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At least 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Solute Redistribution During Aging in a Laser-Based Powder Bed Fusion-Produced Fe-18Ni-9Co-5Mo-Ti Maraging Steel

Solute distribution during the laser-based powder bed fusion of metals process is highly complex because of solidification. This study builds on a previous investigation of how solute heterogeneities across different scales influence phase distribution and aging physical phenomena in a Fe-18Ni-9Co-5Mo-Ti maraging steel (Santana et al. in Addit Manuf 104494, 2024). Previous work using energy-dispersive X-ray spectroscopy revealed heterogeneous Ni and Mo enrichment at intercellular regions. Using X-ray diffraction, 8 ± 3% retained austenite was quantified in as-built samples. Additionally, electron backscatter diffraction analysis exposed the location of retained austenite along cell boundaries. In this work, scanning transmission electron microscopy results revealed the presence of non-enriched retained austenite in the as-built condition. With increased aging temperature, Ni and Mo enrichment in austenite increased, especially at the austenite/martensite boundary. Solute diffusion was simulated in DICTRA Thermo-Calc® software to assess solute redistribution between the matrix and second phases and to comprehend whether elemental diffusion processes are interconnected. Three different scenarios were considered: (1) solute diffusion in the matrix; (2) diffusion with enriched austenite in the intercellular region; (3) diffusion with non-enriched austenite in the intercellular region. Results showed that Ni partitioning controls austenite growth and that boundary regions exhibit higher element enrichment than the core.

42 ENGINEERING↗
DOE OSTI2025

Investigation of UO 2 doped with Fe 2 O 3 sintered under a reducing atmosphere

Nuclear fuel produced with trace amounts of transition metal additives is of potential interest for introducing intentional signatures for accelerating nuclear forensics. In this work, we investigate the effects on microstructure, grain size, crystal structure, and stoichiometry when trace amounts of Fe in the form of Fe 2 O 3 are added to UO 2 . Sintering of compacts with different concentrations, from 250 to 3000 ppmw, was performed under a reducing atmosphere at 1773 K. The persistence of the taggant during the fuel fabrication process as well as its impact on grain size, crystal lattice, and first-neighbor chemistry was evaluated using inductively coupled plasma–optical emission spectroscopy, powder X-ray diffraction (pXRD), Raman spectroscopy, scanning electron microscopy–backscatter electron spectroscopy, energy dispersive spectroscopy, and thermogravimetric analysis. We observed that a negligible amount of Fe was lost during sintering. Our results indicate that the feedstock, Fe 2 O 3 transforms into Fe and FeO under the test sintering conditions. For all compositions, metallic Fe precipitate was found in grain boundaries as a secondary phase. In conclusion, the potential incorporation of ionic Fe into the UO 2 unit cell was determined by pXRD and Raman spectra.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Hydrogen Storage Performance of Preferentially Oriented Mg/rGO Hybrids

Chemical interactions on the surface of a functional nanoparticle are closely related to its crystal facets, which can regulate the corresponding energy storage properties like hydrogen absorption. In this study, we reported a one-step growth of magnesium (Mg) particles with both close- and nonclose-packed facets, that is, {0001} and {$2\overline{116}$} planes, on atomically thin reduced graphene oxide (rGO). The detailed microstructures of Mg/rGO hybrids were revealed by X-ray diffraction, selected-area electron diffraction, high-resolution transmission electron microscopy, and fast Fourier transform analysis. Hydrogen storage performance of Mg/rGO hybrids with different orientations varies: Mg with preferential high-index {$2\overline{116}$} crystal surface shows remarkably increased hydrogen absorption up to 6.2 wt % compared with the system exposing no preferentially oriented crystal surfaces showing inferior performance of 5.1 wt % within the first 2 h. First-principles calculations revealed improved hydrogen sorption properties on the {$2\overline{116}$} surface with a lower hydrogen dissociation energy barrier and higher stability of hydrogen atoms than those on the {0001} basal plane, supporting the hydrogen uptake experiment. In addition, the hydrogen penetration energy barrier is found to be much lower than that of {0001} because of low surface atom packing density, which might be the most critical process to the hydrogenation kinetics. Here, the experimental and calculation results present a new handle for regulating the hydrogen storage of metal hydrides by controlled Mg facets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Interfacial Hydrophilicity Controls Mineral Transformation Outcomes for Enstatite and Amorphous MgSiO 3

Subsurface injection of carbon dioxide (CO 2 ) into mafic-ultramafic rocks for permanent storage via mineralization is being studied to reduce emissions. Here, we investigated the carbonation products of enstatite (MgSiO 3 ) to assess its efficiency in sequestering CO 2 for safe and permanent storage as carbonate minerals. This was accomplished by conducting variable temperature carbonation reactions with samples of differing crystallinities and surface chemistries. Reaction progress was monitored utilizing in situ X-ray diffraction, and the presence of carbonate products was confirmed using additional techniques, such as thermogravimetric analysis coupled with mass spectrometry and scanning electron microscopy with energy dispersive spectrometry. Our results show that crystalline enstatite produces small amounts of the anhydrous form of MgCO 3 (magnesite), while amorphous MgSiO 3 , which was used to simulate mafic glass, more readily converts to the hydrated/hydroxylated hydromagnesite [Mg 5 (CO 3 ) 4 (OH) 2 ·4H 2 O]. These results, supplemented with dynamic vapor sorption experiments, suggest that surface properties play a significant role in the pathway and degree of carbonation. These developments concerning the reactivity of CO 2 with reactive mafic phases will help further our understanding of the reactivity of these mafic-ultramafic minerals with implications for permanent carbon storage and other subsurface engineering scenarios involving reactive reservoirs.

basalt↗
DOE OSTI2022

Transuranium Sulfide via the Boron Chalcogen Mixture Method and Reversible Water Uptake in the NaCu T S 3 Family

The behavior of 5f electrons in soft ligand environments makes actinides, and especially transuranium chalcogenides, an intriguing class of materials for fundamental studies. Due to the affinity of actinides for oxygen, however, it is a challenge to synthesize actinide chalcogenides using non-metallic reagents. Using the Boron Chalcogen Mixture (BCM) method, we achieved the synthesis of the transuranium sulfide NaCuNpS 3 starting from the oxide reagent, NpO 2 . Via the same synthetic route, the isostructural composition of NaCuUS 3 was synthesized and the material contrasted with NaCuNpS 3 . Single crystals of the U-analog, NaCuUS 3 , were found to undergo an unexpected reversible hydration process to form NaCuUS 3 ·xH 2 O (x ≈ 1.5). Here, a large combination of techniques was used to fully characterize the structure, hydration process, and electronic structures, specifically a combination of single crystal, powder, high temperature powder X-ray diffraction, extended X-ray ab-sorption fine structure, infrared, and inductively coupled plasma spectroscopies, thermogravimetric analysis, and density functional theory calculations. The outcome of these analyses enabled us to determine the composition of NaCuUS 3 ·xH 2 O and obtain a structural model that demonstrated the retention of the local structure within the [CuUS 3 ] – layers throughout the hydration-dehydration process. Band structure, density of states, and Bader charge calculations for NaCuUS 3 , NaCu-US 3 ·xH 2 O, and NaCuNpS 3 along with X-ray absorption near edge structure, UV-vis-NIR and work function measurements on ACuUS 3 (A = Na, K, and Rb) and NaCuUS 3 ·xH 2 O samples were carried out to demonstrate that electronic properties arise from the [CuTS 3 ] – layers and show surprisingly little dependence on the interlayer distance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Capacity Fade of Graphite/NMC811: Influence of Particle Morphology, Electrolyte, and Charge Voltage

LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) is an important Li-ion battery cathode material; however, there is a tradeoff between delivered capacity and capacity retention. As the charge potential increases the capacity rises but at the expense of capacity retention. The decrease in capacity retention has been ascribed to several factors including particle cracking, surface reconstruction, transition metal dissolution, and electrolyte reactivity. The present study compares 4.1 and 4.3 V charging limits in commercially relevant graphite/NMC811 pouch cells for single crystal (SC) and polycrystalline (PC) NMC811 with ethylene carbonate (EC)-containing or EC-free electrolytes. The electrochemistry is rationalized through analysis of electrochemical impedance spectroscopy, positive electrode X-ray photoelectron spectroscopy, soft X-ray absorption spectroscopy, X-ray diffraction, and negative electrode mapping by X-ray fluorescence. Graphite/SC-NMC811 cells show high-capacity retention at 4.1 V but exhibit degradation at 4.3 V charging potentials. The EC-free electrolyte cells led to higher capacity fade, especially when charged to 4.3 V. Cathode dissolution and deposition on the negative electrode from PC-NMC811 cells was higher than for samples from SC-NMC811 cells. This study reveals the impact of material type, charge voltage, and electrolyte composition on the reactions at the positive electrode, their influence on the negative electrode, and evolution with cycle number.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Atomistic insight into the ferroelastic post-stishovite transition by high-pressure single-crystal X-ray diffraction

Abstract The post-stishovite transition is a classic pseudo-proper typed ferroelastic transition with a symmetry-breaking spontaneous strain. This transition has been studied using high-pressure spontaneous strains, optic modes, and elastic moduli (Cij) based on the Landau modeling, but its atomistic information and structural distortion remain poorly understood. Here we have conducted synchrotron single-crystal X-ray diffraction measurements on stishovite crystals up to 75.3 GPa in a diamond-anvil cell. Analysis of the data reveals atomic positions, bond lengths, bond angles, and variations of SiO6 octahedra across the transition at high pressure. Our results show that the O coordinates split at ~51.4 GPa, where the apical and equatorial Si-O bond lengths cross over, the SiO6 octahedral distortion vanishes, and the SiO6 octahedra start to rotate about the c axis. Moreover, distortion mode analysis shows that an in-plane stretching distortion (GM1+ mode) occurs in the stishovite structure at high pressure while a rotational distortion (GM2+ mode) becomes dominant in the post-stishovite structure. These results are used to correlate with elastic moduli and Landau parameters (symmetry-breaking strain e1–e2 and order parameter Q) to provide atomistic insight into the ferroelastic transition. When the bond lengths of two Si-O bonds are equal due to the contribution from the GM1+ stretching mode, C11 converges with C12, and the shear wave VS1[110] polarizing along [110] and propagating along [110] vanishes. Values of e1–e2 and Q are proportional to the SiO6 rotation angle from the occurrence of the GM1+ rotational mode in the post-stishovite structure. Our results on the pseudo-proper type transition are also compared with that for the proper type in albite and improper type in CaSiO3 perovskite. The symmetry-breaking strain, in all these types of transitions, arises as the primary effect from the structural angle (such as SiO6 rotation or lattice constant angle) and its relevant distortion mode in the low-symmetry ferroelastic phase.

Geochemistry & Geophysics↗
DOE OSTI2021

Understanding nanoscale structural distortions in Pb(Zr 0.2 Ti 0.8 )O 3 by utilizing X-ray nanodiffraction and clustering algorithm analysis

Hard X-ray nanodiffraction provides a unique nondestructive technique to quantify local strain and structural inhomogeneities at nanometer length scales. However, sample mosaicity and phase separation can result in a complex diffraction pattern that can make it challenging to quantify nanoscale structural distortions. In this work, a k-means clustering algorithm was utilized to identify local maxima of intensity by partitioning diffraction data in a three-dimensional feature space of detector coordinates and intensity. This technique has been applied to X-ray nanodiffraction measurements of a patterned ferroelectric PbZr 0.2 Ti 0.8 O 3 sample. The analysis reveals the presence of two phases in the sample with different lattice parameters. A highly heterogeneous distribution of lattice parameters with a variation of 0.02 Å was also observed within one ferroelectric domain. This approach provides a nanoscale survey of subtle structural distortions as well as phase separation in ferroelectric domains in a patterned sample.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2020

Femtosecond laser produced periodic plasma in a colloidal crystal probed by XFEL radiation

With the rapid development of short-pulse intense laser sources, studies of matter under extreme irradiation conditions enter further unexplored regimes. In addition, an application of X-ray Free-Electron Lasers (XFELs) delivering intense femtosecond X-ray pulses, allows to investigate sample evolution in IR pump - X-ray probe experiments with an unprecedented time resolution. Here we present a detailed study of the periodic plasma created from the colloidal crystal. Both experimental data and theory modeling show that the periodicity in the sample survives to a large extent the extreme excitation and shock wave propagation inside the colloidal crystal. This feature enables probing the excited crystal, using the powerful Bragg peak analysis, in contrast to the conventional studies of dense plasma created from bulk samples for which probing with Bragg diffraction technique is not possible. X-ray diffraction measurements of excited colloidal crystals may then lead towards a better understanding of matter phase transitions under extreme irradiation conditions.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Analysis of Deformation and Fracture Mechanisms in the Harvested High-Dose Baffle-Former Bolt with Stress-Corrosion Cracks Formed While in Service

This report presents the results of advanced mechanical testing conducted on miniature tensile specimens excised from an irradiated baffle-former bolt, a commercial pressurized water reactor component. The specimens were extracted from the midsection of the bolt shank, where the estimated damage dose reached 23 displacements per atom. The mechanical testing included the following tests: (1) conventional tensile testing at room temperature, augmented by digital image correlation (DIC) to enable noncontact strain measurements, and (2) in situ tensile testing within a scanning electron microscopy (SEM) instrument equipped with energy-dispersive x-ray spectroscopy (EDS) and electron backscatter diffraction (EBSD) detectors to evaluate active deformation and fracture mechanisms. Additionally, SEM fractographic analysis revealed alterations in the fracture mechanism from a predominantly ductile fracture in nonirradiated steel to a mixed fracture mode (still dominating ductile and minor cleavage spots) in irradiated specimens derived from the baffle bolts. The findings indicate a complex strain localization behavior for in-service irradiated steel specimens. Beyond conventional necking at the macro scale and defect-free channel formation at the micro scale, DIC results identified the presence of deformation bands approximately 100 μm in width. These bands consist of chains of grains exhibiting elevated local strain levels and may be considered an intermediate or mesoscale level of strain localization. These bands become discernible near the yield stress as localized hot spots, areas of elevated strain, persisting throughout most of the experiment. The formation of mesoscale deformation bands as a strain localization mechanism may exacerbate the defect-free channel formation in irradiated materials, further promoting irradiation-assisted stress corrosion crack initiation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2024

Synthesis and structural characterization of 2,2’-bipyridine zinc formate: Analysis of formate bonding and hydrosilylation of CO 2 and carbonyl compounds

The zinc formate compound (bipy)Zn(O 2 CH) 2 is obtained via the reaction of Zn(O 2 CH) 2 with 2,2’-bipyridine (bipy). In addition, (bipy)Zn(O 2 CH) 2 may be formed from zinc hydride via addition of bipy followed by addition of (i) HCO 2 H and (ii) CO 2 . The molecular structure of (bipy)Zn(O 2 CH) 2 has been determined by X-ray diffraction, thereby demonstrating that it exists as a monomeric species with a distorted tetrahedral zinc center and monodentate formate ligands. Analysis of the bonding within the formate ligand indicates that the zinc–formate moiety is not best represented by a Zn–O–C(=O)H resonance structure, but instead possesses a significant ionic component that reduces the C=O bond order and increases the C–O bond order. The formate compound (bipy)Zn(O 2 CH) 2 participates in hydrosilylation transformations involving CO 2 and carbonyl compounds.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Systematic investigations on iron cycling in phosphorus/siderophore systems: Synergism or antagonism?

Synergisms between microbial exudates on Fe (hydr)oxide dissolution as an effective Fe acquisition pathway have been recently addressed and vigorously debated. However, Fe liberation mechanisms and where siderophores and phosphorus (P) coexist received little attentions. Current study systematically investigated ferrihydrite dissolution in the presence of desferrioxamine B (DFOB) (a kind of fungally-derived siderophores) and inorganic/organic phosphorus (orthophosphate, Pi; myo-inositol hexaphosphate, IHP), as a function of solute pH, reaction time and reagent content. Reacted solids were characterized by N 2 -BET adsorption, zeta (ζ) potential analysis, sequential extraction analysis (SEDEX), field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), micro Raman spectroscopy and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). Our results indicate that upon reaction with P-only or (DFOB + P) systems, interfacial complexation partially switched from monolayer bidentate-binuclear surface complexes to ternary complexes, or laterally transformed into amorphous Fe–P precipitates. The Fe-Pi complex precipitated more readily under acidic conditions, and Fe-IHP complex preferentially nucleated in neutral-alkaline environments. Phosphorus slightly promoted Fe release from minerals and fixation to the leached layer or interfacial liquid zone initially, but subsequently prevented further attacks from protons and DFOB. The co-effects of P and DFOB likely correspond to two successive scenarios: 1) DFOB is preferentially attracted toward ferrihydrite surfaces by negative electrical fields induced by adsorbed phosphorus and can act synergistically with labile P–Fe complexes, resulting in intensive temporal dissolution of Fh; 2) subsequent Fe shuttling to DFOB can be prohibited by stabilized, passive P/Fe–P layers. Finally, our results emphasize the antagonism between P compounds and siderophores (i.e., DFOB here) on ferrihydrite dissolution to improve understanding of the biologically-mediated Fe cycling in natural systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Multimodal study of the impact of stimulation pH on shale pore structure, with an emphasis on organics behavior in alkaline environments

The tight nature of shale formations calls for hydraulic fracturing techniques able of altering the pore architecture to facilitate the production of hydrocarbon resources. The composition, pH, salinity, density and chemistry of Hydraulic Fracturing Fluids (HFF) vary substantially depending on reservoir characteristics. pH is among the most important stimulation fluid properties, ranging from very acidic, for carbonate reservoirs, to basic, in the case of clay-rich formations. pH regulates what geochemical reactions take place between the stimulation fluid and shale, as well as pore architecture alteration. The dissolution of carbonates and pyrite, and the precipitation of common minerals such as barite, gypsum and iron oxides in acidic environments have been extensively documented. In contrast, alkali stimulation environments and the role of organic components have received less attention. This research provides insight into the role of both minerals and organic components during alkaline stimulation, and the resulting pore architecture alterations. Here, a set of reactive experiments are performed using three different shales, with varying organic matter (OM) content, at different pH (3, 6, 8, 10, 12). The analysis of pore architecture alteration induced by the reaction was performed via nitrogen (N2) gas adsorption and Time-Domain Nuclear Magnetic Resonance (TD-NMR). Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES) was used to measure the composition of the stimulation fluid post-reaction. The system with a larger impact on the pore architecture (pH 12) underwent a more extensive analysis through the application of Focused Ion Beam Scanning Electron Microscopy (FIB-SEM) and x-ray Diffraction (XRD). Results show that mineral dissolution contributed to the creation of secondary porosity, mainly through dissolution of clays and silicates. We show that the abundance and distribution of organic matter both play a significant role in changes in pore architecture. Most samples showed an increase in inter-organic porosity, likely due to the organic acids within kerogen reacting with the stimulation fluid. Samples with a larger amount and more widespread distribution of organic matter show the most significant alterations. Finally, we also highlight the dissolution process of iron-rich minerals, including framboidal pyrite, as another important source of secondary porosity.

04 OIL SHALES AND TAR SANDS↗
DOE OSTI2022

Isolating intermediate Mg 11 Cu 6 Al 12 phase in ternary Mg-Cu-Al alloy by electrolytic dealloying

While dealloying is widely used to create nanoporous materials, it has rarely been employed to isolate difficult-to-synthesize intermediate phases. Here, in this work, we show how air-free, electrolytic dealloying at room temperature can be used to isolate the ternary intermetallic Mg 11 Cu 6 Al 12 phase. We create a ternary Mg-Cu-Al parent alloy containing the Mg 11 Cu 6 Al 12 compound and other phases, then subsequently remove these other phases via electrolytic dealloying to isolate the Mg 11 Cu 6 Al 12 phase. Isolated Mg 11 Cu 6 Al 12 phase exhibits ≈1 μm diameter rod-shaped microstructure. Phase and chemical analysis conducted using various techniques, including inductively coupled plasma and lab and synchrotron-based X-ray diffraction, show minimal impurities. This new approach to isolate the Mg 11 Cu 6 Al 12 phase can unlock its use in fundamental research and can be applied to other difficult-to-synthesize intermetallic compounds.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Iodine capture with mechanically robust heat-treated Ag-Al-Si-O xerogel sorbents

Silver-loaded heat-treated aluminosilicate xerogels (Ag-HTX) were evaluated as sorbents for iodine [I2(g)] capture. The heat treatment step was performed to help increase the mechanical integrity of the gels. The synthesized xerogels were characterized using powder X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy, Brunauer-Emmett-Teller analysis, gravimetric iodine loading, nanoindentation, and dynamic mechanical analysis. The structural and chemical analyses of Ag-HTX showed uniform distribution of Ag throughout the gel network after Ag-exchange. After I2(g) capture, the AgI crystallites were observed in the sorbent verifying chemisorption as the iodine capture mechanism. Iodine loading of this xerogel was 0.43 g g-1 at 150°C over 1 d and 0.52 g g-1 at 22°C over 33 d. The specific surface area of Ag-HTX was 202 m2 g-1 and decreased to 87 m2 g-1 after iodine loading. The hardness of the heat-treated xerogel was 160 times higher than heat-treated aerogel of the same composition. The heat-treatment process increased the modulus value to 40.77 MPa from 6.99 MPa of as-made xerogel, demonstrating the need for this added step in the synthesis process. These results show that Ag-HTX is a promising sorbent for I2(g) capture with good loading capacity and mechanical stability.

xerogels, aerogels, iodine capture, hardness testi↗
DOE OSTI2022

Boron nitride on SiC(0001)

Here, in the field of van der Waals heterostructures, the twist angle between stacked two-dimensional layers has been identified to be of utmost importance for the properties of the heterostructures. In this context, we previously reported the growth of a single layer of unconventionally oriented epitaxial graphene that forms in a surfactant atmosphere [F. C. Bocquet et al., Phys. Rev. Lett. 125, 106102 (2020)]. The resulting G-R0° layer is aligned with the SiC lattice, and hence represents an important milestone towards high-quality twisted bilayer graphene, a frequently investigated model system in this field. Here, we focus on the surface structures obtained in the same surfactant atmosphere, but at lower preparation temperatures at which a boron nitride template layer forms on SiC(0001). In a comprehensive study based on complementary experimental and theoretical techniques, we find—in contrast to the literature—that this template layer is a hexagonal B x N y layer, but not high-quality hBN. It is aligned with the SiC lattice and gradually replaced by low-quality graphene in the 0° orientation of the B x N y template layer upon annealing.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Mudstone Baffles and Barriers in Lower Cretaceous Strata at a Proposed CO 2 Storage Hub in Kemper County, Mississippi, United States

The Cretaceous and Tertiary deposits in Mississippi, Alabama, and the adjacent continental shelf constitute a widespread succession of sandstone, mudstone, and carbonate that has proven to be an important target for geologic CO 2 storage in the onshore Gulf of Mexico basin. Integrated analysis of stratigraphy, sedimentology, and reservoir properties based on cores and geophysical well logs indicates that the Paluxy Formation and Washita- Fredericksburg interval present gigatonne-class storage opportunities. The distribution, geometry, and composition of the area is a direct reflection of the original depositional environments, and understanding these factors is essential for understanding the geologic storage potential of the Paluxy Formation and Washita-Fredericksburg interval at the Kemper County energy facility in Mississippi. Geologic characterization of the Mississippi Embayment at the energy facility focused primarily on characterizing the confinement potential of the storage complex. Integration of core analyses and geophysical well logs has yielded a high-resolution stratigraphic analysis of storage reservoirs, baffles, barriers, and seals. Scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDS), and quantitative X-ray diffraction (XRD) was used to characterize microfabric, pore types, and mineralogy within mudstone of the east-central Mississippi Embayment at the Kemper County energy facility. Mudstone beds in the Paluxy Formation and Washita-Fredericksburg interval have variable thickness and continuity. High water saturation in the Cretaceous mudstone units influences swelling smectite clay and mudrock permeability based on pulse decay analysis is 1–96 nD. These low permeability values indicate that the mudstone units are effective baffles, barriers, and confining intervals that make significant migration of injected CO 2 out of the storage complex unlikely. The numerous baffles and barriers within the target reservoir intervals, moreover, favor the retention of multiple CO 2 in plumes within the abundant stacked sandstone bodies.

03 NATURAL GAS↗
DOE OSTI2020

A method for mapping submicron-scale crystallographic order/disorder applied to human tooth enamel

Tooth enamel, the outermost layer of human teeth, is a complex, hierarchically structured biocomposite. The details of this structure are important in multiple human health contexts, from understanding the progression of dental caries (tooth decay) to understanding the process of amelogenesis and related developmental defects. Enamel is composed primarily of long, nanoscale crystallites of hydroxyapatite that are bundled by the thousands to form micron-scale rods. Studies with transmission electron microscopy show the relationships between small groups of crystallites and X-ray diffraction characterize averages over many rods, but the direct measurement of variations in local crystallographic structure across and between enamel rods has been missing. Here, we describe a synchrotron X-ray-based experimental approach and a novel analysis method developed to address this gap in knowledge. A ~500-nm-wide beam of monochromatic X-rays in conjunction with a sample section only 1 μm in thickness enables 2D diffraction patterns to be collected from small well-separated volumes within the enamel microstructure but still probes enough crystallites (~300 per pattern) to extract population-level statistics on crystallographic features like lattice parameter, crystallite size, and orientation distributions. Furthermore, the development of a quantitative metric to characterize relative order and disorder based on the azimuthal autocorrelation of diffracted intensity enables these crystallographic measurements to be correlated with their location within the enamel microstructure (e.g., between rod and interrod regions). These methods represent a step forward in the characterization of human enamel and will elucidate the variation of the crystallographic structure across and between enamel rods for the first time.

crystallographic order/disorder↗