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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Nanoscale elemental mapping reveals the effect of light and temperature on Gephyrocapsa huxleyi coccoliths

Coccolithophores produce vast quantities of stable calcium carbonate coccoliths, occupying the distinctive position as one of the most productive calcifying organisms on Earth. Gephyrocapsa huxleyi, the most abundant species of coccolithophores across modern oceans, plays an important role in the biological carbon pump and may serve as inspiration for nature-based carbon capture and sequestration technologies. Despite intensive study into G. huxleyi, the biological mechanisms of coccolith synthesis remain unclear. Here, we employ synchrotron X-ray fluorescence to quantitatively map elemental incorporation (calcium, Ca; strontium, Sr; sulfur, S; iron, Fe; and silicon, Si) into G. huxleyi coccoliths at 40-nanometer resolution. Trace elements play a role in determining the thermodynamic stability of coccolith carbonate sequestration and may provide insight into unknown mechanisms of coccolithogenesis. Although the coccolith Sr/Ca ratio has been widely applied as a paleoceanographic proxy, understanding of the Sr/Ca phenomena is limited. Our results confirm that Sr/Ca is temperature dependent but challenge the hypothesis that growth rate is a primary determinant. We find that increased light irradiance led to an ~30% decrease in calcium incorporated into the coccoliths. Surprisingly, X-ray fluorescence spectra and mapping revealed evidence of sulfur, at approximately three times the concentration of Sr, embedded in and around the calcite matrix, suggesting that G. huxleyi coccoliths may play an expanded role in the global sulfur cycle. Here, based on our elemental maps, we postulate that sulfur is active in the intracellular coccolith vesicle and plays a direct role in formation of G. huxleyi coccoliths.

36 MATERIALS SCIENCE↗
DOE OSTI2023

EDS-PhaSe: Phase Segmentation and Analysis from EDS Elemental Map Images Using Markers of Elemental Segregation

Scanning electron microscopy (SEM), combined with energy-dispersive spectroscopy (EDS), is an extensively used technique for in-depth microstructural analysis. Here, we present the EDS-Phase Segmentation (EDS-PhaSe) tool that enables phase segmentation and phase analysis using the EDS elemental map images. Importantly, it converts the EDS map images into estimated composition maps for calculating markers of selective elemental redistribution in the scanned area and creates a phase-segmented micrograph while providing approximate fraction and composition of each identified phase. EDS-PhaSe offers two unique advantages. Firstly, it enables the direct processing of EDS elemental map images without requiring any raw or proprietary data/software, thereby allowing the analysis of EDS results available in the published literature as images. Secondly, it enables segmentation and analysis of phases even when the phase contrast is missing in backscattered micrographs, assisting in correlating the XRD and SEM-EDS data as shown in this work for a AlCoCrFeNi high-entropy alloy.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Proof of principle study: synchrotron X-ray fluorescence microscopy for identification of previously radioactive microparticles and elemental mapping of FFPE tissues

Biobanks containing formalin-fixed, paraffin-embedded (FFPE) tissues from animals and human atomic-bomb survivors exposed to radioactive particulates remain a vital resource for understanding the molecular effects of radiation exposure. These samples are often decades old and prepared using harsh fixation processes which limit sample imaging options. Optical imaging of hematoxylin and eosin (H&E) stained tissues may be the only feasible processing option, however, H&E images provide no information about radioactive microparticles or radioactive history. Synchrotron X-ray fluorescence microscopy (XFM) is a robust, non-destructive, semi-quantitative technique for elemental mapping and identifying candidate chemical element biomarkers in FFPE tissues. Still, XFM has never been used to uncover distribution of formerly radioactive micro-particulates in FFPE canine specimens collected more than 30 years ago. In this work, we demonstrate the first use of low-, medium-, and high-resolution XFM to generate 2D elemental maps of ~ 35-year-old, canine FFPE lung and lymph node specimens stored in the Northwestern University Radiobiology Archive documenting distribution of formerly radioactive micro-particulates. Additionally, we use XFM to identify individual microparticles and detect daughter products of radioactive decay. The results of this proof-of-principle study support the use of XFM to map chemical element composition in historic FFPE specimens and conduct radioactive micro-particulate forensics.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2020

Sample preparation with sucrose cryoprotection dramatically alters Zn distribution in the rodent hippocampus, as revealed by elemental mapping

Transition metal ions (Fe, Mn, Cu, Zn) are essential for healthy brain function, but altered concentration, distribution, or chemical form of the metal ions has been implicated in numerous brain pathologies. Currently, it is not possible to image the cellular or sub-cellular distribution of metal ions in vivo and therefore, studying brain-metal homeostasis largely relies on ex vivo in situ elemental mapping. Sample preparation methods that accurately preserve the in vivo elemental distribution are essential if one wishes to translate the knowledge of elemental distributions measured ex vivo toward increased understanding of chemical and physiological pathways of brain disease. Furthermore, the choice of sample preparation is particularly important for metal ions that exist in a labile or mobile form, for which the in vivo distribution could be easily distorted by inappropriate sample preparation. One of the most widely studied brain structures, the hippocampus, contains a large pool of labile and mobile Zn. Herein, we describe how sucrose cryoprotection, the gold standard method of preparing tissues for immuno-histochemistry or immuno-fluorescence, which is also often used as a sample preparation method for elemental mapping studies, drastically alters hippocampal Zn distribution. Based on the results of this study, in combination with a comparison against the strong body of published literature that has used either rapid plunge freezing of brain tissue, or sucrose cryo-protection, we strongly urge investigators in the future to cease using sucrose cryoprotection as a method of sample preparation for elemental mapping, especially if Zn is an analyte of interest.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Exploration of LIBS as a novel and rapid elemental mapping technique of nuclear fuels in the form of surrogate TRISO particles

Laser-induced breakdown spectroscopy (LIBS) was employed to characterize coatings on surrogate fuel particles. Tri-structural isotropic (TRISO) particles are a proposed nuclear fuel alternative for high temperature reactors. These particles are constructed of a ZrO 2 kernel (as a surrogate to uranium), surrounded by an inner pyrolytic carbon layer and are surrounded by an outer carbide layer (ZrC, presented here) to act as a barrier to fission products generated during nuclear reactions. These particles are embedded within a graphite compact and housed within the reactor core. Simply put, due to their robust nature, performing elemental analysis of these particles poses a challenge. Presented here, LIBS is explored as a method for characterizing elemental constituents of these particles, with the focus being on rapid elemental mapping and depth profiling. Different from traditional elemental analysis techniques (e.g., inductively coupled plasma – based methods), LIBS is advantageous because it can directly analyze the sample surface and can detect light elements such as C and O, making it a viable technique for the analysis of small, multilayered particles as spatial elemental information is warranted in the production of these particles. In the work presented here, LIBS was successfully used for discerning small layers (30–50 μm), detecting the location of carbon and oxygen layers, providing fast 2-D mapping (<5 min per particle) and rapid depth profiling (10 s per particle).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Nanoscale Elemental Mapping of Intact Solid–Liquid Interfaces and Reactive Materials in Energy Devices Enabled by Cryo-FIB/SEM

Many modern energy devices rely on solid–liquid interfaces, highly reactive materials, or both, for their operation and performance. The difficulty of characterizing such materials means these devices often lack high-resolution characterization in an unaltered state. Here, we demonstrate how cryogenic sample preparation and transfer can extend the capabilities of FIB/SEM techniques to solid–liquid interfaces and reactive materials common to energy devices by preserving their integrity through all stages of preparation and characterization. We additionally show how cryo-FIB/SEM paired with energy dispersive X-ray spectroscopy enables nanoscale elemental mapping of cross-sections produced in these materials and discuss strategies to achieve optimal results. Finally, we consider current limitations of the technique and propose future developments that could enhance its capabilities. Our results illustrate that cryo-FIB/SEM will be a useful technique for fields where solid–liquid interfaces or reactive materials play an important role and could, thus far, not be characterized at high resolution.

25 ENERGY STORAGE↗
NASA NTRS2014

Comparison of Nickel XANES Spectra and Elemental Maps from a Ureilite, a LL3.8 Ordinary Chondrite, Two Carbonaceous Chondrites and Two Large Cluster IDPs

Nickel in the extraterrestrial world is commonly found in both Fe-Ni sulfide and Fe-Ni met-al forms [1] and in the pure metal state in the interior of iron meteorites where it is not easily oxidized. Ni is also found in olivine, pyroxene and glasses and in some melts the partitioning of Ni between the olivines and glass is controlled by the amount of S in the melt [2]. Its most common valence state is Ni(2+) but Ni also occurs as Ni(0), Ni(+), and Ni(3+) and rarely as Ni(2-), Ni(1-) and Ni(4+) [3]. It's valence state in olivines is Ni(2+) in octa-hedral coordination on the M1 site and rarely on the M2 site.[4]. The chemical sensitivity of X-ray absorp-tion near-edge structure (XANES) spectroscopy is well established and can be used to determine not only va-lence states but also coordination sites [5]. We report here Ni XANES spectroscopy and elemental maps collected from 2 carbonaceous chondrites, 2 large clus-ter IDPs, 1 ureilite and 1 LL3 orginary chondrite.Using XANES it may be possible to find a common trait in the large cluster IDPs that will also be found in mete-orite samples.

Wirick, S.↗
NASA NTRS2004

Element Mapping in Anhydrous IDPs: Identification of the Host Phases of Major/Minor Elements as a Test of Nebula Condensation Models

Many anhydrous interplanetary dust particles (IDPs) are the most pristine samples of primitive solar system dust currently available for laboratory analysis. Their primitive nature is demonstrated by: 1) the high content of moderately volatile elements, indicating they have not been heated significantly since formation, 2) the absence of hydrated material, indicating they never experienced aqueous processing, 3) the presence of unequilibrated mineral assemblages, 4) the presence of large isotopic anomalies (e.g., D and 15N enrichment), in these IDPs.

Flynn, G. J.↗
NASA NTRS1993

Gamma Ray/neutron Spectrometers for Planetary Elemental Mapping

Los Alamos has designed gamma ray and neutron spectrometers for Lunar Scout, two robotic missions to map the Moon from 100 km polar orbits. Knowledge of the elemental composition is desirable in identifying resources and for geochemical studies and can be obtained using gamma ray and neutron spectrometers. Measurements with gamma ray and neutron spectrometers complement each other in determining elemental abundances in a planet's surface. Various aspects of the instruments are discussed.

Reedy, R. C.↗
NASA NTRS2011

A Radiation-Hard Silicon Drift Detector Array for Extraterrestrial Element Mapping

Measurement of x-rays from the surface of objects can tell us about the chemical composition Absorption of radiation causes characteristic fluorescence from material being irradiated. By measuring the spectrum of the radiation and identifying lines in the spectrum, the emitting element (s) can be identified. This technique works for any object that has no absorbing atmosphere and significant surface irradiation : Our Moon, the icy moons of Jupiter, the moons of Mars, the planet Mercury, Asteroids and Comets

Gaskin, Jessica↗
NASA NTRS2004

Sub-Micrometer Scale Minor Element Mapping in Interplanetary Dust Particles: A Test for Stratospheric Contamination

Combined X-ray microprobe (XRM), energy dispersive x-ray fluorescence using a Transmission Electron Microscope (TEM), and electron microprobe measurements have determined that the average bulk chemical composition of the interplanetary dust particles (IDPs) collected from the Earth s stratosphere is enriched relative to the CI meteorite composition by a factor of 2 to 4 for carbon and for the moderately volatile elements Na, K, P, Mn, Cu, Zn, Ga, Ge, and Se, and enriched to approximately 30 times CI for Br. However, Jessberger et al., who have reported similar bulk enrichments using Proton Induced X-ray Emission (PIXE), attribute the enrichments to contamination by meteor-derived atmospheric aerosols during the several weeks these IDPs reside in the Earth s atmosphere prior to collection. Using scanning Auger spectroscopy, a very sensitive surface analysis technique, Mackinnon and Mogk have observed S contamination on the surface of IDPs, presumably due to the accretion of sulfate aerosols during stratospheric residence. But the S-rich layer they detected was so thin (approximately 100 angstroms thick) that the total amount of S on the surface was too small to significantly perturb the bulk S-content of a chondritic IDP. Stephan et al. provide support for the contamination hypothesis by reporting the enrichment of Br on the edges of the IDPs using Time-of-Flight Secondary-Ion Mass-Spectrometry (TOFSIMS), but TOF-SIMS is notorious for producing false edge-effects, particularly on irregularly-shaped samples like IDPs. Sutton et al. mapped the spatial distribution of Fe, Ni, Zn, Br, and Sr, at the approximately 2 m scale, in four IDPs using element-specific x-ray fluorescence (XRF) computed microtomography. They found the moderately volatile elements Zn and Br, although spatially inhomogeneous, were not concentrated on the surface of any of the IDPs they examined, suggesting that the Zn and the Br enrichments in the IDPs are not due to contamination during stratospheric residence.

Flynn, G. J.↗
DOE OSTI2025

LABQ3: Bayesian method for quantification of mineral compositions and nano-scale elemental mapping of 3D synchrotron XCT data

Quantitative analysis of mineral compositions is essential in understanding geochemical, mineralogical and environmental processes. Fine-resolution 3D imaging is widely done using synchrotron X-ray computed tomography (XCT), but existing analyses are limited to visualization and segmentation. This paper presents a new method, Linear Attenuation Bayesian Quantitative 3D-mapper (LABQ3), based on the linearity of X-ray attenuation with respect to elemental concentrations. To address the random variability in attenuation measurements, LABQ3 employs Bayesian decision theory to minimize classification error, using reference attenuation distributions from scans of pure mineral standards. To demonstrate LABQ3 and test its performance, we studied precipitated carbonate samples. XCT scans were done at multiple energies using the transmission X-ray microscope (TXM) at beamline 32-ID-C of the Advanced Photon Source at Argonne National Laboratory. The reconstructed 3D images have a voxel size of 20 nm. Analyses revealed rich nano-scale compositional heterogeneity within individual particles. A mixture of calcium and cadmium produced an overall stoichiometric composition of (Ca 0.78 ,Cd 0.22 )CO 3 , with some voxels containing nearly pure CdCO 3 . The addition of zinc led to an overall stoichiometric composition of 33% Ca, 28% Cd, 39% Zn, with a nearly pure CaCO 3 core and compositional zonation through the rim. These compositional gradients are related to temporal sequences of carbonate mineral formation where Cd precipitated at the beginning in (Ca,Cd)CO 3 , while Cd and Zn precipitated at the end in (Ca, Cd,Zn)CO 3 . Results differ from bulk analyses using Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), showing that LABQ3 provides particle-specific insights. LABQ3 distinguishes itself by quantifying chemical compositions along a continuum, making it different from XCT analyses based on segmentation. LABQ3 allows simultaneous acquisition of morphology and chemical composition in 3D, facilitating the interpretation of chemical gradients of trace elements, quantification of solid solution compositions, inferences about temporal sequences of mineral precipitation, and addressing other concerns about solid-phase chemistry.

58 GEOSCIENCES↗
DOE OSTI2022

Chemical and elemental mapping of spent nuclear fuel sections by soft X-ray spectromicroscopy

Soft X-ray spectromicroscopy at the O K -edge, U N 4,5 -edges and Ce M 4,5 -edges has been performed on focused ion beam sections of spent nuclear fuel for the first time, yielding chemical information on the sub-micrometer scale. To analyze these data, a modification to non-negative matrix factorization (NMF) was developed, in which the data are no longer required to be non-negative, but the non-negativity of the spectral components and fit coefficients is largely preserved. The modified NMF method was utilized at the O K -edge to distinguish between two components, one present in the bulk of the sample similar to UO 2 and one present at the interface of the sample which is a hyperstoichiometric UO 2+ x species. The species maps are consistent with a model of a thin layer of UO 2+ x over the entire sample, which is likely explained by oxidation after focused ion beam (FIB) sectioning. In addition to the uranium oxide bulk of the sample, Ce measurements were also performed to investigate the oxidation state of that fission product, which is the subject of considerable interest. Analysis of the Ce spectra shows that Ce is in a predominantly trivalent state, with a possible contribution from tetravalent Ce. Atom probe analysis was performed to provide confirmation of the presence and localization of Ce in the spent fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2019

Simultaneous three-dimensional elemental mapping of Hollandite and Pyrochlore material phases in ceramic waste form materials

In this study, differential X-ray absorption contrast tomography was performed on model ceramic composite systems to image the 3D spatial distributions of Ga and Nd containing phases. The model material systems were fabricated such that they contained two constituent phases. Ga–doped Ba hollandite (Ba 1.33 Ga 2.66 Ti 5.34 O 16 ), and pyrochlore (Nd 2 Ti 2 O 7 ) which are under consideration as nuclear waste immobilization matrices. Two complementary techniques have been used to characterize the 3D distribution of phases. The analysis suggests that the 3D spatial distributions of hollandite and pyrochlore can be readily identified through the distributions Ga and Nd, respectively. These results represent a critical development towards characterizing the complex microstructure inherent to practical materials such as multiphase ceramic composite waste forms. Furthermore, these methods can be applied to elucidate microstructural features that fundamentally determine the performance and properties of complex systems, which is central to the design of durable waste forms as well as many other real materials such fuel cells, batteries, ultra-high temperature ceramics.

36 MATERIALS SCIENCE↗
NASA NTRS1992

High-resolution Elemental Mapping of the Lunar Surface

New instruments and missions are being proposed to study the lunar surface as a result of the resurgence of interest in returning to the Moon. One instrument recently proposed is similar in concept to the x-ray fluorescence detectors flown on Apollo, but utilizes fluorescence from the L- and M-shells rather than the K-shell. This soft X-Ray Flourescence Imager (XRFI) is discussed.

Edwards, Bradley C.↗
NASA NTRS2014

Development of Genesis Solar Wind Sample Cleanliness Assessment: Initial Report on Sample 60341 Optical Imagery and Elemental Mapping

Since 2005 the Genesis science team has experimented with techniques for removing the contaminant particles and films from the collection surface of the Genesis fragments. A subset of ~40 samples have been designated as "cleaning matrix" samples. These are small samples to which various cleaning approaches are applied and then cleanliness is assessed optically, by TRXRF, SEM, ToF-SIMS, XPS, ellipsometry or other means [1-9]. Most of these sam-ples remain available for allocation, with cleanliness assessment data. This assessment allows evaluation of various cleaning techniques and handling or analytical effects. Cleaning techniques investigated by the Genesis community include acid/base etching, acetate replica peels, ion beam, and CO2 snow jet cleaning [10-16]. JSC provides surface cleaning using UV ozone exposure and ultra-pure water (UPW) [17-20]. The UPW rinse is commonly used to clean samples for handling debris between processing by different researchers. Optical microscopic images of the sample taken before and after UPW cleaning show what has been added or removed during the cleaning process.

Gonzalez, C. P.↗