X-ray diffraction contrast tomography: a novel technique for three-dimensional grain mapping of polycrystals. II. The combined case

2008 ◽  
Vol 41 (2) ◽  
pp. 310-318 ◽  
Author(s):  
Greg Johnson ◽  
Andrew King ◽  
Marcelo Goncalves Honnicke ◽  
J. Marrow ◽  
Wolfgang Ludwig
Keyword(s):  
Electron Backscatter Diffraction ◽  
Three Dimensional ◽  
Real Data ◽  
X Ray Diffraction ◽  
Data Set ◽  
Transmitted Beam ◽  
X Ray ◽  
Diffraction Contrast ◽  
Simultaneous Acquisition ◽  
Backscatter Diffraction

By simultaneous acquisition of the transmitted and the diffracted beams, the applicability of the previously introduced diffraction contrast tomography technique [Ludwig, Schmidt, Lauridsen & Poulsen (2008).J. Appl. Cryst.41, 302–309] can be extended to the case of undeformed polycrystalline samples containing more than 100 grains per cross section. The grains are still imaged using the occasionally occurring diffraction contribution to the X-ray attenuation coefficient, which can be observed as a reduction in the intensity of the transmitted beam when a grain fulfils the diffraction condition. Automating the segmentation of the extinction spot images is possible with the additional diffracted beam information, even in the presence of significant spot overlap. By pairing the corresponding direct (`extinction') and diffracted beam spots a robust sorting and indexing approach has been implemented. The analysis procedure is illustrated on a real data set and the result is validated by comparison with a two-dimensional grain map obtained by electron backscatter diffraction.

scholarly journals Stable and Metastable Phase Equilibria Involving the Cu6Sn5 Intermetallic

2021 ◽  
Author(s):  
A. Leineweber ◽  
M. Löffler ◽  
S. Martin
Keyword(s):  
Phase Equilibria ◽  
Electron Backscatter Diffraction ◽  
Metastable Phase ◽  
Stable Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Heat Treated ◽  
Ordered Phases ◽  
Backscatter Diffraction ◽  
Kinetics Of

Abstract Cu6Sn5 intermetallic occurs in the form of differently ordered phases η, η′ and η′′. In solder joints, this intermetallic can undergo changes in composition and the state of order without or while interacting with excess Cu and excess Sn in the system, potentially giving rise to detrimental changes in the mechanical properties of the solder. In order to study such processes in fundamental detail and to get more detailed information about the metastable and stable phase equilibria, model alloys consisting of Cu3Sn + Cu6Sn5 as well as Cu6Sn5 + Sn-rich melt were heat treated. Powder x-ray diffraction and scanning electron microscopy supplemented by electron backscatter diffraction were used to investigate the structural and microstructural changes. It was shown that Sn-poor η can increase its Sn content by Cu3Sn precipitation at grain boundaries or by uptake of Sn from the Sn-rich melt. From the kinetics of the former process at 513 K and the grain size of the η phase, we obtained an interdiffusion coefficient in η of (3 ± 1) × 10−16 m2 s−1. Comparison of this value with literature data implies that this value reflects pure volume (inter)diffusion, while Cu6Sn5 growth at low temperature is typically strongly influenced by grain-boundary diffusion. These investigations also confirm that η′′ forming below a composition-dependent transus temperature gradually enriches in Sn content, confirming that Sn-poor η′′ is metastable against decomposition into Cu3Sn and more Sn-rich η or (at lower temperatures) η′. Graphic Abstract

scholarly journals Validation of three-dimensional diffraction contrast tomography reconstructions by means of electron backscatter diffraction characterization

2013 ◽  
Vol 46 (4) ◽  
pp. 1145-1150 ◽  
Author(s):  
Melanie Syha ◽  
Andreas Trenkle ◽  
Barbara Lödermann ◽  
Andreas Graff ◽  
Wolfgang Ludwig ◽  
...  
Keyword(s):  
Electron Backscatter Diffraction ◽  
Three Dimensional ◽  
Data Reconstruction ◽  
Characterization Methods ◽  
Diffraction Contrast ◽  
Ebsd Data ◽  
Electron Backscatter ◽  
Backscatter Diffraction ◽  
Tomography Data ◽  
Good Agreement

Microstructure reconstructions resulting from diffraction contrast tomography data of polycrystalline bulk strontium titanate were reinvestigated by means of electron backscatter diffraction (EBSD) characterization. Corresponding two-dimensional grain maps from the two characterization methods were aligned and compared, focusing on the spatial resolution at the internal interfaces. The compared grain boundary networks show a remarkably good agreement both morphologically and in crystallographic orientation. Deviations are critically assessed and discussed in the context of diffraction data reconstruction and EBSD data collection techniques.

Mitrofanovite, Pt3Te4, a new mineral from the East Chuarvy deposit, Fedorovo–Pana intrusion, Kola Peninsula, Russia

2018 ◽  
Vol 83 (4) ◽  
pp. 523-530 ◽  
Author(s):  
Victor V. Subbotin ◽  
Anna Vymazalová ◽  
František Laufek ◽  
Yevgeny E. Savchenko ◽  
Chris J. Stanley ◽  
...  
Keyword(s):  
Kola Peninsula ◽  
Electron Backscatter Diffraction ◽  
New Mineral ◽  
Synthetic Analogue ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Identity ◽  
Polarised Light ◽  
Fe Alloys ◽  
Backscatter Diffraction

AbstractMitrofanovite, Pt3Te4, is a new telluride discovered in low-sulfide disseminated ore in the East Chuarvy deposit, Fedorovo–Pana intrusion, Kola Peninsula, Russia. It forms anhedral grains (up to ~20 μm × 50 μm) commonly in intergrowths with moncheite in aggregates with lukkulaisvaaraite, kotulskite, vysotskite, braggite, keithconnite, rustenburgite and Pt–Fe alloys hosted by a chalcopyrite–pentlandite–pyrrhotite matrix. Associated silicates are: orthopyroxene, augite, olivine, amphiboles and plagioclase. Mitrofanovite is brittle; it has a metallic lustre and a grey streak. Mitrofanovite has a good cleavage, along {001}. In plane-polarised light, mitrofanovite is bright white with medium to strong bireflectance, slight pleochroism, and strong anisotropy on non-basal sections with greyish brown rotation tints; it exhibits no internal reflections. Reflectance values for the synthetic analogue of mitrofanovite in air (Ro, Re’ in %) are: 58.4, 54.6 at 470 nm; 62.7, 58.0 at 546 nm; 63.4, 59.1 at 589 nm; and 63.6, 59.5 at 650 nm. Fifteen electron-microprobe analyses of mitrofanovite gave an average composition: Pt 52.08, Pd 0.19, Te 47.08 and Bi 0.91, total 100.27 wt.%, corresponding to the formula (Pt2.91Pd0.02)Σ2.93(Te4.02Bi0.05)Σ4.07 based on 7 atoms; the average of eleven analyses on synthetic analogue is: Pt 52.57 and Te 47.45, total 100.02 wt.%, corresponding to Pt2.94Te4.06. The density, calculated on the basis of the formula, is 11.18 g/cm3. The mineral is trigonal, space group R$\overline 3 $m, with a = 3.9874(1), c = 35.361(1) Å, V = 486.91(2) Å3 and Z = 3. The crystal structure was solved and refined from the powder X-ray-diffraction data of synthetic Pt3Te4. Mitrofanovite is structurally and chemically related to moncheite (PtTe2). The strongest lines in the powder X-ray diffraction pattern of synthetic mitrofanovite [d in Å (I) (hkl)] are: 11.790(23)(003), 5.891(100)(006), 2.851(26)(107), 2.137(16)(1013), 2.039(18)(0114), 1.574(24)(0120), 1.3098(21)(0027). The structural identity of natural mitrofanovite with synthetic Pt3Te4 was confirmed by electron backscatter diffraction measurements on the natural sample. The mineral name is chosen to honour Felix P. Mitrofanov, a Russian geologist who was among the first to discover platinum-group element mineralisation in the Fedorova–Pana complex.

scholarly journals X-Ray Single Crystal Structural Analysis of Magnetically Oriented Microcrystals

2014 ◽  
Vol 70 (a1) ◽  
pp. C1138-C1138
Author(s):  
Chiaki Tsuboi ◽  
Kazuki Aburaya ◽  
Shingo Higuchi ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Three Dimensional ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
Data Set ◽  
Uv Curable ◽  
X Ray

We have developed magnetically oriented microcrystal array (MOMA) technique that enables single crystal X-ray diffraction analyses from microcrystalline powder. In this method, microcrystals suspended in a UV-curable monomer matrix are there-dimensionally aligned by special rotating magnetic field, followed by consolidation of the matrix by photopolymerization. From thus achieved MOMAs, we have been succeeded in crystal structure analysis for some substances [1, 2]. Though MOMA method is an effective technique, it has some problems as follows: in a MOMA, the alignment is deteriorated during the consolidation process. In addition, the sample microcrystals cannot be recovered from a MOMA. To overcome these problems, we performed an in-situ X-ray diffraction measurement using a three-dimensional magnetically oriented microcrystal suspension (3D MOMS) of L-alanine. An experimental setting of the in-situ X-ray measurement of MOMS is schematically shown in the figure. L-alanine microcrystal suspension was poured into a glass capillary and placed on the rotating unit equipped with a pair of neodymium magnets. Rotating X-ray chopper with 10°-slits was placed between the collimator and the suspension. By using this chopper, it was possible to expose the X-ray only when the rotating MOMS makes a specific direction with respect to the impinging X-ray. This has the same effect as the omega oscillation in conventional single crystal measurement. A total of 22 XRD images of 10° increments from 0° to 220° were obtained. The data set was processed by using conventional software to obtain three-dimensional molecular structure of L-alanine. The structure is in good agreement with that reported for the single crystal. R1 and wR2 were 6.53 and 17.4 %, respectively. RMSD value between the determined molecular structure and the reported one was 0.0045 Å. From this result, we conclude that this method can be effective and practical to be used widely for crystal structure analyses.

scholarly journals Effects of Annealing Temperature on Recrystallization Texture and Microstructure Uniformity of High Purity Tantalum

Metals ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 75 ◽  
Author(s):  
Jialin Zhu ◽  
Chao Deng ◽  
Yahui Liu ◽  
Nan Lin ◽  
Shifeng Liu
Keyword(s):  
Low Temperature ◽  
Electron Backscatter Diffraction ◽  
Stored Energy ◽  
X Ray Diffraction ◽  
Center Layer ◽  
X Ray ◽  
Texture Intensity ◽  
Low Temperature Annealing ◽  
Transmission Electron ◽  
Backscatter Diffraction

One hundred and thirty-five degree clock rolling significantly improves the texture homogeneity of tantalum sheets along the thickness, but a distinctly fragmented substructure is formed within {111} (<111>//normal direction (ND)) and {100} (<100>//ND) deformation grains, which is not suitable to obtain a uniform recrystallization microstructure. Thus, effects of different annealing temperatures on the microstructure and texture heterogeneity of tantalum sheets along the thickness were investigated by X-ray diffraction (XRD), electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results show that the texture distribution along θ-fiber and γ-fiber is irregular and many large grains with {111} orientation develop during annealing at high temperature. However, low-temperature annealing can not only weaken the texture intensity in the surface and the center layer but also introduce a more uniform grain size distribution. This result can be attributed to the subgrain-nucleation-dominated recrystallization mechanism induced by recovery at low temperature, and moreover, a considerable decline of recrystallization driving force resulting from the release of stored energy in the deformation matrix.

scholarly journals Effect of TiO2-Nanoparticles on Ni Electrodeposition on Copper Wire

Metals ◽  
2020 ◽  
Vol 10 (3) ◽  
pp. 406
Author(s):  
Samiha Saad ◽  
Zakaria Boumerzoug ◽  
Anne Laure Helbert ◽  
François Brisset ◽  
Thierry Baudin
Keyword(s):  
Surface Morphology ◽  
Tio2 Nanoparticles ◽  
Vickers Microhardness ◽  
Electron Backscatter Diffraction ◽  
Copper Wire ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electron Backscatter ◽  
Electrodeposited Nickel ◽  
Backscatter Diffraction

The objective of this work is to study, on a copper wire, the effect of TiO2-nanoparticles on electrodeposited nickel. Both the microstructure and surface morphology (texture) of the coating were investigated. This deposit is obtained from baths of sulfated electroplating Watts. The Ni-TO2 composite coating is deposited at a temperature of 45 °C. The composite deposit is prepared by adding nanoparticles of TiO2 to the electrolyte. The characterization has been carried out by X-ray diffraction, scanning electron microscopy, microhardness measurements, and electron backscatter diffraction (EBSD). Vickers microhardness was used to characterize the mechanical properties of the electrodeposited nickel. The results showed the effects of the TiO2 on the composition, the surface morphology, and the hardness of the deposited layer. However, there was not an effect of TiO2 nanoparticles on texture.

Surface Crystallization of Cordierite from Glass Studied by High-Temperature X-ray Diffraction and Electron Backscatter Diffraction (EBSD)

2011 ◽  
Vol 11 (10) ◽  
pp. 4660-4666 ◽  
Author(s):  
Wolfgang Wisniewski ◽  
Carlos André Baptista ◽  
Matthias Müller ◽  
Günter Völksch ◽  
Christian Rüssel
Keyword(s):  
High Temperature ◽  
Electron Backscatter Diffraction ◽  
Surface Crystallization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Electron Backscatter ◽  
Backscatter Diffraction
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