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At least 37 records · Page 2

Synchrotron X-Ray Diffraction Studies of Olivine from Comet Wild 2

We have analyzed a collection of the Comet Wild 2 coma grains returned by the NASA Stardust Mission, using micro-area Laue diffraction equipment. The purpose of the diffraction experiment is to permit the structure refinement of olivine including site occupancies. In addition to the intrinsic importance of the olivine structures for revealing the thermal history of Wild 2 materials, we wish to test reports that olivine recovered after hypervelocity capture in silica aerogel has undergone a basic structural change due to capture heating [1]. The diffraction equipment placed at beam line BL- 4B1 of PF, KEK was developed with a micropinhole and an imaging plate (Fuji Co. Ltd.) using the Laue method combined with polychromatic X-ray of synchrotron radiation operated at energy of 2.5 GeV. The incident beam is limited to 1.6 m in diameter by a micropinhole set just upstream of the sample [2, 3]. It is essential to apply a microbeam to obtain diffracted intensities with high signal to noise ratios. This equipment has been successfully applied to various extraterrestrial materials, including meteorites and interplanetary dust particles [4]. The Laue pattern of the sample C2067,1,111,4 (Fig. 1) was successfully taken on an imaging plate after a 120 minute exposure (Fig. 2).

Source record↗

Nanoscale lattice strains in self-ion implanted tungsten

Developing a comprehensive understanding of the modification of material properties by neutron irradiation is important for the design of future fission and fusion power reactors. Self-ion implantation is commonly used to mimic neutron irradiation damage, however an interesting question concerns the effect of ion energy on the resulting damage structures. The reduction in the thickness of the implanted layer as the implantation energy is reduced results in the significant quandary: Does one attempt to match the primary knock-on atom energy produced during neutron irradiation or implant at a much higher energy, such that a thicker damage layer is produced? In this work, we address this question by measuring the full strain tensor for two ion implantation energies, 2 MeV and 20 MeV in self-ion implanted tungsten, a critical material for the first wall and divertor of fusion reactors. A comparison of 2 MeV and 20 MeV implanted samples is shown to result in similar lattice swelling. Multi-reflection Bragg coherent diffractive imaging (MBCDI) shows that implantation induced strain is in fact heterogeneous at the nanoscale, suggesting that there is a non-uniform distribution of defects, an observation that is not fully captured by micro-beam Laue diffraction. At the surface, MBCDI and high-resolution electron back-scattered diffraction (HR-EBSD) strain measurements agree quite well in terms of this clustering/non-uniformity of the strain distribution. However, MBCDI reveals that the heterogeneity at greater depths in the sample is much larger than at the surface. This combination of techniques provides a powerful method for detailed investigation of the microstructural damage caused by ion bombardment, and more generally of strain related phenomena in micro-volumes that are inaccessible via any other technique.

36 MATERIALS SCIENCE↗

Fleetite, Cu 2 RhIrSb 2 , a New Species of Platinum-Group Mineral from the Miass Placer Zone, Southern Urals, Russia

Fleetite, Cu 2 RhIrSb 2 , a new species of platinum-group mineral (PGM), was discovered intergrown with an Os–Ir–Ru alloy in the Miass Placer Zone (Au–PGE), southern Urals, Russia. A single grain 50 μm across was found. Osmium, ruthenium, and iridium are the main associated minerals; also present are Pt–Fe alloys, laurite, Sb-rich irarsite, Rh-rich tolovkite, kashinite, anduoite, ferronickelplatinum, heazlewoodite, PGE-bearing pentlandite and digenite, as well as micrometric inclusions of forsterite (Fo 93.7 ), chromite–magnesiochromite, and Mg-rich edenite. In reflected light, fleetite is light gray; it is opaque, isotropic, non-pleochroic, and non-bireflectant. We report reflectance values measured in air. A mean of seven point-analyses (wavelength-dispersive spectrometry) gave Cu 13.93, Ni 8.60, Fe 0.10, Ir 28.07, Rh 7.91, Ru 1.96, Sb 39.28, total 99.85 wt.%, corresponding to (Cu 1.41 Ni 0.58 Fe 0.01 ) Σ2.00 (Rh 0.49 Ni 0.36 Ru 0.12 ) Σ0.97 Ir 0.95 Sb 2.08 on the basis of six atoms per formula unit, taking into account the structural results. The calculated density is 10.83 g/cm 3 . Single-crystal X-ray studies show that fleetite is cubic, space group Fdm (#227), a = 11.6682(8) Å, V = 1588.59(19) Å 3 , and Z = 16. A least-squares refinement of X-ray powder-diffraction data gave a = 11.6575(5) Å and V = 1584.22(19) Å 3 . The strongest five reflections in the powder pattern [d in Å(I)(hkl)] are: 6.70(75)(111), 4.13(100)(220), 3.52(30)(311), 2.380(50)(422), 2.064(40)(440). Results of synchrotron micro-Laue diffraction experiments are consistent [a = 11.66(2) Å]. The crystal structure of fleetite was solved and refined to R = 0.0340 based upon 153 reflections with F o > 4σ(F o ). It is isotypic with Pd 11 Bi 2 Se 2 and best described as intermetallic, with all metal atoms in 12-fold coordination. Fleetite and other late exotic phases were formed by reaction of the associated alloy phases with a fluid phase enriched in Sb, As, and S in circulation in the cooling ophiolite source-rock. The mineral is named after Michael E. Fleet (1938–2017) in recognition of his significant contributions to the Earth Sciences.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Derived crystal structure of martensitic materials by solid–solid phase transformation

A mathematical description of crystal structure is proposed consisting of two parts: the underlying translational periodicity and the distinct atomic positions up to the symmetry operations in the unit cell, consistent with the International Tables for Crystallography. By the Cauchy–Born hypothesis, such a description can be integrated with the theory of continuum mechanics to calculate a derived crystal structure produced by solid–solid phase transformation. In addition, the expressions for the orientation relationship between the parent lattice and the derived lattice are generalized. Additionally, the derived structure rationalizes the lattice parameters and the general equivalent atomic positions that assist the indexing process of X-ray diffraction analysis for low-symmetry martensitic materials undergoing phase transformation. The analysis is demonstrated in a CuAlMn shape memory alloy. From its austenite phase (L2 1 face-centered cubic structure), it is identified that the derived martensitic structure has orthorhombic symmetry Pmmn with the derived lattice parameters a d = 4.36491, b d = 5.40865 and c d = 4.2402 Å, by which the complicated X-ray Laue diffraction pattern can be well indexed, and the orientation relationship can be verified.

36 MATERIALS SCIENCE↗

Revealing the Subsurface Basal $\langle$a$\rangle$ Dislocation Activity in Magnesium Through Lattice Rotation Analysis

A method was proposed in this study to reveal the subsurface basal dislocation activity in Mg-Y alloy and determine the corresponding Burgers vector. This is achieved by correlating the slip directions of dislocations to the lattice rotation represented by the {0001} pole figure. The identified basal slip system by this approach was verified by micro-Laue diffraction. This method can be applied as a complementary method to the conventional slip trace analysis to study the dislocation behavior of Mg alloys.

36 MATERIALS SCIENCE↗

Characterising Ion-Irradiated FeCr: Hardness, Thermal Diffusivity and Lattice Strain

Ion-irradiated FeCr alloys are useful for understanding and predicting neutron damage in the structural steels of future nuclear reactors. Previous studies have largely focused on the structure of irradiation induced defects, probed by transmission electron microscopy (TEM), as well as changes in mechanical properties. Across these studies, a wide range of irradiation conditions has been employed on samples with different processing histories, which complicates the analysis of the relationship between defect structures and material properties. Furthermore, key properties, such as irradiation-induced changes in thermal transport and lattice strain, are little explored. Here we present a systematic study of Fe3Cr, Fe5Cr and Fe10Cr binary alloys implanted with 20 MeV Fe3+ ions to nominal doses of 0.01 dpa and 0.1 dpa at room temperature. Nanoindentation, transient grating spectroscopy (TGS) and X-ray micro-beam Laue diffraction were used to study the changes in hardness, thermal diffusivity and strain in the material as a function of damage and Cr content. Our results suggest that Cr leads to an increased retention of irradiation-induced defects, causing substantial changes in hardness and lattice strain. However, thermal diffusivity varies little with increasing damage and instead degrades significantly with increasing Cr content in the material. We find significant lattice strains even in samples exposed to a nominal displacement damage of 0.01 dpa. The defect density predicted from the lattice strain measurements is significantly higher than that observed in previous TEM studies, suggesting that TEM may not fully capture the irradiation-induced defect population. (C) 2020 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

FeCr alloys↗

High Magnetic Anisotropy and Magnetocaloric Effects in Single-Crystal Cr 2 Te 3

Here, we report a systematic investigation of anisotropic magnetocaloric effects in single-crystal Cr 2 Te 3 . Single-crystal samples are synthesized by chemical vapor transport and characterized by X-ray and Laue diffraction methods. The maximum magnetic entropy change –ΔS M max is 4.50 J kg –1 K –1 for the easy c-axis (3.36 J kg –1 K –1 for the hard axis along ab-plane), and the relative cooling power (RCP) is 296.7 J kg –1 for the easy c-axis (183.84 J kg –1 for the hard axis along ab-plane) for a magnetic field change of 9 T near the Curie temperature. The magneto-crystalline anisotropy constant K u is estimated to be 580.12 kJ m –3 at 140 K, decreasing to 148.60 kJ m –3 at 168 K. Meanwhile, the maximum of the rotational magnetic entropy change –ΔS M R (T, H) between the c-axis and the ab-plane is about 1.14 J kg –1 K –1 for magnetic-field change of 9 T. The critical exponents are estimated by analyzing magnetocaloric effects, which indicate a 2D-Ising type magnetic system. The accuracy of estimated critical exponents is verified by scaling analysis. The maximum magnetic entropy change –ΔS M max ≈ 5.25 J kg –1 K –1 (along the c-axis) and the corresponding adiabatic temperature change ΔT ad ≈ 3.31 K (along the c-axis) are estimated by analyzing heat capacity measurements with a magnetic field up to 9 T.

36 MATERIALS SCIENCE↗

EXTENDED VERSION OF SOFTWARE POLYLAUE

(SF-24-031) Software PolyLaue, having ANL OPEN SOURCE LICENSE, will be extended by KITWARE, INC. New functionality, including file manager, visualizer and mapping routine will substantially improve the procedure to identify single-crystals across compression with Laue diffraction technique.

Popov, DmitryYu↗

Criticality and Magnetic Phases of Ising Shastry–Sutherland Candidate Holmium Tetraboride

Frustrated magnetic systems arising in geometrically constrained lattices represent rich platforms for exploring unconventional phases of matter, including fractional magnetization plateaus, incommensurate orders and complex domain dynamics. However, determining the microscopic spin configurations that stabilize such phases is a key challenge, especially when in-plane and out-of-plane spin components coexist and compete. Here, we combine neutron scattering and magnetic susceptibility experiments with simulations to investigate the emergence of field-induced fractional plateaus and the related criticality in a frustrated magnet holmium tetraboride (HoB 4 ) that represents the family of rare earth tetraborides that crystalize in a Shastry–Sutherland lattice in the ab plane. We focus on the interplay between classical and quantum criticality near phase boundaries, as well as the role of material defects in the stabilization of the ordered phases. We find that simulations using classical annealing can explain certain observed features in the experimental Laue diffraction and the origin of multiple magnetization plateaus. Our results show that defects and out-of-plane interactions play an important role and can guide the route towards resolving microscopic spin textures in highly frustrated magnets.

Frustration↗

Unnamed Pt(Cu 0.67 Sn 0.33 ) from the Bolshoy Khailyk River, Western Sayans, Russia, and a Review of Related Compounds and Solid Solutions

We describe a potentially new species of a platinum cupride–stannide mineral (PCSM) of composition Pt(Cu 0.67 Sn 0.33 ). It occurs in a placer deposit in the River Bolshoy Khailyk, southern Krasnoyarskiy kray, Russia. A synthetic equivalent of PCSM was obtained and characterized. The PCSM occurs as anhedral or subhedral grains up to 15 μm × 30 μm in association with various platinum-group minerals, Rh–Co-rich pentlandite and magnetite, all hosted by a placer grain of Cu–Au–Pt alloy. Synchrotron micro-Laue diffraction studies indicate that the PCSM mineral is tetragonal and belongs to the inferred space-group P4/mmm (#123). Its unit-cell parameters are a = 2.838 (3) Å, c = 3.650 (4) Å, and V = 29.40 (10) Å 3 , and Z = 1. The c:a ratio calculated from the unit-cell parameters is 1.286. These characteristics are in good agreement with those obtained for specimens of synthetic Pt(Cu 0.67 Sn 0.33 ). A review on related minerals and unnamed phases is provided to outline compositional variations and extents of solid solutions in the relevant systems PtNi–PtFe–PtCu, PdCu–PdHg–PdAu, PdHg–PtHg, and AuCu–PtCu. The PCSM-bearing mineralization appears to be related genetically with an ophiolitic source-rock of the Aktovrakskiy complex of the western Sayans. The unnamed phase likely crystallized from microvolumes of a highly fractionated melt rich in Cu and Sn.

36 MATERIALS SCIENCE↗

Growth of ZnTe by Physical Vapor Transport and Traveling Heater Method

ZnTe crystals were grown by horizontal physical vapor transport (PVT) and a Te-solution vertical traveling heater method (THM). The grown crystals were examined by X-ray Laue diffraction technique and Hall measurements to determine the growth orientation and the electrical properties of the crystals. They were also characterized by low temperature infrared (IR) absorption measurements. Several sets of distinct peaks were observed in the IR absorption spectra for the THM samples and were identified as resulting from CU(2+) impurities. Similar measurements on vapor grown ZnTe showed featureless absorption spectra. Chemical analyses were carried out to measure the impurity content in various ZnTe samples and synchrotron radiation topography was used to Study crystalline microstructure of the (111) ZnTe single crystals grown by PVT.

Su, Ching-Hua↗

Characterization of 4H <000-1> Silicon Carbide Films Grown by Solvent-Laser Heated Floating Zone

Commercially available bulk silicon carbide (SiC) has a high number (>2000/sq cm) of screw dislocations (SD) that have been linked to degradation of high-field power device electrical performance properties. Researchers at the NASA Glenn Research Center have proposed a method to mass-produce significantly higher quality bulk SiC. In order for this bulk growth method to become reality, growth of long single crystal SiC fibers must first be achieved. Therefore, a new growth method, Solvent-Laser Heated Floating Zone (Solvent-LHFZ), has been implemented. While some of the initial Solvent-LHFZ results have recently been reported, this paper focuses on further characterization of grown crystals and their growth fronts. To this end, secondary ion mass spectroscopy (SIMS) depth profiles, cross section analysis by focused ion beam (FIB) milling and mechanical polishing, and orientation and structural characterization by x-ray transmission Laue diffraction patterns and x-ray topography were used. Results paint a picture of a chaotic growth front, with Fe incorporation dependant on C concentration.

Woodworth, Andrew, A↗

Extracting information from X-ray diffraction patterns containing Laue oscillations

The presence of Laue oscillations in a film grown on a solid surface is broadly taken as indicating a high quality, crystallographically aligned film of the targeted compound. In this paper we briefly review the origins of both Laue oscillations and Kiessig fringes and show how they can be used together to determine if extra thickness exists above or below the coherently diffracting domains. The differences between experimental and “ideal” films are discussed and the effect of structural features (roughness, different thickness coherently diffracting domains and thickness in addition to the coherently diffracting domains) are illustrated with experimental and simulated data for metal and mixed-metal chalcogenide films of titanium, bismuth, vanadium/iron, and bismuth/molybdenum. Examples are given showing how quantitative information can be extracted from experimental diffraction patterns.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Economical Laue x-ray diffraction using photographic film and orientation of single crystals

Many Laue x-ray diffraction systems using the Polaroid XR-7 Land Diffraction Cassette camera became inactive after production of the required high sensitivity Polaroid T-57 instant film ceased. This Tutorial reports on a low-cost solution using the readily available replacement film with push processing to increase the effective film speed. The use of this film in the polaroid camera is described along with film development and digitization. The orientation of single crystals with the obtained data and free software is explained. A simple method to prepare single crystals with surfaces perpendicular to a desired crystallographic orientation is described. The content of this Tutorial may prove beneficial for educational and research laboratories.

47 OTHER INSTRUMENTATION↗

Synchrotron x-Ray Study of Heterostructured Materials: A Review

Heterostructured materials (HSMs) have shown great potential for breaking the strength-ductility tradeoff. HSMs consist of heterogeneous zones that may have different sizes, shapes, compositions, structures, etc. Interactions and competitions among them often lead to unprecedented properties. However, due to the complex structures in a broad range of length scales, it is challenging to unravel deformation physics and strengthening mechanisms underlying extraordinary mechanical properties. Synchrotron x-rays provide powerful techniques and indispensable tools for investigating HSMs at various length scales. Here, we will present in situ high-energy x-ray diffraction and Laue x-ray microdiffraction techniques and their application in studying the HSMs. In this study, the principles of these techniques will be briefly introduced. We will focus on their application in studying stress partitioning and plastic accommodation during tensile deformation, thermo-driven and/or stress-driven phase transformations and various deformation microstructures like geometrically necessary dislocations and local stress/strain distributions, etc., in HSMs. Some important findings will be summarized. Challenging issues remain in studying HSMs and will be discussed.

36 MATERIALS SCIENCE↗

X-ray Laue Microdiffraction and Raman Spectroscopic Investigation of Natural Silicon and Moissanite

Moissanite, SiC, is an uncommon accessory mineral that forms under low oxygen fugacity. Here, we analyze natural SiC from a Miocene tuff-sandstone using synchrotron Laue microdiffraction and Raman spectroscopy, in order to better understand the SiC phases and formation physics. The studied crystals of SiC consist of 4H- and 6H-SiC domains, formed from either, continuous growth or, in one case, intergrown, together with native Si. The native Si is polycrystalline, with a large crystal size relative to the analytical beam dimensions (>1–2 μm). We find that the intergrown region shows low distortion or dislocation density in SiC, but these features are comparatively high in Si. The distortion/deformation observed in Si may have been caused by a mismatch in the coefficients of thermal expansion of the two materials. Raman spectroscopic measurements are discussed in combination with our Laue microdiffraction results. Our results suggest that these SiC grains likely grew from an igneous melt.

58 GEOSCIENCES↗