scholarly journals Microstructural characterization of polycrystalline materials using a X-ray single-crystal diffractometer equipped with an area detector

2011 ◽  
Vol 67 (a1) ◽  
pp. C671-C671
Author(s):  
A. B. Rodríguez-Navarro ◽  
P. Alvarez-Lloret
2007 ◽  
Vol 40 (3) ◽  
pp. 631-634 ◽  
Author(s):  
Alejandro B. Rodriguez-Navarro

The orientation of crystals in a polycrystalline sample is adequately described using pole figures, displaying the three-dimensional distribution of specific crystallographic directions or poles. Registration of pole figures is necessary to characterize the preferred orientation of crystals and its influence on the anisotropy of properties in textured materials. It is also useful to understand the development of highly organized microstructures in polycrystalline materials. Pole figures can be registered efficiently using an area detector, available at most modern single-crystal diffractometers. This paper describes in detail the procedure of data collection and processing of pole figures using a single-crystal diffractometer equipped with an area detector. Specifically, a Bruker SMART APEX diffractometer was used, but this methodology can be readily adapted to other diffractometers.


2000 ◽  
Vol 33 (2) ◽  
pp. 226-233 ◽  
Author(s):  
Y. Kudo ◽  
K.-Y. Liu ◽  
S. Kawado ◽  
K. Hirano

Variations in lattice plane spacing and lattice plane orientation,i.e.Δd/dand Δα, reflect variations in lattice distortion in a single crystal. Double-crystal X-ray topography (DCT) using synchrotron radiation can be used to measure Δd/dand Δα of a silicon single crystal. However, both Δd/dand Δα measured using DCT are always overlapped by extrinsic components, showing particular long-range variations. The extrinsic components should be eliminated from the measured Δd/dand Δα for quantitative characterization of silicon single crystals. A sample-rotation and area-detector-traverse (RT) method, applicable to X-ray optics for DCT, has been newly developed. The extrinsic components are eliminated by modification of the intensity distribution on the X-ray topographs using the RT method. From theoretical considerations, it is confirmed that the extrinsic components are mainly due to the (+,−) non-parallel setting between the monochromator and the collimator, and a minute bend in the sample due to its physical restraint.


2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.


2014 ◽  
Vol 805 ◽  
pp. 343-349
Author(s):  
Carine F. Machado ◽  
Weber G. Moravia

This work evaluated the influence of additions of the ceramic shell residue (CSR), from the industries of Lost Wax Casting, in the modulus of elasticity and porosity of concrete. The CSR was ground and underwent a physical, chemical, and microstructural characterization. It was also analyzed, the environmental risk of the residue. In the physical characterization of the residue were analyzed, the surface area, and particle size distribution. In chemical characterization, the material powder was subjected to testing of X-ray fluorescence (XRF). Microstructural characterization was performed by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The residue was utilized like addition by substitution of cement in concrete in the percentages of 10% and 15% by weight of Portland cement. It was evaluated properties of concrete in the fresh and hardened state, such as compressive strength, modulus of elasticity, absorption of water by total immersion and by capillarity. The results showed that the residue can be used in cement matrix and improve some properties of concrete. Thus, the CSR may contribute to improved sustainability and benefit the construction industry.


1993 ◽  
Vol 115 (22) ◽  
pp. 10392-10393 ◽  
Author(s):  
Alain Penicaud ◽  
Aaron Perez-Benitez ◽  
R. Gleason V. ◽  
E. Munoz P. ◽  
R. Escudero
Keyword(s):  

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.


Author(s):  
Filip Topić ◽  
Joseph M. Marrett ◽  
Tristan H. Borchers ◽  
Hatem M. Titi ◽  
Christopher J. Barrett ◽  
...  

Inorganics ◽  
2018 ◽  
Vol 6 (3) ◽  
pp. 97 ◽  
Author(s):  
Marie Gaschard ◽  
Farzaneh Nehzat ◽  
Thomas Cheminel ◽  
Bruno Therrien

The synthesis and characterization of three metalla-rectangles of the general formula [Ru4(η6-p-cymene)4(μ4-clip)2(μ2-Lanthr)2][CF3SO3]4 (Lanthr: 9,10-bis(3,3’-ethynylpyridyl) anthracene; clip = oxa: oxalato; dobq: 2,5-dioxido-1,4-benzoquinonato; donq: 5,8-dioxido-1,4-naphthoquinonato) are presented. The molecular structure of the metalla-rectangle [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2]4+ has been confirmed by the single-crystal X-ray structure analysis of [Ru4(η6-p-cymene)4(μ4-oxa)2(μ2-Lanthr)2][CF3SO3]4 · 4 acetone (A2 · 4 acetone), thus showing the anthracene moieties to be available for reaction with oxygen. While the formation of the endoperoxide form of Lanthr was observed in solution upon white light irradiation, the same reaction does not occur when Lanthr is part of the metalla-assemblies.


2017 ◽  
Vol 46 (40) ◽  
pp. 14012-14020
Author(s):  
Kazuhiro Uemura ◽  
Masahiro Taoka

An intermediate compound of a tetranuclear Pt–Fe⋯Fe–Pt complex in the synthetic process to form a trinuclear Pt–Fe–Pt complex by mixing the “amidate-hanging” Pt mononuclear complex and iron sources was successfully isolated and characterized by single-crystal X-ray analysis and several physical measurements.


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