X-Ray Diffraction for Nondestructive Characterization of Polycrystalline Materials

1988 ◽  
Vol 142 ◽  
Author(s):  
C. O. Ruud ◽  
S. D. Weedman
Keyword(s):  
Computer Control ◽  
Polycrystalline Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Position Sensitive ◽  
Computer Controlled ◽  
Xrd Techniques ◽  
Nondestructive Characterization

AbstractX-ray diffraction has long been the mainstay for materials characterization in the laboratory. This characterization includes the determination of phase composition, residual stress, microstrain, grain size, and crystallographic texture of polycrystalline metals, ceramics, and minerals. The analytical capabilities of XRD techniques have been expanded recently by the application of computer control to data collection and processing. These capabilities include the identification of irregularities in metals and ceramics that are caused by processing and fatigue damage, as well as the apriori prediction of processing anomolies. While the above applications have been largely restricted to the laboratory, the possibility for exploitation of the nondestructive nature of x-ray diffraction for inprocess evaluation of materials is now being realized. The availability of computer-controlled position-sensitive x-ray detectors can now provide rapid, non-contacting, in-process interrogation of materials. The examples of nondestructive characterization illustrated in this paper will be those that can be used for process control and/or damage assessment.

New Coordination Compounds of Fe(III) with Organic Ligands

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  
Keyword(s):  
Chemical Analysis ◽  
Complex Compounds ◽  
Organic Ligands ◽  
X Ray Diffraction ◽  
X Ray ◽  
Elemental Chemical Analysis ◽  
Structural Formulae ◽  
Paramagnetic Properties

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.

One Step Synthesis and Characterization of Zirconia-Graphene Composites

2012 ◽  
Vol 600 ◽  
pp. 174-177 ◽  
Author(s):  
Jian Fei Xia ◽  
Zong Hua Wang ◽  
Yan Zhi Xia ◽  
Fei Fei Zhang ◽  
Fu Qiang Zhu ◽  
...  
Keyword(s):  
Synthesis And Characterization ◽  
Two Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Graphene Composite ◽  
Transmission Electron ◽  
One Step ◽  
Ft Ir ◽  
Xrd Techniques

Zirconia-graphene composite (ZrO2-G) has been successfully synthesized via decomposition of ZrOCl2•6H2O in a water-isopropanol system with dispersed graphene oxide (GO) utilizing Na2S as a precursor could enable the occurrence of the deposition of Zr4+ and the deoxygenation of GO at the same time. Transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD) techniques were used to characterize the samples. It was found that graphene were fully coated with ZrO2, and the ZrO2 existing in tetragonal phase, which resulted in the formation of two-dimensional composite.

Micro Diffraction Imaging of Bulk Polycrystalline Materials

2006 ◽  
Vol 524-525 ◽  
pp. 273-278
Author(s):  
Thomas Wroblewski ◽  
A. Bjeoumikhov ◽  
Bernd Hasse
Keyword(s):  
High Spatial Resolution ◽  
Polycrystalline Materials ◽  
X Rays ◽  
X Ray Diffraction ◽  
Short Sample ◽  
X Ray ◽  
Detector Distance ◽  
Transmission Geometry ◽  
Diffraction Imaging ◽  
Position Sensitive

X-ray diffraction imaging applies an array of parallel capillaries in front of a position sensitive detector. Conventional micro channel plates of a few millimetre thickness have successfully been used as collimator arrays but require short sample to detector distances to achieve high spatial resolution. Furthermore, their limited absorption restricts their applications to low energy X-rays of around 10 keV. Progress in the fabrication of long polycapillaries allows an increase in the sample to detector distance without decreasing resolution and the use of high X-ray energies enables bulk investigations in transmission geometry.

Computer Controlled X-Ray Diffraction Measurement of Residual Stress

1972 ◽  
Vol 16 ◽  
pp. 344-353 ◽  
Author(s):  
Carol J. Kelly ◽  
E. Eichen
Keyword(s):  
Residual Stress ◽  
Computer Control ◽  
Sample Surface ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
X Ray ◽  
Intensity Measurements ◽  
On Line ◽  
Computer Controlled ◽  
The Difference

AbstractThe system to be described includes hardware and software for the on-line computer control of the X-ray diffraction measurement of residual stress. This determination involves accurately measuring the angles at which a back-reflection line is diffracted, first by diffracting planes parallel to the sample surface, and then by planes at an angle (ψ) to the sample surface. The residual stress is calculated from the difference in the two measured diffraetion angles. The procedure executed by the computer consists of locating the peaks, selecting three angles for collection of X-ray counts, correcting the measured counts, fitting the equi-angular intensity measurements to a three-point parabola, calculating the peak angles, calculating the residual stress from the measured angles and typing a report. This automation has eliminated the tedium of the manual X-ray data accumulation and of the residual stress calculation. The online control has also permitted improvements in the technique not practicable with the manually performed measurement of residual stress.

Synthesis and Structural Characterization of Ca14NbxIn1-xAs11 (x ≈ 0.85)

2016 ◽  
Vol 257 ◽  
pp. 147-151 ◽  
Author(s):  
Yi Wang ◽  
Svilen Bobev
Keyword(s):  
Physical Properties ◽  
Side Reaction ◽  
Structure Type ◽  
Major Product ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ongoing Work ◽  
Set Up

Single-crystals of the new compound Ca14NbxIn1–xAs11 have been obtained from a solid-state reaction in a sealed Nb ampoule. The initial experiment had been set up with the aim to investigate the effect of electron doping (via In) on the crystal structure and physical properties of Ca14MnAs11. Subsequent single-crystal X-ray diffraction and elemental analysis work suggested that instead of Ca14MnxIn1–xAs11, the major product of the reaction is the phase Ca14NbxIn1–xAs11. This supposition was corroborated when the title compound was synthesized from a reaction of Ca, In and As in a sealed Nb ampoule, proving that, 1) Mn metal is not included in the structure, and 2) that the inadvertent side reaction of As with the walls of the Nb container is the source of the niobium. The overall structure is isotypic with the tetragonal Ca14AlSb11 structure type (space group I41/acd), although some marked differences between the two must be noted. Current ongoing work is focused on the synthesis of phase pure polycrystalline samples and determination of the physical properties of this unusual transition metal Zintl phase.

Second Order Stresses Distribution in Textured Copper

2006 ◽  
Vol 524-525 ◽  
pp. 859-864
Author(s):  
Neila Hfaiedh ◽  
Manuel François ◽  
Khemais Saanouni
Keyword(s):  
Peak Position ◽  
Second Order ◽  
Polycrystalline Materials ◽  
Internal Stresses ◽  
Plastic Strains ◽  
Sensitive Detector ◽  
X Ray Diffraction ◽  
X Ray ◽  
Position Sensitive ◽  
Specific Correction

Internal stresses are an important factor in understanding the work hardening behaviour of polycrystalline materials. The goal of the present paper is to study the development of second order stresses in textured copper sheets at large plastic strains, up to fracture by X-ray diffraction. Second order stresses manifest themselves as peak displacements and width changes as azimuth and tilt angles are varied. As the acquisition is performed with a position sensitive detector, a specific correction of intensities is required in order to take into account texture influence on peak shape and consequently on peak position and width.

Preparation and Characterization of PCL/PVP Blend Membrane

2011 ◽  
Vol 311-313 ◽  
pp. 1638-1641
Author(s):  
Jun Hua Wang ◽  
Xiang Biao Cheng ◽  
Gang Huang ◽  
Feng Chun Dong ◽  
Yong Tang Jia
Keyword(s):  
Mechanical Property ◽  
Membrane Structure ◽  
Solution Method ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Blend Membrane ◽  
X Ray ◽  
Structure And Morphology ◽  
Xrd Techniques

PCL/PVP blend membrane was prepared by casting solution method. Scanning electron microscopy (SEM), diffraction scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques were employed to characterize membrane structure and morphology. Moreover, the hydrophilicity, mechanical property and biodegradability of membranes were investigated. Due to introducing PVP, the crystallinity and mechanical property of PCL altered to some extent. The hydrophilicity of the blend membrane improved remarkably with increasing PVP content, which was expressed by the contact angle declining and the rate of water absorption increasing. Lipase accelerated the degradation rate of PCL/PVP membrane.

Characterization of Nanocrystalline γ–Fe2O3Prepared by Wet Chemical Method

1999 ◽  
Vol 14 (4) ◽  
pp. 1570-1575 ◽  
Author(s):  
G. Ennas ◽  
G. Marongiu ◽  
A. Musinu ◽  
A. Falqui ◽  
P. Ballirano ◽  
...  
Keyword(s):  
Isothermal Treatment ◽  
X Ray Diffraction ◽  
Ferrous Chloride ◽  
Scanning Calorimetry ◽  
Direct Transformation ◽  
X Ray ◽  
Transmission Electron ◽  
Xrd Techniques ◽  
Kinetics Of

Homogeneous maghemite (γ–Fe2O3) nanoparticles with an average crystal size around 5 nm were synthesized by successive hydrolysis, oxidation, and dehydration of tetrapyridino-ferrous chloride. Morphological, thermal, and structural properties were investigated by transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD) techniques. Rietveld refinement indicated a cubic cell. The superstructure reflections, related to the ordering of cation lattice vacancies, were not detected in the diffraction pattern. Kinetics of the solid-state phase transition of nanocrystalline maghemite to hematite (α–Fe2O3), investigated by energy dispersive x-ray diffraction (EDXRD), indicates that direct transformation from nanocrystalline maghemite to microcrystalline hematite takes place during isothermal treatment at 385 °C. This temperature is lower than that observed both for microcrystalline maghemite and for nanocrystalline maghemite supported on silica.

Instrumental aspects in X-ray diffraction on polycrystalline materials

2005 ◽  
Vol 20 (4) ◽  
pp. 294-305 ◽  
Author(s):  
R. Guinebretière ◽  
A. Boulle ◽  
O. Masson ◽  
A. Dauger
Keyword(s):  
Polycrystalline Materials ◽  
Acquisition Time ◽  
X Ray Diffraction ◽  
X Ray ◽  
Experimental Parameters ◽  
Recent Developments ◽  
Instrumental Resolution ◽  
Position Sensitive ◽  
Two Parameters ◽  
Position Sensitive Detectors

The purpose of this paper is to give a rapid overview of the recent developments in the field of X-ray diffraction on polycrystalline materials from the viewpoint of the instruments. After a brief historical report, the main types of laboratory diffractometers are presented. At the end of the twentieth century the apparition of position sensitive detectors and artificial crystal monochromators have induced the conception of new diffractometer often based on old geometrical arrangements. Those modern diffractometers are described with respect to the more conventional ones. Among the experimental parameters which can characterize a given diffractometer, the instrumental resolution function and the acquisition time of the pattern are of primary importance. The different apparatus are compared with respect to those two parameters.

Synthesis, Phase Formation and Characterization of Co4Nb2O9 Powders Synthesized by Solid-State Reaction

2008 ◽  
Vol 55-57 ◽  
pp. 873-876 ◽  
Author(s):  
N. Chaiyo ◽  
R. Muanghlua ◽  
A. Ruangphanit ◽  
Wanwilai C. Vittayakorn ◽  
Naratip Vittayakorn
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Solid State Reaction ◽  
Dwell Time ◽  
Single Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Xrd Techniques ◽  
Scanning Electron

A corundum-type structure of cobalt niobate (Co4Nb2O9) has been synthesized by a solid-state reaction. The formation of the Co4Nb2O9 phase in the calcined powders was investigated as a function of calcination conditions by differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. Morphology and particle size have been determined by scanning electron microscopy (SEM). It was found that the minor phases of unreacted Co3O4 tend to form together with the columbite CoNb2O6 phase at a low calcination temperature and short dwell time. It seems that the single-phase of Co4Nb2O9 in a corundum phase can be obtained successfully at the calcination conditions of 900°C for 60 min, with heating/cooling rates of 20°C /min.

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