to 3.5 Å resolution were collected from a single crystal (2 × 2 × 5 µm) using a 5 µm beam. The space groupP6522 (unit-cell parametersa=b= 141.8,c= 149.7 Å, α = β = 90, γ = 120°) was confirmed by molecular replacement. Refinement is in progress.

Download Full-text