scholarly journals X-ray diffraction using focused-ion-beam-prepared single crystals

2020 ◽  
Vol 53 (3) ◽  
pp. 614-622
Author(s):  
Tina Weigel ◽  
Claudia Funke ◽  
Matthias Zschornak ◽  
Thomas Behm ◽  
Hartmut Stöcker ◽  
...  
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Preparation Technique ◽  
X Rays ◽  
X Ray Diffraction ◽  
Electron Densities ◽  
X Ray ◽  
Absorption Correction

High-quality single-crystal X-ray diffraction measurements are a prerequisite for obtaining precise and reliable structure data and electron densities. The single crystal should therefore fulfill several conditions, of which a regular defined shape is of particularly high importance for compounds consisting of heavy elements with high X-ray absorption coefficients. The absorption of X-rays passing through a 50 µm-thick LiNbO3 crystal can reduce the transmission of Mo Kα radiation by several tens of percent, which makes an absorption correction of the reflection intensities necessary. In order to reduce ambiguities concerning the shape of a crystal, used for the necessary absorption correction, a method for preparation of regularly shaped single crystals out of large samples is presented and evaluated. This method utilizes a focused ion beam to cut crystals with defined size and shape reproducibly and carefully without splintering. For evaluation, a single-crystal X-ray diffraction study using a laboratory diffractometer is presented, comparing differently prepared LiNbO3 crystals originating from the same macroscopic crystal plate. Results of the data reduction, structure refinement and electron density reconstruction indicate qualitatively similar values for all prepared crystals. Thus, the different preparation techniques have a smaller impact than expected. However, the atomic coordinates, electron densities and atomic charges are supposed to be more reliable since the focused-ion-beam-prepared crystal exhibits the smallest extinction influences. This preparation technique is especially recommended for susceptible samples, for cases where a minimal invasive preparation procedure is needed, and for the preparation of crystals from specific areas, complex material architectures and materials that cannot be prepared with common methods (breaking or grinding).

Extraction of plutonium-containing microcrystals from Hanford soil using a focused ion beam for single-crystal X-ray diffraction analysis

2019 ◽  
Vol 52 (6) ◽  
pp. 1244-1252 ◽  
Author(s):  
Jordan F. Corbey ◽  
Dallas D. Reilly ◽  
Lucas E. Sweet ◽  
Timothy G. Lach
Keyword(s):  
Single Crystal ◽  
Diffraction Analysis ◽  
Focused Ion Beam ◽  
Crystal Size ◽  
Ion Beam ◽  
X Ray Diffraction ◽  
Charge Coupled Device ◽  
X Ray ◽  
Size Limits ◽  
A Charge

Herein, the successful use of a focused ion beam/scanning electron microscope to prepare microsamples of radioactive single crystals for X-ray diffraction analysis is reported. This technique was used to extract and analyze crystalline Pu-containing particles as small as 28 µm3 from Hanford soil taken from the 216-Z-9 waste crib, which were then crystallographically characterized using single-crystal X-ray diffraction to confirm the cubic structure of PuO2. As a systematic proof of concept, the technique was first tested using UO2 crystals milled into cubic shapes with approximate volumes of 4620, 1331, 125, 8 and 1 µm3, in order to empirically determine the crystal size limits for characterization by a laboratory-based diffractometer with a sealed tube Mo or Ag anode X-ray source and a charge-coupled device detector.

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

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.

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

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).

Characterization of Natural and Synthesized FeTiO3 Crystals With RBS/PIXE/XRD

1997 ◽  
Vol 07 (03n04) ◽  
pp. 265-275
Author(s):  
R. Q. Zhang ◽  
S. Yamamoto ◽  
Z. N. Dai ◽  
K. Narumi ◽  
A. Miyashita ◽  
...  
Keyword(s):  
Single Crystals ◽  
Ion Beam ◽  
Pressure Control ◽  
Floating Zone ◽  
X Ray Diffraction ◽  
X Ray ◽  
Beam Analysis ◽  
Ppm Level

Natural FeTiO 3 (illuminate) and synthesized FeTiO 3, single crystals were characterized by Rutherford backscattering spectroscopy combined with channeling technique and particle-induced x-ray emission (RBS-C and PIXE). The results obtained by the ion beam analysis were supplemented by the x-ray diffraction analysis to identify the crystallographic phase. Oriented single crystals of synthesized FeTiO 3 were grown under the pressure control of CO 2 and H 2 mixture gas using a single-crystal floating zone technique. The crystal quality of synthesized FeTiO 3 single crystals could be improved by the thermal treatment but the exact pressure control is needed to avoid the precipitation of Fe 2 O 3 even during the annealing procedure. Natural FeTiO 3 contains several kinds of impurities such as Mn , Mg , Na and Si . The synthesized samples contain Al , Si and Na which are around 100 ppm level as impurities. The PBS-C results of the natural sample imply that Mn impurities occupy the Fe sublattice in FeTiO 3 or in mixed phase between ilmenite and hematite.

Oxidation of Alloy-X in Subcritical, Transition, and Supercritical Water

CORROSION ◽  
10.5006/3881 ◽  
2021 ◽  
Author(s):  
Zachary Karmiol ◽  
Dev Chidambaram
Keyword(s):  
Supercritical Water ◽  
Photoelectron Spectroscopy ◽  
Focused Ion Beam ◽  
Elevated Temperatures ◽  
Subcritical Water ◽  
Ion Beam ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nickel Based Superalloy ◽  
Before And After

This work investigates the oxidation of a nickel based superalloy, namely Alloy X, in water at elevated temperatures: subcritical water at 261°C and 27 MPa, the transition between subcritical and supercritical water at 374°C and 27 MPa, and supercritical water at 380°C and 27 MPa for 100 hours. The morphology of the sample surfaces were studied using scanning electron microscopy coupled with focused ion beam milling, and the surface chemistry was investigated using X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy before and after exposure studies. Surfaces of all samples were identified to comprise of a ferrite spinel containing aluminum.

scholarly journals Rubidium tetrafluoridobromate(III): redetermination of the crystal structure from single-crystal X-ray diffraction data

IUCrData ◽  
2019 ◽  
Vol 4 (11) ◽  
Author(s):  
Artem V. Malin ◽  
Sergei I. Ivlev ◽  
Roman V. Ostvald ◽  
Florian Kraus
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
Structure Type ◽  
X Ray Diffraction ◽  
X Ray ◽  
Square Planar ◽  
Atomic Coordinates

Single crystals of rubidium tetrafluoridobromate(III), RbBrF4, were grown by melting and recrystallizing RbBrF4 from its melt. This is the first determination of the crystal structure of RbBrF4 using single-crystal X-ray diffraction data. We confirmed that the structure contains square-planar [BrF4]− anions and rubidium cations that are coordinated by F atoms in a square-antiprismatic manner. The compound crystallizes in the KBrF4 structure type. Atomic coordinates and bond lengths and angles were determined with higher precision than in a previous report based on powder X-ray diffraction data [Ivlev et al. (2015). Z. Anorg. Allg. Chem. 641, 2593–2598].

Crystallinity of YBa2Cu3O7−x single crystals grown by the pulling method

1996 ◽  
Vol 11 (4) ◽  
pp. 804-812 ◽  
Author(s):  
Y. Namikawa ◽  
M. Egami ◽  
S. Koyama ◽  
Y. Shiohara ◽  
H. Kutami
Keyword(s):  
Single Crystal ◽  
Single Crystals ◽  
Growth Direction ◽  
Annealed Sample ◽  
Seed Crystal ◽  
X Ray Diffraction ◽  
Rocking Curve ◽  
X Ray ◽  
Crystal Seed ◽  
Better Than

Large YBa2Cu3O7−x (Y123) single crystals (larger than 13 mm cubed) have been grown along the c-axis reproducibly by the modified pulling method. The crystallinity of Y123 single crystal was investigated by x-ray diffraction and x-ray topography. Crystals grown from an MgO single crystal seed had some low angle subgrain boundaries which tilted 0.1–0.8° from each other. These grain boundaries originated from the seed crystal, and the subgrains were extended along the growth direction from the seed crystal. Y123 single crystals with no marked subgrains in the whole area were obtained by using Y123 single subgrain crystal seeds. FWHM of the x-ray rocking curve for the crystal so produced was about 0.14°, which was much better than the spectrum consisting of several separated peaks obtained from the previous crystals. Tc onset of the annealed sample was about 93.6 K, and the transition width was about 0.9 K. The low angle subgrain boundaries did not seem to be effective pinning centers for the magnetic flux.

Refinement of the layered titanosilicate AM-1 from single-crystal X-ray diffraction data

2007 ◽  
Vol 63 (11) ◽  
pp. i186-i186 ◽  
Author(s):  
Stanislav Ferdov ◽  
Uwe Kolitsch ◽  
Christian Lengauer ◽  
Ekkehart Tillmanns ◽  
Zhi Lin ◽  
...  
Keyword(s):  
Raman Spectroscopy ◽  
Hydrogen Bonding ◽  
Single Crystal ◽  
Single Crystals ◽  
Diffraction Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
First Time ◽  
Ir And Raman ◽  
Bonding Scheme

The structure of the layered noncentrosymmetric titanosilicate AM-1 (also known as JDF-L1, disodium titanium tetrasilicate dihydrate), Na4Ti2Si8O22·4H2O, grown as small single crystals without the use of organics, has been refined from single-crystal X-ray diffraction data. The H atom has been located for the first time, and the hydrogen-bonding scheme is also characterized by IR and Raman spectroscopy. All atoms are in general positions except for the Na, the Ti, one Ti-bound O, one Si-bound O and the water O atoms (site symmetries 2, 4, 4, 2 and 2, respectively).

scholarly journals Crystal structure, homogeneity range and electronic structure of rhombohedral γ-Mn5Al8

2017 ◽  
Vol 232 (7-9) ◽  
Author(s):  
Srinivasa Thimmaiah ◽  
Zachary Tener ◽  
Tej N. Lamichhane ◽  
Paul C. Canfield ◽  
Gordon J. Miller
Keyword(s):  
Crystal Structure ◽  
Phase Diagram ◽  
Electronic Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Homogeneity Range ◽  
X Ray Diffraction ◽  
X Ray ◽  
Eds Analysis

AbstractThe γ-region of the Mn–Al phase diagram between 45 and 70 at.% Al was re-investigated by a combination of powder and single crystal X-ray diffraction as well as EDS analysis to establish the distribution of Mn and Al atoms. Single crystals of γ-Mn

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