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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 217 records · Page 12
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Beamline K11 DIAD: a new instrument for dual imaging and diffraction at Diamond Light Source

The Dual Imaging and Diffraction (DIAD) beamline at Diamond Light Source is a new dual-beam instrument for full-field imaging/tomography and powder diffraction. This instrument provides the user community with the capability to dynamically image 2D and 3D complex structures and perform phase identification and/or strain mapping using micro-diffraction. The aim is to enable in situ and in operando experiments that require spatially correlated results from both techniques, by providing measurements from the same specimen location quasi-simultaneously. Using an unusual optical layout, DIAD has two independent beams originating from one source that operate in the medium energy range (7–38 keV) and are combined at one sample position. Here, either radiography or tomography can be performed using monochromatic or pink beam, with a 1.4 mm × 1.2 mm field of view and a feature resolution of 1.2 µm. Micro-diffraction is possible with a variable beam size between 13 µm × 4 µm and 50 µm × 50 µm. One key functionality of the beamline is image-guided diffraction, a setup in which the micro-diffraction beam can be scanned over the complete area of the imaging field-of-view. This moving beam setup enables the collection of location-specific information about the phase composition and/or strains at any given position within the image/tomography field of view. The dual beam design allows fast switching between imaging and diffraction mode without the need of complicated and time-consuming mode switches. Real-time selection of areas of interest for diffraction measurements as well as the simultaneous collection of both imaging and diffraction data of (irreversible) in situ and in operando experiments are possible.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Electron Microscopy Studies of Soft Nanomaterials

This review highlights recent efforts on applying electron microscopy (EM) to soft (including biological) nanomaterials. We will show how developments of both the hardware and software of EM have enabled new insights into the formation, assembly, and functioning (e.g., energy conversion and storage, phonon/photon modulation) of these materials by providing shape, size, phase, structural, and chemical information at the nanometer or higher spatial resolution. Specifically, we first discuss standard real-space two-dimensional imaging and analytical techniques which are offered conveniently by microscopes without special holders or advanced beam technology. The discussion is then extended to recent advancements, including visualizing three-dimensional morphology of soft nanomaterials using electron tomography and its variations, identifying local structure and strain by electron diffraction, and recording motions and transformation by in situ EM. On these advancements, we cover state-of-the-art technologies designed for overcoming the technical barriers for EM to characterize soft materials as well as representative application examples. Here, the even more recent integration of machine learning and its impacts on EM are also discussed in detail. With our perspectives of future opportunities offered at the end, we expect this review to inspire and stimulate more efforts in developing and utilizing EM-based characterization methods for soft nanomaterials at the atomic to nanometer length scales in academic research and industrial applications.

Imaging↗
DOE OSTI2024

Focused‐beam X‐ray fluorescence and diffraction microtomographies for mineralogical and chemical characterization of unsectioned extraterrestrial samples

Abstract This study describes the application of new synchrotron X‐ray fluorescence (XRF) and diffraction (XRD) microtomographies for the 3‐D visualization of chemical and mineralogical variations in unsectioned extraterrestrial samples. These improved methods have been applied to three compositionally diverse chondritic meteorite samples that were between 300 and 400 μm in diameter, including samples prepared from fragments of the CR2 chondrite LaPaz Icefield (LAP) 02342, H5 chondrite MacAlpine Hills (MAC) 88203, and the CM2 chondrite Murchison. The synchrotron‐based XRF and XRD tomographies used are focused‐beam techniques that measure the intensities of fluorescent and diffracted X‐rays in a sample simultaneously during irradiation by a high‐energy microfocused incident X‐ray beam. Measured sinograms of the emitted and diffracted intensities were then tomographically reconstructed to generate 2‐D slices of XRF and XRD intensity through the sample, with reconstructed pixel resolution of 1–2 μm, defined by the resolution of the focused incident X‐ray beam. For sample LAP 02342, primary mineral phases that were visualized in reconstructed slices using these techniques included isolated grains of α‐Fe, orthopyroxene, and olivine. For our sample of MAC 88203, XRF/XRD tomography allowed visualization of forsteritic olivine as a primary mineral phase, a vitrified fusion crust at the sample surface, identification of localized Cr‐rich spinels at spatial resolutions of several micrometers, and imaging of a plagioclase‐rich glassy matrix. In the sample of Murchison, major identifiable phases include clinoenstatite‐ and olivine‐rich chondrules, variable serpentine matrix minerals and small Cr‐rich spinels. Most notable in the tomographic analysis of Murchison is the ability to quantitatively distinguish and visualize the complex mixture of serpentine‐group minerals and associated tochilinite–cronstedtite intergrowths. These methods provide new opportunities for spatially resolved characterization of sample texture, mineralogy, crystal structure, and chemical state in unsectioned samples. This provides researchers an ability to characterize such samples internally with minimal disruption of sample micro‐structures and chemistry, possibly without the need for sample extraction from some types of sampling and capture media.

Geochemistry & Geophysics↗
DOE OSTI2023

Densification and microstructure features of lithium hydride fabrication

The manufacturing of lithium hydride (LiH) utilizing uniaxial pressing, which offers fabrication with tailorable properties via microstructure control, can lead to the expansion in application of LiH while bypassing the challenges presented by historical casting manufacturing techniques. Through control of consolidation conditions such as pressure, temperature, dwell time and powder load, the presented work highlights the densification of LiH, with an emphasis on quantifying oxygen content, for applications requiring a specific density range necessary for optimized material performance. Karl Fischer Titration and X-ray Diffraction proved useful in determining oxygen and phase content while Computed Tomography and Scanning Electron Microscopy provided structural analysis. The temperature dependent densification of LiH fit with an Arrhenius term resulted in an activation energy of 21.2 kJ/mol. Images of fractured surfaces of LiH pressed at 500 °C revealed drastic grain coarsening, aided by the presence of oxygen impurities.

36 MATERIALS SCIENCE↗
DOE OSTI2023

A high-strength precipitation hardened cobalt-free high-entropy alloy

Recent studies on precipitation-hardened high-entropy alloys (HEAs) demonstrate their high strength and thermal stability, making them promising materials for high-temperature structural applications such as nuclear reactors. However, many existing HEAs contain cobalt (Co), which is unsuitable for nuclear applications because of the long-term activation issue of Co. Co is also expensive and considered a critical material for other applications. Therefore, it is desired to exclude Co from the composition. A Co-free (Fe 0.3 Ni 0.3 Mn 0.3 Cr 0.1 ) 88 Ti 4 Al 8 HEA was developed and studied in this work. In contrast to previous Co-free HEAs, this alloy is close to equiatomic in its composition and promises a more pronounced high-entropy effect. Scanning electron microscopy, transmission electron microscopy, atom probe tomography, and synchrotron-based, high-energy X-ray diffraction were used to characterize this alloy and revealed a complex four-phase structure, with an FCC matrix, γ’ precipitates, and a network of B2 and χ phase particles. This structure granted 2151 MPa compressive strength and good thermal stability, but with limited ductility and slow precipitation kinetics. A strengthening analysis of the alloy shows that the B2 and χ provided the most significant strengthening contribution, adding 312 MPa and 788 MPa respectively. Furthermore the strengthening effect from the nanoscale γ' is also considerable, adding 608 MPa in total. This study lays the foundation for the continued development of high-strength Co-free HEAs with improved and satisfactory ductility.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Evolution of micro-pores in Ni–Cr alloys via molten salt dealloying

Porous materials with high specific surface area, high porosity, and high electrical conductivity are promising materials for functional applications, including catalysis, sensing, and energy storage. Molten salt dealloying was recently demonstrated in microwires as an alternative method to fabricate porous structures. The method takes advantage of the selective dissolution process introduced by impurities often observed in molten salt corrosion. This work further investigates molten salt dealloying in bulk Ni–20Cr alloy in both KCl–MgCl 2 and KCl–NaCl salts at 700 °C, using scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffraction (XRD), as well as synchrotron X-ray nano-tomography. Micro-sized pores with irregular shapes and sizes ranging from sub-micron to several microns and ligaments formed during the process, while the molten salt dealloying was found to progress several microns into the bulk materials within 1–16 h, a relatively short reaction time, enhancing the practicality of using the method for synthesis. The ligament size increased from ~ 0.7 μm to ~ 1.3 μm in KCl–MgCl 2 from 1 to 16 h due to coarsening, while remaining ~ 0.4 μm in KCl–NaCl during 16 h of exposure. The XRD analysis shows that the corrosion occurred primarily near the surface of the bulk sample, and Cr 2 O 3 was identified as a corrosion product when the reaction was conducted in an air environment (controlled amount sealed in capillaries); thus surface oxides are likely to slow the morphological coarsening rate by hindering the surface diffusion in the dealloyed structure. 3D-connected pores and grain boundary corrosion were visualized by synchrotron X-ray nano-tomography. This study provides insights into the morphological and chemical evolution of molten salt dealloying in bulk materials, with a connection to molten salt corrosion concerns in the design of next-generation nuclear and solar energy power plants.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Technology Enabling Zero-EPZ Micro Modular Reactors: Fabrication of Zirconium Hydride with Controlled Hydrogen Loading

This report completes Milestone M2.2.2 - ZrH pellet fabricated with controlled hydride loading: ZrH1.5±0.1 single phase pellets fabricated with controlled and thermally stable hydride loading. Hydrogen content to be quantified and single-phase confirmed by X-ray diffraction. In this milestone, we report the successful fabrication of delta-phase zirconium hydride pellets using the ORNL bulk metal hydriding system. The successful deployment of zirconium hydride moderator in advanced reactors requires development of a consistent and affordable production pathway along with implementation of a hydrogen retention solution throughout the reactor life. Fabrication of delta-phase zirconium hydride is challenging since the absorption of a large amount of hydrogen into alpha-zirconium induces significant volume expansion and the present hydrogen concentration gradient results in cracking. A fully programmable hydriding system with continuous hydrogen partial pressure and flow control to facilitate processing of massive metal hydride has been developed at ORNL. In this report, the working principle of the hydriding system will be introduced. Characterization of the produced zirconium hydride includes X-ray powder diffraction to identify the present phases and X-ray Computed Tomography to visualize the internal microstructure (including cracks). The results indicate that single delta-phase zirconium hydride pellets with various sizes have been successfully produced.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Analysis of Coronado State Historic Site artifacts using X-rays

Two historic-period metal artifacts were provided by the New Mexico Historic Sites to Los Alamos National Laboratory for non-destructive analysis. The artifacts were a crossbow quarrel (or bolthead) and a reliquary pendant recovered from Kuaua Pueblo (also known as the Coronado Historic Site) in Bernalillo, NM. The quarrel is a heavily patinated metal that had been flattened due to compressive forces. The pendant consisted of a metal casing that had previously surrounded two center gemstones on the front and rear face of the pendant. The gemstone in the rear setting had fractured and was displaced from the setting, leaving only a small, loose fragment within the pendant for study. The front gem appeared to be very dark, near-black in color, and the fragment of the rear gem was a bright red color. The artifacts were analyzed to ascertain their composition and glean insight into their provenance using the following X-ray techniques: X-ray computed tomography, confocal micro X-ray fluorescence, and X-ray diffraction. Infrared spectroscopy and electron microscopy were used on selected areas. Ultraviolet Raman spectra were collected on the two gems and the pendant. The metal material of the artifacts was found to be primarily composed of copper. The gems in the pendant were composed of manganese (front gem) and calcium (side gem).

36 MATERIALS SCIENCE↗
NASA NTRS1991

Verifying X-Radiographs With Computed Tomographs

Nondestructive technique gives added confidence in inspection. Ambiguous indications in radiographic inspections of metal castings checked by computed tomography. Fast and inexpensive conventional x-ray inspection used to make film image of overall casting, and slower, more costly computed tomography used to reinspect relatively few parts of casting presenting possible diffraction patterns or other difficult-to-interpret features. Method effective in resolving ambiguities in radiographs of turbine blades. Provides same information as metallurgical sectioning.

Roy, Jagatjit↗
DOE OSTI2026

Optical interference for the guidance of cryogenic focused ion beam milling beyond the axial diffraction limit

Cryogenic focused ion beam (Cryo-FIB) milling has become a standard step in the cryogenic electron tomography (Cryo-ET) workflow and is required to thin cells to electron-semitransparency. However, this destructive process removes the vast majority of the cellular material and raises a critical question: what thin section should be preserved for Cryo-ET analysis? Using a tri-coincident cryogenic FIB-SEM-LM system, we identify an interferometric optical response that can be used for targeting lamella production to fluorescently labeled structures with accuracy beyond the diffraction limit. Here we demonstrate this approach using synthetic samples of fluorescent beads embedded in micron-scale droplets of amorphous ice. We then apply the approach to capture virions inside host cells. Successful targeting is confirmed by Cryo-ET revealing clusters of virions in intracellular vesicles. The method does not require any fluorescent fiducials or axial registration and can be performed on any fluorescently labeled structure that is visible in widefield fluorescence microscopy.

Cryoelectron microscopy↗
DOE OSTI2025

Model-based iterative reconstruction with adaptive regularization for artifact reduction in electron tomography

Obtaining high-quality 3D reconstructions from electron tomography of crystalline particles embedded in lighter support elements is crucial for various material systems such as catalysts for fuel cell applications. However, significant challenges arise due to the limited tilt range, sparse and low signal-to-noise ratio of the measurements. In addition, small metal particles can cause strong streaking and shading artifacts in the 3D reconstructions when using conventional reconstruction algorithms due to the presence of Bragg diffraction and the large scattering cross-section difference between the materials of the particles and the background support regions. These artifacts lead to errors in the downstream characterization affecting extraction of critical features such as the size of the metal particles, their distribution and the volume of the lighter support regions. In this paper, we present a two-stage algorithm based on metal artifact reduction, utilizing model-based iterative reconstruction methods with adaptive adjustment of regularization parameters. Our approach yields high-quality 3D reconstructions compared to traditional algorithms, accurately capturing both the metal particles as well as the background support. We demonstrate the effectiveness of our algorithm through simulated and experimental bright-field electron tomography data, showing significant improvements in reconstruction quality compared to traditional methods.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2021

X-ray diffraction and in situ pressurization of dentine apatite reveals nanocrystal modulus stiffening upon carbonate removal

Bone-like materials comprise carbonated-hydroxyapatite nanocrystals (c-Ap) embedding a fibrillar collagen matrix. The mineral particles stiffen the nanocomposite by tight attachment to the protein fibrils creating a high strength and toughness material. The nanometer dimensions of c-Ap crystals make it very challenging to measure their mechanical properties. Mineral in bony tissues such as dentine contains 2~6 wt.% carbonate with possibly different elastic properties as compared with crystalline hydroxyapatite. Here we determine strain in biogenic apatite nanocrystals by directly measuring atomic deformation in pig dentine before and after removing carbonate. Transmission electron microscopy revealed the platy 3D morphology while atom probe tomography revealed carbon inside the calcium rich domains. High-energy X-ray diffraction in combination with in situ hydrostatic pressurization quantified reversible c-Ap deformations. Additionally, crystal strains differed between annealed and ashed (decarbonated) samples, following 1 or 10 h heating at 250 °C or 550 °C respectively. Measured bulk moduli (K) and a-/c-lattice deformation ratios (η) were used to generate synthetic K syn and ηsyn identifying the most likely elastic constants C 33 and C 13 for c-Ap. These were then used to calculate the nanoparticle elastic moduli. For ashed samples, we find an average E 11 =107 GPa and E 33 =128 GPa corresponding to ~5% and ~17% stiffening of the a-/c-axes of the nanocrystals as compared with the biogenic nanocrystals in annealed samples. Ashed samples exhibit ~10% lower Poisson's ratios as compared with the 0.25~0.36 range of carbonated apatite. Carbonate in c-Ap may therefore serve for tuning local deformability within bony tissues.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In situ X-ray and IR probes relevant to Earth science at the Advanced Light Source at Lawrence Berkeley Laboratory

Access to synchrotron X-ray facilities has become an important aspect for many disciplines in experimental Earth science. This is especially important for studies that rely on probing samples in situ under natural conditions different from the ones found at the surface of the Earth. The non-ambient condition Earth science program at the Advanced Light Source (ALS), Lawrence Berkeley National Laboratory, offers a variety of tools utilizing the infra-red and hard X-ray spectrum that allow Earth scientists to probe Earth and environmental materials at variable conditions of pressure, stress, temperature, atmospheric composition, and humidity. These facilities are important tools for the user community in that they offer not only considerable capacity (non-ambient condition diffraction) but also complementary (IR spectroscopy, microtomography), and in some cases unique (Laue microdiffraction) instruments. The availability of the ALS’ in situ probes to the Earth science community grows especially critical during the ongoing dark time of the Advanced Photon Source in Chicago, which massively reduces available in situ synchrotron user time in North America.

58 GEOSCIENCES↗
DOE OSTI2017

The effect of carbon on the microstructures, mechanical properties, and deformation mechanisms of thermo-mechanically treated Fe 40.4 Ni 11.3 Mn 34.8 Al 7.5 Cr 6 high entropy alloys

We investigated the effects of cold rolling followed by annealing on the mechanical properties and dislocation substructure evolution of undoped and 1.1 at. % carbon-doped Fe 40.4 Ni 11.3 Mn 34.8 Al 7.5 Cr 6 high entropy alloys (HEAs). X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atom probe tomography (APT) were employed to characterize the microstructures. The as-cast HEAs were coarse-grained and single phase f.c.c., whereas the thermo-mechanical treatment caused recrystallization (to fine grain sizes) and precipitation (a B2 phase for the undoped HEA; and a B2 phase, and M 23 C 6 and M 7 C 3 carbides for the C-doped HEA). Carbon, which was found to have segregated to the grain boundaries using APT, retarded recrystallization. The reduction in grain size resulted in a sharp increase in strength, while the precipitation, which produced only a small increase in strength, probably accounted for the small decrease in ductility for both undoped and C-doped HEAs. For both undoped and C-doped HEAs, the smaller grain-sized material initially exhibited higher strain hardening than the coarse-grained material but showed a much lower strain hardening at large tensile strains. Wavy slip in the undoped HEAs and planar slip in C-doped HEAs were found at the early stages of deformation irrespective of grain size. At higher strains, dislocation cell structures formed in the 19 μm grain-sized undoped HEA, while microbands formed in the 23 μm grain-sized C-doped HEA. Conversely, localized dislocation clusters were found in both HEAs at the finest grain sizes (5 μm). The inhibition of grain subdivision by the grain boundaries and precipitates lead to the transformation from regular dislocation configurations consisting of dislocation-cells and microbands to irregular dislocation configurations consisting of localized dislocation clusters, which further account for the decrease in ductility. Our investigation of the formation mechanism and strain hardening of dislocation cells and microbands could benefit future structural material design.

36 MATERIALS SCIENCE↗
DOE OSTI2021

On the existence of orthorhombic martensite in a near-α titanium base alloy used for additive manufacturing

Additive manufacturing is a state-of-the-art production technology to produce tailor-made and highly complex parts. Among various other alloys, Ti base alloys are frequently used in this manufacturing technique due to their well-balanced properties and their wide range of applications. Allotropic phases and the occurrence of athermal phase transformations are the main reasons why these alloys hold a great development potential and are the basis of extensive use. High cooling rates during manufacturing lead to martensitic phases and the formation of nanometer-sized microstructures resulting in extraordinary strength. Simultaneously, such high cooling rates cause a high amount of lattice defects and the occurrence of residual stresses, which finally may result in delamination effects and cracks. Usually, a common approach to reduce residual stresses during additive manufacturing is to decrease thermal gradients by increasing the heat input or preheating the building platform. Instead of applying the typical approaches to lower thermal gradients, this study deals with the origin of the ‘softer’ orthorhombic martensite by accelerating the solidification process. The implementation of the orthorhombic phase in bulk components was inspired by a new phase transformation herein reported for the first time in the powder material, which also validates the possible occurrence of two martensitic phases in the same alloy. Various sophisticated characterization techniques like high energy and high-temperature X-ray diffraction, high-resolution transmission electron microscopy as well as atom probe tomography were applied to characterize this softer orthorhombic martensitic phase in detail aiming to highlight the opportunities accompanied by this new approach for additive manufacturing of titanium alloys.

36 MATERIALS SCIENCE↗