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At least 109 records · Page 6

A Denoising Autoencoder for Improved Kikuchi Pattern Quality and Indexing in Electron Backscatter Diffraction

The rapid collection and indexing of electron diffraction patterns as produced via electron backscatter diffraction (EBSD) has enabled crystallographic orientation and structural determination, as well as additional property-determining strain and dislocation density information with increasing speed, resolution, and efficiency. Pattern indexing quality is reliant on the noise of the collected electron diffraction patterns, which is often convoluted by sample preparation and data collection parameters. EBSD acquisition is sensitive to many factors and thus can result in low confidence index (CI), poor image quality (IQ), and improper minimization of fit, which can result in noisy datasets and misrepresent the microstructure. In an attempt to enable both higher speed EBSD data collection and enable greater orientation fit accuracy with noisy datasets, an image denoising autoencoder was implemented to improve pattern quality. Here, we show that EBSD data processed through the autoencoder results in a higher CI, IQ, and a more accurate degree of fit. In addition, using denoised datasets in HR-EBSD cross correlative strain analysis can result in reduced phantom strain from erroneous calculations due to the increased indexing accuracy and improved correspondence between collected and simulated patterns.

36 MATERIALS SCIENCE↗

Characterizing Corrosion Mechanisms Of Structural Alloys In Actinide-based Molten Chloride Salt

This is a dataset consisting of 33 GB of .png image files, each featuring a two-dimensional distribution of different element species captured an individual slice of the specimen, and .ang files that capture microstructural information captured from each respective slice using a technique called electron backscatter diffraction. The .ang files can be processed to visualize alloy grains captured in a respective slice.

Copeland, Trishelle M.↗

Automated Grain Boundary (GB) Segmentation and Microstructural Analysis in 347H Stainless Steel Using Deep Learning and Multimodal Microscopy

Austenitic 347H stainless steel offers superior mechanical properties and corrosion resistance required for extreme operating conditions such as high temperature. The change in microstructure due to composition and process variations is expected to impact material properties. Identifying microstructural features such as grain boundaries thus becomes an important task in the process-microstructure-properties loop. Applying convolutional neural network (CNN)-based deep learning models is a powerful technique to detect features from material micrographs in an automated manner. In contrast to microstructural classification, supervised CNN models for segmentation tasks require pixel-wise annotation labels. However, manual labeling of the images for the segmentation task poses a major bottleneck for generating training data and labels in a reliable and reproducible way within a reasonable timeframe. Microstructural characterization especially needs to be expedited for faster material discovery by changing alloy compositions. Here, in this study, we attempt to overcome such limitations by utilizing multimodal microscopy to generate labels directly instead of manual labeling. We combine scanning electron microscopy images of 347H stainless steel as training data and electron backscatter diffraction micrographs as pixel-wise labels for grain boundary detection as a semantic segmentation task. The viability of our method is evaluated by considering a set of deep CNN architectures. We demonstrate that despite producing instrumentation drift during data collection between two modes of microscopy, this method performs comparably to similar segmentation tasks that used manual labeling. Additionally, we find that naïve pixel-wise segmentation results in small gaps and missing boundaries in the predicted grain boundary map. By incorporating topological information during model training, the connectivity of the grain boundary network and segmentation performance is improved. Finally, our approach is validated by accurate computation on downstream tasks of predicting the underlying grain morphology distributions which are the ultimate quantities of interest for microstructural characterization.

36 MATERIALS SCIENCE↗

Formation of wide-blocky calcite veins by extreme growth competition

Liassic limestones on the coast of Somerset in the UK contain dense arrays of calcite microveins with a common, but poorly understood microstructure, characterized by laterally wide crystals that form bridges across the vein. We investigated the mechanisms of formation and evolution of these ‘wide-blocky’ vein microstructures using a combination of high-resolution analytical methods, including virtual petrography, optical cathodoluminescence and scanning electron microscopy techniques (e.g. energy-dispersive X-ray spectrometry, back-scattered electron imaging, cathodoluminescence and electron back-scattered diffraction), laboratory experiments and multiphase field modelling. Our results indicate that the studied veins formed in open, fluid-filled fractures, each in a single opening and sealing episode. As shown by the optical and electron back-scattered diffraction images, the vein crystals grew epitaxially on grains of the wall rock and we hypothesize that their growth rates differed depending on whether the crystals were on a wall rock grain substrate that fractured intergranularly (slow growth rates) or transgranularly (rapid growth rates). Our multiphase field models support this hypothesis, showing that wide, blocky crystals only form where there are significant differences in the growth rate and are dependent on the type of seed grain. These results provide strong evidence for extreme growth competition, a process that we propose controls vein-filling in many micritic carbonate reservoirs, as well as demonstrate that the characteristics of the fracture wall can affect the filling processes in syntaxial veins. Supplementary material: The description and images of the studied thin sections are available at https://doi.org/10.6084/m9.figshare.c.5172371 . High-resolution optical microscopy mosaics (under plane-polarized- and crossed polarized light) of the thin section collection in PetroScan file format are available on request from the authors.

Geology↗

Primary Objective Grating Astronomical Telescope

It has been 370 years since a seventeenth century French mathematician, Mersenne, presciently sketched out an astronomical telescope based on dual parabolic reflectors. Since that time the concept of the primary objective has been virtually unchanged. Now a new class of astronomical telescope with a primary objective grating (POG) has been studied as an alternative. The POG competes with mirrors, in part, because diffraction gratings provide the very chromatic dispersion that mirrors defeat. The resulting telescope deals effectively with long-standing restrictions on multiple object spectroscopy (MOS). Other potential benefits include unprecedented apertures and collection areas. The new design also favors space deployment as a gossamer membrane. The inventor, Tom Ditto, first discovered that higher-order diffraction images contain hidden depth cues, for which he was granted a seminal range finding patent in 1987. Subsequently, he invented and patented 3D localizers, profilometers and microscopes using POGs. The POG telescope was placed in the public domain to expedite research. The function of a telescopes primary objective is to collect flux and to deliver images. Both functions dictate that size matters, and bigger is better. For that reason, there has been a steady push over the past century to ramp up the size of the primary mirror. However, for every doubling of mirror diameter, the elapsed time between initial effort and first light has also doubled. Meanwhile, costs escalated beyond the mirror alone, because larger instruments required larger enclosures and better pointing mechanisms. One key catalog of observation, spectrographic data, is far more difficult to amass than two-dimensional imagery. While the number of observable objects has increased with mirror size, the capacity to take spectra has not increased proportionately. In the best of circumstances, spectrograms are available for one per cent of the all objects surveyed. Spectroscopy was a historical afterthought introduced in the nineteenth century shortly after the invention of the diffraction grating and over a century after Newtons 1670 telescope. Spectroscopy is generally accomplished using a diffraction grating as the disperser in the secondary. The light being delivered to the spectrograph is first captured by a primary mirror which provides no chromatic magnification by itself. Sizeable spectrographs could not be deployed while diffraction gratings were rare commodities scribed using mechanical ruling engines that produced one grating line at a time. Today diffraction gratings are commonplace. Their recent availability is a product of both the invention of holography and the mass replication of surface microstructures. Holography permits all lines in a grating to be made simultaneously in a single photographic exposure. Holograms can then be reproduced by embossing processes. The improvement in replication is analogous to how Gutenberg changed the availability of books. The masters may be expensive, but the copies are not. Computer science is another technology that emerged in the second half of the twentieth century without which our proposed spectrographic instrument could not function due to the complexity of image processing required in data reduction. The employment of very large diffraction gratings as primary objectives for astronomical telescopes requires a novel

spectroscopy↗

Development of combined microstructure and structure characterization facility for in situ and operando studies at the Advanced Photon Source

Following many years of evolutionary development, first at the National Synchrotron Light Source, Brookhaven National Laboratory, and then at the Advanced Photon Source (APS), Argonne National Laboratory, the APS ultra-small-angle X-ray scattering (USAXS) facility has been transformed by several new developments. These comprise a conversion to higher-order crystal optics and higher X-ray energies as the standard operating mode, rapid fly scan measurements also as a standard operational mode, automated contiguous pinhole small-angle X-ray scattering (SAXS) measurements at intermediate scattering vectors, and associated rapid wide-angle X-ray scattering (WAXS) measurements for X-ray diffraction without disturbing the sample geometry. With each mode using the USAXS incident beam optics upstream of the sample, USAXS/SAXS/WAXS measurements can now be made within 5 min, allowing in situ and operando measurement capabilities with great flexibility under a wide range of sample conditions. Furthermore, these developments are described, together with examples of their application to investigate materials phenomena of technological importance. Developments of two novel USAXS applications, USAXS-based X-ray photon correlation spectroscopy and USAXS imaging, are also briefly reviewed.

47 OTHER INSTRUMENTATION↗

Defect identification in simulated Bragg coherent diffraction imaging by automated AI

X-ray Bragg coherent diffraction imaging is a powerful technique for operando and in situ materials characterization and provides a unique means of quantifying the influence of one-dimensional (1D) and two-dimensional (2D) material defects on material response. However, obtaining full images from raw x-ray diffraction data is nontrivial and computationally intensive, precluding real-time experimental feedback. Here, we present a machine learning approach to identify the presence of crystalline line defects (edge and screw) in samples from the raw, 2D, coherent diffraction data without the need for image reconstruction through iterative phase retrieval. Further, we compare different approaches to designing neural networks for this application and demonstrate the potential of automated ML (autoML) approaches.

36 MATERIALS SCIENCE↗

Understanding the structural and morphological effects of synthesis route on NpO 2

The availability of actinide standard materials for use in nuclear safeguard applications is critical, as is thorough characterization thereof. Although accurate trace element compositions and isotopic considerations are paramount for deployment of reference standards, structural characterization is also essential towards accurately describing the chemical form and potential matrix effects in candidate materials. Here, to this end, samples of NpO 2 were synthesized via a direct denitration (DD) method and probed with powder X-ray diffraction (PXRD), Raman spectroscopy, and scanning electron microscopy (SEM) for structural and morphological characterization and comparison with NpO 2 materials produced via modified direct denitration (MDD). PXRD confirmed the bulk identity of NpO 2 , and no additional phases were identified using this method. Analysis of Raman data collected using a 532 nm excitation wavelength indicates that samples are mostly phase pure; however, some variability in spectral features is observed. Analysis of additional spectroscopic data collected with a 785 nm excitation wavelength revealed variability in the relative intensity of spectral features. Raman spectroscopy indicates that the sample is primarily NpO 2 ; however, additional signals indicate possible structural disorder, oxidized species, or potential contributions from other Np phases. To further investigate the possibility of additional phase contributions within the sample of NpO 2 , Raman spectroscopic mapping was employed to examine the homogeneity of the sample produced via DD. From this analysis, we determined that despite variability in the intensity of Raman-active vibrational modes, consistent spectra are obtained throughout the area of the sample investigated. SEM images show aggregates with variable sizes and shapes, with rounded, primary particles possessing an average diameter of approximately 100 nm. Comparison of the results of these multimodal analyses to the literature indicates that the crystal chemical, spectroscopic, and microstructural properties of NpO 2 vary based on synthesis method, even if X-ray diffraction data indicate that the bulk phase is NpO 2 .

Direct denitration↗

Four-dimensional microstructurally small fatigue crack growth in cyclically loaded nickel superalloy specimen

Here, we nondestructively image a low-solvus high refractory (LSHR) nickel base specimen microstructure during cyclic loading to characterize crack propagation during the microstructurally small crack (MSC) growth regime. Micro-computed tomography (uCT) is used to characterize the material density and identify crack interfaces, while high-energy diffraction microscopy (HEDM) provides snapshots of the microstructural orientation field changes. From these measurements, data are computationally reconstructed and coregistered to describe the specimen’s configuration before load, before crack nucleation, and throughout the crack propagation/loading process. An MSC forms at a FIB-cut notch, which was previously placed to concentrate stress at the center of the specimen gauge, and propagates along a facet parallel to the local {1 1 1} crystallographic plane. Analysis of available crystallographic slip directions and measured point-to-point disorientation axes indicate probable single and coplanar slip activity along FCC octahedral planes within this region. Similar analyses of other crack propagation facets reveal generally slower growth along directions favoring zig-zag cross and codirectional cross slip, which are often disfavored at room temperature.

36 MATERIALS SCIENCE↗

The 650 °C Tensile Deformation of Graded IN718-René41 Superalloy Fabricated by Laser Blown-Powder Directed Energy Deposition

The microstructure and 650 °C tensile properties of a compositionally graded IN718-René41 (718-R41) superalloy fabricated by laser blown-powder directed energy deposition (DED-LB/M) are investigated to understand structure–property relationships and baseline tensile properties. Digital Image Correlation (DIC), in situ neutron diffraction, and conventional characterization techniques are performed to study the as-built and heat-treated states. The applied heat treatment generates static recrystallization and equiaxed grains in 718-rich compositions, while R41-rich compositions remain partially or un-recrystallized possibly influenced by a higher MC carbide fraction (>0.5%). The yield strengths of the 718 and R41 sections in the heat-treated state are comparable to wrought forms but the graded compositions show weakness due to unoptimized heat treatment. Diffraction elastic constants first decrease and then increase along the 718-R41 composition gradient, while a small difference is observed between the as-built and heat-treated states and γ, γ′ phases. Overall, the compositionally graded region shows a smooth transition in the elastic properties. Grain-level load transfer from the (220) to (200) grains shows compositional dependence, and qualitatively agrees with DIC-measured macroscopic yield strength. Within the (200) grains, the γ/γ′ phases deform elastically until the γ phase yields and afterwards, the γ′ phase takes load from the γ phase.

Huang, Shenyan (ORCID:0000000196528114)↗

3D Reconstruction of a High-Energy Diffraction Microscopy Sample Using Multi-modal Serial Sectioning with High-Precision EBSD and Surface Profilometry

High-energy diffraction microscopy (HEDM) combined with in situ mechanical testing is a powerful nondestructive technique for tracking the evolving microstructure within polycrystalline materials during deformation. This technique relies on a sophisticated analysis of X-ray diffraction patterns to produce a three-dimensional reconstruction of grains and other microstructural features within the interrogated volume. However, it is known that HEDM can fail to identify certain microstructural features, particularly smaller grains or twinned regions. Characterization of the identical sample volume using high-resolution surface-specific techniques, particularly electron backscatter diffraction (EBSD), can not only provide additional microstructure information about the interrogated volume but also highlight opportunities for improvement of the HEDM reconstruction algorithms. In this study, a sample fabricated from undeformed “low solvus, high refractory” nickel-based superalloy was scanned using HEDM. The volume interrogated by HEDM was then carefully characterized using a combination of surface-specific techniques, including epi-illumination optical microscopy, zero-tilt secondary and backscattered electron imaging, scanning white light interferometry, and high-precision EBSD. Custom data fusion protocols were developed to integrate and align the microstructure maps captured by these surface-specific techniques and HEDM. The raw and processed data from HEDM and serial sectioning have been made available via the Materials Data Facility (MDF) at https://doi.org/10.18126/4y0p-v604 for further investigation.

36 MATERIALS SCIENCE↗

Ultrafast Relativistic Electron Nanoprobes

Abstract One of the frontiers in electron scattering is to couple ultrafast temporal resolution with highly localized probes to investigate the role of microstructure on material properties. Here, taking advantage of the high average brightness of our electron source, we demonstrate the generation of ultrafast relativistic electron beams with picometer-scale emittance and their ability to probe nanoscale features on materials with complex microstructures. The electron beam is tightly focused at the sample plane by a custom in-vacuum lens system, and its evolution around the waist is accurately reconstructed. We then use the focused beam to characterize a Ti-6 wt% Al polycrystalline sample by correlating the diffraction and imaging modality, showcasing the capability to locate grain boundaries and map adjacent crystallographic domains with sub-micron precision. This work provides a paradigm for ultrafast electron instrumentation, enabling characterization techniques such as relativistic ultrafast electron nano-diffraction and ultrafast scanning transmission electron microscopy.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Simultaneous bright- and dark-field X-ray microscopy at X-ray free electron lasers

Abstract The structures, strain fields, and defect distributions in solid materials underlie the mechanical and physical properties across numerous applications. Many modern microstructural microscopy tools characterize crystal grains, domains and defects required to map lattice distortions or deformation, but are limited to studies of the (near) surface. Generally speaking, such tools cannot probe the structural dynamics in a way that is representative of bulk behavior. Synchrotron X-ray diffraction based imaging has long mapped the deeply embedded structural elements, and with enhanced resolution, dark field X-ray microscopy (DFXM) can now map those features with the requisite nm-resolution. However, these techniques still suffer from the required integration times due to limitations from the source and optics. This work extends DFXM to X-ray free electron lasers, showing how the $$10^{12}$$ 10 12 photons per pulse available at these sources offer structural characterization down to 100 fs resolution (orders of magnitude faster than current synchrotron images). We introduce the XFEL DFXM setup with simultaneous bright field microscopy to probe density changes within the same volume. This work presents a comprehensive guide to the multi-modal ultrafast high-resolution X-ray microscope that we constructed and tested at two XFELs, and shows initial data demonstrating two timing strategies to study associated reversible or irreversible lattice dynamics.

47 OTHER INSTRUMENTATION↗

Effects of deposition and annealing conditions on the crystallisation of NiTi thin films by e-beam evaporation

This Letter demonstrates the effects of deposition and annealing conditions on the crystallisation of nickel–titanium (NiTi) thin films deposited by the e-beam evaporation. NiTi thin films of 0.5 μm thick are fabricated on P-type (110) silicon substrates using the e-beam evaporation technique. We find that with the characterisations using the X-ray diffraction method, the results indicate that low e-beam deposition rate and argon employed annealing procedures can be beneficial to the formation of NiTi crystalline structure. Additionally, the as-deposited NiTi thin films without annealing procedures are amorphous, when deposited on the substrates at low temperatures. The differential scanning calorimetry studies show NiTi thin films formed by the e-beam evaporation are Ni-rich. Furthermore, SEM images illustrate that high-precision patterned NiTi thin film microstructures can be fabricated by combining with the e-beam evaporation and lift-off resist methods, without any wet or dry etching procedures. The proposed fabrication process for NiTi thin film microstructures shows great potential for application in shape memory alloy medical devices, as well as the micro-robotics.

36 MATERIALS SCIENCE↗

Investigation of the effect of structural defects from hydride precipitation on superconducting properties of high purity SRF cavity Nb using magneto-optical and electron imaging methods

Abstract Nb is an elemental superconductor with a critical temperature of 9.3 K and is widely used to fabricate superconducting radiofrequency (SRF) cavities for particle accelerators. However, microstructural defects in Nb, such as grain boundaries (GBs) and dislocations, can act as pinning centers for magnetic flux that can degrade SRF cavity performance. Hydrogen contamination is also detrimental to SRF cavity performance due to the formation of normal conducting hydrides during cool down. In this study, disc shaped Nb bi-crystals extracted from high-purity large-grain Nb slices were investigated to study the effects of GBs, hydrogen, and dislocations on superconducting properties. Grain orientation and GB misorientation were measured using Laue x-ray diffraction and electron backscattered diffraction (EBSD) analyses. Cryogenic magneto-optical imaging was used to directly observe magnetic flux penetration below T c = 9.3 K. Damage caused by low temperature precipitation of hydrides and their dissolution upon reheating after cryogenic cycles was examined using electron channeling contrast imaging, and EBSD. The relationships between hydride formation, dislocation content, GBs, cryo-cooling, heat treatment (HT), and flux penetration indicate that both GB character and hydrogen content affect magnetic flux penetration. Such flux penetration could be facilitated by dislocation structures and low angle GBs resulting from hydride precipitation and HT.

36 MATERIALS SCIENCE↗

Heat-treated glassy carbon under pressure exhibiting superior hardness, strength and elasticity

Glassy carbon (GC) is a type of non-graphitizing disordered carbon material at ambient pressure and high temperatures, which has been widely used due to its excellent mechanical properties. Here we report the changes in the microstructure and mechanical properties of GC treated at high pressures (up to 5 GPa) and high temperatures. The formation of intermediate sp 2 –sp 3 phases is identified at moderate treatment temperatures before the complete graphitization of GC, by analyzing synchrotron X-ray diffraction, Raman spectra, and transmission electron microscopy images. The intermediate metastable carbon materials exhibit superior mechanical properties with hardness reaching up to 10 GPa and compressive strength reaching as high as 2.5 GPa, nearly doubling those of raw GC, and improving elasticity and thermal stability. The synthesis pressure used in this study can be achieved in the industry on a commercial scale, enabling the scalable synthesis of this type of strong, hard, and elastic carbon materials.

36 MATERIALS SCIENCE↗

Synthesis of δ-Bi2O3/Bi2MoO6 composites with enhanced photocatalytic activity by hydrothermal method

Highlights: • The δ-Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} composites were first synthesized by hydrothermal method. • The product was δ-Bi{sub 2}O{sub 3} rather than α-Bi{sub 2}O{sub 3} with the preset of Bi{sub 2}MoO{sub 6}. • The composites show enhanced photocatalytic activity compared to Bi{sub 2}MoO{sub 6}, α- and δ-Bi{sub 2}O{sub 3}. • The excellent photocatalytic performance was attributed to δ- Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} heterojunctions. - Abstract: The δ-Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} composites were synthesized by hydrothermal method and the microstructure and photocatalytic property were characterized. The X-ray diffraction (XRD) analysis revealed that δ-Bi{sub 2}O{sub 3} was obtained with the existence of Bi{sub 2}MoO{sub 6}, while the product was α-Bi{sub 2}O{sub 3} without Bi{sub 2}MoO{sub 6} under the same experimental condition. The SEM images and the selected area electron diffraction (SAED) patterns have further verified that δ-Bi{sub 2}O{sub 3} was deposited on Bi{sub 2}MoO{sub 6}. The X-ray photoelectron spectroscopy (XPS) spectrum confirmed that the composites were composed of δ-Bi{sub 2}O{sub 3} and Bi{sub 2}MoO{sub 6}, while a fraction of Mo changed from Mo{sup 6+} to Mo{sup 5+}. The coexistence of Mo{sup 5+}/Mo{sup 6+} can be a critical factor in the formation of stable δ-Bi{sub 2}O{sub 3} on Bi{sub 2}MoO{sub 6}. Particularly, the δ-Bi{sub 2}O{sub 3}/Bi{sub 2}MoO{sub 6} photocatalysts possess favorable photocatalytic performance under simulated sunlight illumination since the recombination of photogenerated electrons and holes was inhibited due to the p-n junction at the interface of δ-Bi{sub 2}O{sub 3} and Bi{sub 2}MoO{sub 6}, and the mechanism was discussed in detail.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Calcium-Magnesium-Aluminosilicate (CMAS) Reactions and Degradation Mechanisms of Advanced Environmental Barrier Coatings

The thermochemical reactions between calcium-magnesium-aluminosilicate- (CMAS-) based road sand and several advanced turbine engine environmental barrier coating (EBC) materials were studied. The phase stability, reaction kinetics and degradation mechanisms of rare earth (RE)-silicates Yb2SiO5, Y2Si2O7, and RE-oxide doped HfO2 and ZrO2 under the CMAS infiltration condition at 1500 C were investigated, and the microstructure and phase characteristics of CMAS-EBC specimens were examined using Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD). Experimental results showed that the CMAS dissolved RE-silicates to form crystalline, highly non-stoichiometric apatite phases, and in particular attacking the silicate grain boundaries. Cross-section images show that the CMAS reacted with specimens and deeply penetrated into the EBC grain boundaries and formed extensive low-melting eutectic phases, causing grain boundary recession with increasing testing time in the silicate materials. The preliminary results also showed that CMAS reactions also formed low melting grain boundary phases in the higher concentration RE-oxide doped HfO2 systems. The effect of the test temperature on CMAS reactions of the EBC materials will also be discussed. The faster diffusion exhibited by apatite and RE-doped oxide phases and the formation of extensive grain boundary low-melting phases may limit the CMAS resistance of some of the environmental barrier coatings at high temperatures.

Ahlborg, Nadia L.↗