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Carbon Tracers of Aqueous Processes: Isotopic Analysis of Cr Carbonate Grains With Implications for Bennu Samples

Carbonate grains in carbonaceous chondrites record aqueous alteration events on the asteroidal parent bodies, including evidence for episodic alteration, timing of alteration, and time and temperature evolution of volatiles. Spectral features in the 3.4 μm region at asteroid Bennu have been interpreted as coming from carbonate minerals. Coordinated analysis of carbonate grains will be a valuable tool for analysis of Bennu samples, and related analysis of analog materials provides important context for understanding aqueous alteration of carbonaceous asteroids more broadly. To that end, our team is analyzing carbonates in Bennu analog materials, using Raman spectroscopy to identify carbonates and assess the maturity of related organic materials, vacuum reflectance spectroscopy from the ultraviolet through thermal infrared range to constrain contributions from carbonates and organics, X-ray microtomography and electron probe microanalysis (EPMA) to assess the distribution of void space, transmission electron microscopy to characterize space weathering effects, and EPMA and secondary ion mass spectrometry (SIMS) to measure composition and isotopic ratios. Here, we describe in situ analysis of carbon and oxygen isotopes from carbonates in Grosvenor Mountains (GRO) 95577.

K E Miller↗
DOE OSTI2020

Computational Methods to Accelerate Development of Corrosion Resistant Coatings for Industrial Gas Turbines

Oxidation resistant overlay coatings protect the underlying superalloy component in industrial gas turbines from oxidation attack. Rate of depletion of the Al-rich β-phase in the bond coat governs the lifetime of these coatings. The applicability of a computational method in accelerating the development of corrosion resistant coatings and significantly reducing the extensive experimental effort to predict coating lifetimes and microstructural changes in three-coated Ni-based superalloys for real operational durations (20–40 kh) was undertaken in the present study. Scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and electron microprobe analysis (EPMA) were employed to characterize MCrAlY-coated superalloy substrates (1483, 247 and X4) after exposure at 900 °C in air + 10% H 2 O for up to 20,000 h. The model predicted the longest coating lifetime for the coating on X4 substrate. Precipitation of γ' in the coatings was correctly predicted for all three coating systems. Additionally, the model was able to predict the formation of topologically close packed (TCP)-phases in the investigated coating systems.

Pillai, Rishi R.↗
DOE OSTI2026

Characterizing microscale signatures in uranium ore concentrates using electron probe microanalyzer

Impurities in uranium ore concentrates (UOCs) serve as forensic signatures of processing history and origin. Here, this study utilizes Electron Probe Microanalyzer (EPMA) to characterize microscale compositional and textural features in individual UOC particles from both commercial and bench-scale production. At the particle scale, multiple internal phases with distinct morphologies, chemical signatures, and stoichiometries are documented. Our data shows that chemical impurities are heterogeneously distributed within single particles and among particles within a sample. These microscale heterogeneities correlate with known processing histories, indicating that microscale signatures of early fuel cycle materials can provide valuable information for nuclear forensic material analysis.

organic↗
DOE OSTI2026

Metal alloy microparticle tagging of UO 2 fuel pellets for nuclear forensics

A tagging strategy for UO 2 fuel pellets will be discussed which involves the creation of alloyed metal microparticles that can be tuned to create a unique identification (“barcode”) indicating provenance of the pellets. These specialized markers would contain high temperature resistant materials, such as Ti, Mo, and Cr, in small quantities such that they do not interfere with the performance of the pellets but are recoverable by standard analytical techniques. The Amazemet rePowder ultrasonic atomization system was used to manufacture the microparticles, and sample pellets were fabricated and sintered containing these dopants. Various techniques, such as Scanning Electron Microscopy (SEM) and Electron Probe Microanalysis (EPMA), were used to evaluate these sample pellets to determine if particles (and their alloy compositions) were recoverable. Details on how the particles were manufactured and characterized will be detailed, as well as results from their incorporation into test pellets. Next steps will involve the scale of this technique using more conventional mass production methods, as well as the implementation of other alloys.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Structural and Electronic Properties of Indium-Doped n-type Cd-Se-Te Crystals

Here, we present a comprehensive investigation into the potential of n-type indium-doped cadmium selenide telluride (CST:In) as a high-performance candidate for solar cell applications, without the need for resource-intensive post-growth treatments that are required for CdTe:In. We compared undoped CST and CST:In crystals under different growth conditions, analyzing their structural and electronic properties using x-ray diffraction (XRD), electron probe microanalysis (EPMA), current-voltage (IV) and Hall effect measurements, time-resolved photoluminescence (TRPL), optical transmission, and photoluminescence (PL) mapping. The results reveal that as-grown CST:In crystals achieve nearly 100% carrier activation, yielding an electron concentration of 9.5x1018 cm -3 , mobility of 653 cm 2 /V.s and a 5 ns lifetime which approaches the radiative limit. Furthermore, comparison of PL maps from crystal growths having different cooling profiles suggests a strong effect of cooling rate on selenium segregation and cubic/hexagonal/polytype phase distribution. Slower cooling leads to a more homogeneous cubic structure with lower Se segregation, while a faster cooling rate results in increased Se segregation, and twin boundaries and stacking faults with polytypic and hexagonal character.

14 SOLAR ENERGY↗
DOE OSTI2025

Microstructure characteristics of LPBF&HIP fabricated graded composite transition joint between ferritic steel and austenitic stainless steel

Graded composite transition joints (GCTJs) offer a promising alternative to conventional dissimilar metal welds (DMWs) by enabling smooth compositional and microstructural transitions. However, GCTJs fabricated solely through additive manufacturing (AM) face challenges such as heat accumulation, complex parameter control, and elemental segregation. In this study, we propose a novel approach that relies on AM to design a spatially graded structure in one alloy and then employs hot isostatic pressing (HIP) as a diffusion bonding method to join it with a second alloy. Here, this method combines the flexibility of AM with the powder net-shaping advantage of HIP. Specifically, a series of closely packed austenitic stainless steel 304 conical structures were printed using laser powder bed fusion (LPBF) and then combined with ferritic steel P91 powder via HIP. By using electron backscatter diffraction (EBSD), electron probe microanalysis (EPMA), and transmission electron microscopy (TEM) techniques, the microstructure characteristics of the GCTJ of 304&P91, especially the interdiffusion zone (IDZ), have been systematically investigated. The microstructure at the interface transitions from austenite-ferrite (A+F) to austenite-martensite-ferrite (A+M+F), and finally to martensite-ferrite (M+F) due to diffusion. Additionally, the diffusion width between 304 and P91 increases with the volume fraction of P91. This unique design also ensures a gradual transition in both hardness and thermal expansion coefficient from 304 to P91, thereby enabling a smooth gradient in functional properties. Overall, this study proposes a novel approach for fabricating GCTJs and contributes to advancing design concepts in the field of dissimilar metal joining.

Additively manufacturing (AM)↗
DOE OSTI2021

Deterioration mechanism of alkali-activated materials in sulfuric acid and the influence of Cu: A micro-to-nano structural, elemental and stable isotopic multi-proxy study

In this study, a multi-proxy approach combining {sup 29}Si, {sup 27}Al and {sup 1}H MAS-NMR, FEG-EPMA, XANES at the Cu K-edge and XRD analytics with hydrochemical tools such as ICP-OES analyses, oxygen-isotope signatures, and thermodynamic modelling was applied to K-silicate-activated metakaolin specimens - with and without CuSO{sub 4}·5H{sub 2}O addition - exposed to sulfuric acid at pH = 2 for 35 days. The results revealed a multistage deterioration mechanism governed by (i) acid diffusion, (ii) leaching of K-A-S-H, (iii) microstructural damage related to precipitation of expansive (K,Ca,Al)-sulfate-hydrate phases (iv) complete dissolution of the K-A-S-H framework, (v) and formation of silica gel in the outermost corroded regions. Copper ions were mainly located in layered spertiniite-chrysocolla-like phases in the as-cured materials. The results demonstrate an overall negative effect of Cu addition on chemical material durability, implying that the reported higher durability of Cu-doped AAM in biocorrosion environments can be best explained by bacteriostatic effects.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Uranium sorption to organic matter and long-term accumulation in a pristine alpine wetland

Understanding the controls on uranium (U) mobility in the environment is key to improve the management of sites contaminated by U mining activities. Previous research has shown that natural or engineered wetlands are particularly able to scavenge high amounts of U(VI) and U(IV) under noncrystalline forms. However, questions remain on the respective roles of sorption and reduction processes in the removal of U from running waters in wetlands, as well as on the long-term stability of U storage. Here, we performed a series of geochemical, isotopic ($δ$ 238 U, ( 234 U/ 238 U)), microscopic (SEM-EDXS, EPMA) and spectroscopic (µ-XRF, µ-XAS, XANES and EXAFS at the U L 3 and M 4 -edges and Fe K-edge) investigations to determine the modes of U accumulation and assess U mobility in a natural exceptionally U-enriched (up to 5000 µg/g) wetland on the shore of Lake Nègre (Mediterranean Alps, France). Uranium (VI) was largely dominant in the two studied soil cores, except a few samples containing as much as ~50 % U(IV). At the particle scale, U is associated to a variety of organic constituents of the soil matrix with a homogenous oxidation state. Bulk EXAFS spectroscopy at the U L 3 -edge shows that U is mostly mononuclear, with dominant monodentate binding to organic moieties (C neighbors at ~3.45 Å). An additional minor fraction of U under polymeric forms is inferred from wavelet (CCWT) analysis of the EXAFS data. These observations are reinforced by 1 M bicarbonate extractions that result in the dissolution of 82–96 % of total U, including putative polymeric species. At the wetland scale, similar or slightly fractionated isotopic ratios ($δ$ 238 U) between the wetland-feeding creek waters and the wetland soils are observed, supporting the idea that U(VI) sorption on organic matter is the primary U scavenging mechanism. Furthermore, it indicates that partial U(VI) reduction to U(IV) occurs as a second step, after sorption. Analysis of U decay chain disequilibria in the cores as a function of depth suggests that U accumulation in this wetland has lasted for several thousand years. In conclusion, we propose that the wetland acts as an active reactor where U has been massively accumulating for ~14500 years, especially as U(VI) forms associated to organic matter and is further partly exported to the lake through soil erosion.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗
DOE OSTI2022

Interaction of beryllium with 316H stainless steel in molten Li 2 BeF 4 (FLiBe)

The increased demand in renewable energy resources has led to a renewed interest in nuclear reactors including a new generation of molten salt reactors. One of the issues encountered in handling of molten chloride or fluoride salts is the inability of metals to form and retain a protective oxide surface layer, generally chromium oxide. The low chromium content, nickel-based alloy INOR-8, later marketed as Hastelloy N, was specifically developed to contain molten fluorides. This alloy had some deficiencies, but its composition resulted in it incurring far less chromium depletion by the molten fluoride salts than alloys like 316 stainless steel. For the next generation of molten salt reactors, an alloy with pressure vessel code approval and higher temperature capability than Hastelloy N is required. Consequently, several reactor designers have reportedly chosen to build the reactor containment vessel from 316H stainless steel. In order to minimize corrosion of the stainless steel by the molten fluoride salt (2LiF-BeF 2 ), it is proposed to add beryllium metal to the salt to react with impurities and provide a means to lower the oxidation potential thus making the salt less corrosive. Even so, there is a concern whether the beryllium would react with components of the stainless steel. To address this concern, static capsule tests were conducted in which selected amounts of beryllium were added to capsules containing 2LiF-BeF 2 (FLiBe) salt and 316H stainless steel and Hastelloy N samples. Following exposure, the samples were cleaned and examined using a variety of analysis techniques including, optical microscopy, SEM-EDS, XPS, LIBS, XRD and EPMA. Tensile samples were also exposed in capsules, and those were subjected to tensile testing. Notably, It was found that for the level of beryllium additions used in this study, intermetallic compounds were formed which could be detrimental to the long-term performance of the 316H stainless steel.

36 MATERIALS SCIENCE↗
DOE OSTI2026

FIB-ToF-SIMS characterization of irradiated U-10Zr

Post-irradiation examination (PIE) is critical for the performance assessment and qualification of nuclear fuels. Secondary ion mass spectrometry (SIMS) is a powerful materials characterization technique that allows for elemental and isotopic mapping with a depth resolution greater than EDS and EPMA. However, it has not yet been applied to PIE of metallic nuclear fuel. Here, in this work, we characterize an fast neutron spectrum irradiated U-10Zr fuel sample using a time-of-flight SIMS (ToF-SIMS) system connected to a FIB/SEM system, which allows for flexible sample analysis compared to a dedicated ToF-SIMS instrument. Analysis of the resulting hyperspectral micrograph data was aided by the development of an unsupervised machine learning (ML) algorithm that iterates on existing methods to segment the 3D micrographic datasets based on the similarity of mass spectra. The results showed that the FIB-ToF-SIMS instrument was potentially capable of spatially resolving closed fission gas bubbles in 3D by continued ion sputtering of the analyzed volume. Additionally, the ML algorithm proved useful in revealing the chemical segregation of light fission products (those with an atomic mass between approximately 85–105 amu, such as ruthenium and rhodium) plus matrix zirconium, heavy fission products (those with an atomic mass between approximately 135–150 amu, such as the lanthanides) and uranium. Future studies are planned to conduct FIB-ToF-SIMS analysis on more irradiated U-Zr samples to study the constituent redistribution.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Microscopic analysis of copper current collectors and mechanisms of fragmentation under compressive forces

Extensive fragmentation of copper current collectors was observed after spherical indentation on prismatic and large-format pouch Li-ion cells by 3D X-ray computed tomography (XCT). Microscopic analysis including scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM) and x-ray photoelectron microscopy (XPS) was carried out on copper current collectors from used commercial cells and pristine anodes. The copper-graphite cross-section images showed rough interface areas affected by reactions and diffusion in the used cell. Electron probe micro-analyzer (EPMA) element mapping showed the interface area was rich in oxygen and phosphorus. A detectable amount of phosphorus was also uniformly distributed inside the current collector. The same oxygen and phosphorus distributions were confirmed by STEM/EDS analysis. XPS depth profiles on multiple elements revealed the interface area of the aged anode was rich in Li, F, P, O and C and diffused at least 50 nm into the copper. In comparison, the pristine anode showed a very smooth C/Cu interface. No other elements were detected. For commercial cells, the reactions in the interface area and diffusion of multiple elements into the lattice and grain boundaries were responsible for the embrittlement of the copper current collectors. Finally, permanent cell capacity loss was observed in electrochemical performance of the indented cells.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Arsenic Accumulation in Microbial Biomass and the Interpretation of Signals of Early Arsenic‐Based Metabolisms

Carbonaceous particles that concentrate arsenic in microbialites as old as ~3.5 Ga are similar to As-rich organic globules in modern microbialites. The former particles have been interpreted as tracers of As cycling by early microbial metabolisms. However, it is unclear if arsenic accumulation is a consequence of biological activity or passive postmortem binding of arsenic by organic matter during diagenesis in volcanically influenced, As-rich environments. Here, we address this uncertainty by evaluating the concentrations, speciation, and detectability of As in active or heat-killed biofilms formed by cyanobacteria or anoxygenic photosynthetic microbes exposed to environmentally relevant concentrations of As(III) or As(V) (50 μM to 3 mM). The genomes or metagenomes of these biofilms contain genes involved in detoxifying or energy-yielding As metabolisms. Biomass accumulates As from the solution in a concentration-dependent manner and with a preference for oxidized As(V) over As(III). Autoclaved biomass accumulates As even more strongly than active biomass, likely because living biofilms actively detoxify As. Active biofilms oxidize and reduce As and accumulate both As(III) and As(V), whereas a small fraction of As(V) can be reduced in inactive biofilms that bind As during diagenesis. Arsenic enrichments in the biomass are detectable by X-ray based spectroscopy techniques (XRF, EPMA-WDS) that are commonly used to analyze geological materials. These findings enable the reconstruction of past active and passive interactions of microbial biomass with arsenic in fossilized microbial biofilms and microbialites from the early Earth.

Madrigal‐Trejo, David↗
DOE OSTI2020

Hydrous olivine alteration on Mars and Earth

In this report hydrous alteration of olivine macrocrysts in a Martian olivine phyric basalt, NWA 10416, and a terrestrial basalt from southern Colorado are examined using SEM, EPMA, TEM, and µXRD techniques. The olivines in the meteorite contain linear nanotubes of hydrous material, amorphous areas, and fluid dissolution textures quite distinct from alteration identified in other Martian meteorites. Instead, they bear resemblance to terrestrial deuteric alteration features. The presence of the hydrous alteration phase Mg‐laihunite within the olivines has been confirmed by µXRD analysis. The cores of the olivines in both Martian and terrestrial samples are overgrown by unaltered rims whose compositions match those of a separate population of groundmass olivines, suggesting that the core olivines are xenocrysts whose alteration preceded crystallization of the groundmass. The terrestrial sample is linked to deep crustal metasomatism and the “ignimbrite flare‐up” of the Oligocene epoch. The comparison of the two samples suggests the existence of an analogous relatively water‐rich magmatic reservoir on Mars.

58 GEOSCIENCES↗
DOE OSTI2021

Seaborgite, LiNa6K2(UO2)(SO4)5(SO3OH)(H2O), the First Uranyl Mineral Containing Lithium

Abstract Seaborgite (IMA2019-087), LiNa6K2(UO2)(SO4)5(SO3OH)(H2O), is a new mineral species from the Blue Lizard mine, Red Canyon, San Juan County, Utah, U.S.A. It is a secondary phase found on gypsum in association with copiapite, ferrinatrite, ivsite, metavoltine, and römerite. Seaborgite occurs in sprays of light-yellow, long flattened prisms or blades, up to about 0.2 mm in length. Crystals are elongated on [100], flattened on {010}, and exhibit the forms {100}, {010}, {001}, and {101}. The mineral is transparent with vitreous luster and very pale-yellow streak. It exhibits bright lime-green fluorescence under a 405 nm laser. The Mohs hardness is ~2½. The mineral has brittle tenacity, curved or conchoidal fracture, and one good cleavage on {100}. The measured density is 2.97(2) g/cm3. The mineral is immediately soluble in H2O at room temperature. The mineral is optically biaxial (–), α = 1.505(2), β = 1.522(2), γ = 1.536(2) (white light); 2Vmeas = 85(1)°; moderate r < ν dispersion; orientation X ^ a ≈ 10°; pleochroic X colorless, Y and Z light green-yellow; X < Y ≈ Z. EPMA and LA-ICP-MS analyses of seaborgite undermeasured its Li, K, and Na. The empirical formula using Li, Na, and K based on the structure refinement is Li1.00Na5.81K2.19(UO2)(SO4)5(SO3OH)(H2O). Seaborgite is triclinic, P1, a = 5.4511(4), b = 14.4870(12), c = 15.8735(15) Å, α = 76.295(5), β = 81.439(6), γ = 85.511(6)°, V = 1203.07(18) Å3, and Z = 2. The structure (R1 = 0.0377 for 1935 I = 2σI) contains [(UO2)2(SO4)8]4– uranyl-sulfate clusters that are linked into a band by bridging LiO4 tetrahedra. The bands are linked through peripheral SO4 tetrahedra forming a thick heteropolyhedral layer. Channels within the layers contain a K site, while an additional K site, six Na sites, and an SO3OH group occupy the space between the heteropolyhedral layers.

Geochemistry & Geophysics↗
DOE OSTI2023

Storage and Diffusion of Carbon and Nitrogen in Crustal Materials

Nitrogen is a primary constituent of Earth’s atmosphere and an essential component of many biological processes. Recent developments in understanding N incorporation into silicate minerals suggest that the solid earth and lithosphere could provide a substantial reservoir for the planetary N budget. Furthermore, determining the concentration and distribution of low abundances of N in silicates presents a significant challenge in microanalysis. We tested capabilities for high spatial resolution quantification of low levels of N using EPMA with the goal of developing standards to be used in coupled N and noble gas analyses of silicate minerals. We investigated the concentration and distribution of N in a suite of ammonium-bearing silicate minerals that reflect the dominant N-bearing phases of the lithosphere: tobelite, buddingtonite, ammonioleucite, tsaregorodtsevite, and hyalophane. These minerals form during NH 4 -rich alteration of K-bearing silicate minerals, and the bonding environment of N in each mineral is likely to differ based on crystal structure. Using an optimized analytical routine for N quantification enables sensitivity approaching 0.02 weight% N and high-resolution quantitative mapping of sub-micron variations in N contents.

58 GEOSCIENCES↗
DOE OSTI2024

Precise Compositional Characterization of Plutonium Alloys by Electron Probe Microanalysis

Key Takeaway Points: • Unlike most other materials, the precise compositional analysis of plutonium, including compounds and alloys, is riddled by numerous difficulties that are unique to the element, including the high atomic number and radioactive nature. There’s work to be done! • Radioactive materials require special handling to ensure precise compositions can be measured by EPMA. • Mean Atomic Number background corrections are limited due to high average atomic number. • Mass Absorption Coefficients are unknown for most light elements. Quantification relies upon calibration curves. • Principal Component Analysis could be a useful tool to improve interpretation of complicated, multiple element X-ray maps.

Maner, IV, James L.↗
DOE OSTI2024

Laser-heated Pedestal Growth and Raman DTS for Harsh-environment Applications

Fibers composed of single crystal (SC) materials are mechanically, thermally, and chemically robust to harsh conditions, and thus attractive for sensing applications in harsh environments. However, SC fibers grown via the laser-heated pedestal growth (LHPG) technique do not intrinsically have a functional cladding layer. We investigate self-segregation of dopants in a crystal matrix within a SC fiber. Ti and Cr dopants within a sapphire matrix were grown via the LHPG method. Cross-sectional dopant concentrations were measured via electron-probe micro-analysis (EPMA). The cross-sectional constituent profiles and resulting transmissivities were characterized as a function of growth parameters.

Lander, Gary↗
DOE OSTI2022

Residual stress and microstructure in IN718-René41 graded superalloy fabricated by laser blown directed energy deposition

Additively printed Ni-based superalloy with a compositionally graded transition from IN718 to René41 was fabricated by laser blown-powder directed energy deposition (DED/LB-M), with the goals of meeting location-specific temperature capability and reducing component cost for hot gas path turbine components. Residual stress distribution in thin wall specimens with three sets of DED build parameters in the as-built and stress-relieved states was measured by neutron diffraction. For calculating residual stress, the calculated d0 method was found to be more appropriate as stress-free reference than using the lattice spacing measured from the stress-relief heat treated specimens. Longer dwell time (lower interpass temperature), higher energy input, smaller layer thickness resulted in a higher magnitude of tensile residual stresses at edges and compressive residual stresses at center of the specimens. The residual stress results did not show a strong dependence on graded compositions, indicating that the residual stress build-up was more geometry and process dependent. Non-destructive neutron imaging based on the attenuation coefficient qualitatively visualized the compositional variation in the bulk and showed good agreement with quantitative Electron Probe Micro-Analysis (EPMA) measurement. Grain structure, texture, and residual plastic strain along the build direction were characterized by Electron Backscatter Diffraction (EBSD). Long columnar grains with (001) preferred grain orientation were dominant along the build direction. Compositional change did not show an obvious effect on the epitaxial growth of dendrites and the continuation of the columnar grains. Residual plastic strain was relatively low in the as-built specimens.

36 MATERIALS SCIENCE↗