Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “SEM”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 253 records · Page 14
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Quantifying dry supercritical CO 2 -induced changes of the Utica Shale

Traditionally, shale formations have been studied as sealing layers that prevent vertical migration of hydrocarbons and CO2 due to their low permeability and fracture porosity. Recent research has focused on storing CO2 in hydrocarbon-bearing shale formations that have already undergone depletion through primary production and using CO2 as a potential fracturing agent for unconventional reservoirs. The injected CO2 will interact with shale components (i.e. clays, organic matter) and affect rock properties through chemical alteration, matrix swelling/shrinkage, and related geomechanical effects. As changes in rock properties will impact both anthropogenic CO2 storage and hydraulic fracturing, it is imperative to increase our understanding of the CO2-shale interactions. In-situ Fourier Transform infrared (FT-IR) spectroscopy coupled with high temperature and pressure capability was used to examine the interaction of dry CO2 on Utica Shale, clay, and kerogen samples at the molecular scale and characterize vibrational changes of sorption bands sensitive to the gas-solid environment. The Utica Shale was also analyzed for micro and macro-scale chemical and physical changes before and after exposure to dry CO2 at subsurface storage conditions using surface relocation techniques via high-resolution field-emission scanning electron microscopy (FE-SEM). Brunauer-Emmett-Teller (BET) surface area/pore size analysis and quantitative adsorption isotherms were applied to understand changes in surface area, pore volumes, and understand the storage potential of CO2 in the Utica Shale sample. FT-IR and feature relocation via FE-SEM indicate carbonate formation and dissolution occurs in shale exposed to dry CO2. Results indicate that etching and pitting occur, with minor calcite precipitation along the surface of the shale sample. Quantitative isotherm results indicate that shales with a higher content of kerogen and illite-smectite clays would be expected to have the highest CO2 storage capacity provided these constituents were accessible for interaction.

04 OIL SHALES AND TAR SANDS↗
DOE OSTI2017

Ambient aging of rhenium filaments used in thermal ionization mass spectrometry: Growth of oxo-rhenium crystallites and anti-aging strategies

Degassing is a common preparation technique for rhenium filaments used for thermal ionization mass spectrometric analysis of actinides, including plutonium. Although optimization studies regarding degassing conditions have been reported, little work has been done to characterize filament aging after degassing. In this study, the effects of filament aging after degassing were explored to determine a “shelf-life” for degassed rhenium filaments, and methods to limit filament aging were investigated. Zone-refined rhenium filaments were degassed by resistance heating under high vacuum before exposure to ambient atmosphere for up to 2 months. After degassing the nucleation and preferential growth of oxo-rhenium crystallites on the surface of polycrystalline rhenium filaments was observed by atomic force microscopy and scanning electron microscopy (SEM). Compositional analysis of the crystallites was conducted using SEM-Raman spectroscopy and SEM energy dispersive X-ray spectroscopy, and grain orientation at the metal surface was investigated by electron back-scatter diffraction mapping. Spectra collected by SEM-Raman suggest crystallites are composed primarily of perrhenic acid. The relative extent of growth and crystallite morphology were found to be grain dependent and affected by the dissolution of carbon into filaments during annealing (often referred to as carbonization or carburization). Crystallites were observed to nucleate in region specific modes and grow over time through transfer of material from the surface. Factors most likely to affect the rates of crystallite growth include rhenium substrate properties such as grain size, orientation, levels of dissolved carbon, and relative abundance of defect sites; as well as environmental factors such as length of exposure to oxygen and relative humidity. Thin (~180 nm) hydrophobic films of poly(vinylbenzyl chloride) were found to slow the growth of oxo-rhenium crystallites on the filament surfaces and may serve as an alternative carbon source for filament carburization.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Transmission Kikuchi diffraction and transmission electron forescatter imaging of electropolished and FIB manufactured TEM specimens

We present a study of the efficiency of the utility of scanning electron microscope (SEM)-based transmission methods for characterizing grain structure in thinned bulk metals. Foils of type 316 stainless steel were prepared by two methods commonly used for transmission electron microscopy — double-jet electropolishing and focused ion beam milling. A customized holder allowed positioning of the foils in a configuration appropriate for both transmission electron forward scatter diffraction, and for transmission imaging by the use of a forescatter detector with two diodes. We found that both crystallographic orientation maps and dark-field transmitted images could be obtained for specimens prepared by either method. However, for both methods, preparation-induced artifacts may affect the quality or accuracy of transmission SEM data, especially those acquired by the use of transmission Kikuchi diffraction. Generally, the quality of orientation data was better for specimens prepared by electropolishing, due to the absence of ion-induced damage. - Highlights: • The transmission imaging and diffraction techniques are emerging in scanning electron microscopy (SEM) as promising new field of materials characterization. • The manuscript titled: “Transmission Kikuchi Diffraction and Transmission Electron Forescatter Imaging of Electropolished and FIB Manufactured TEM Specimens” documents how different specimen thinning procedures can effect efficiency of transmission Kikuchi diffraction and transmission electron forescatter imaging. • The abilities to make precision crystallographic orientation maps and dark-field images in transmission was studied on electropolished versus focus ion beam manufactured TEM specimens. • Depending on the need, electropolished and focused ion beam technique may produce suitable specimens for transmission imaging and diffraction in SEM.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A study on the creep behavior of alloy 709 using in-situ scanning electron microscopy

In this research, an experimental evaluation of creep properties of Alloy 709 in the temperature range of 750–850 °C was undertaken. Alloy 709 is a novel austenitic stainless steel with 20% Cr and 25% Ni by wt% that was developed for application in structural components of nuclear power plants. Creep rupture tests were conducted in an in-situ heating-loading and Scanning Electron Microscope (SEM) unit equipped with Electron Backscatter Diffraction (EBSD) detector and Energy Dispersive Spectroscopy (EDS). “Real-time” creep damage mechanisms of Alloy 709 at various stresses and temperatures using a flat, un-notched sample with continuously reducing cross-section is studied so that the failure and maximum creep damage occurred at the center of the sample where the in-situ SEM imaging could be focused. Accelerated creep tests at temperatures and stresses above service conditions were performed by employing multiple blocks of constant loads where the loads were increased once the sample attained constant creep rate, indicating a secondary creep regime. This technique ensures multiple data points can be obtained from the same test, saves the time required for an otherwise long-term creep test and usage of SEM. Further, Coincident Site Lattice (CSL) boundary maps were collected as control maps before testing, and the grain boundaries were observed during the creep test to understand the effect of grain boundary character on the creep damage mechanism. Void growth, grain boundary separation, and sliding were found to be the main creep mechanisms whose rate is dependent on stress and temperature. Failure mechanisms studied on the fracture surface using SEM fractography were correlated to the sample surface observations to create complementary information to better understand the underline creep mechanism of Alloy 709.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Precession electron diffraction for SiC grain boundary characterization in unirradiated TRISO fuel

Precession electron diffraction (PED), a transmission electron microscopy-based technique, has been evaluated for the suitability for evaluating grain boundary character in the SiC layer of tristructural isotropic (TRISO) fuel. Although the ultimate goal is to determine the grain boundary characteristics of fission product containing grain boundaries of neutron irradiated SiC, our work reports the effect of transmission electron microscope (TEM) lamella thickness on quality of data and establishes a baseline comparison on grain boundary characteristics determined previously using a conventional EBSD scanning electron microscope (SEM) based technique. In general, it was determined that the lamella thickness produced using the standard FIB fabrication process, is sufficient to provide reliable PED measurements with thicker lamellae (~120 nm) produce higher quality orientation data. Analysis of grain boundary character from the TEM-based PED data showed a much lower fraction of low angle grain boundaries compared to SEM-based EBSD data from the SiC layer of the same TRISO-coated particle as well as a SiC layer deposited at a slightly lower temperature. The fractions of high angle and CSL-related grain boundaries determined by PED are similar to those found using SEM-based EBSD. Since the grain size of the SiC layer of TRSIO fuel can be as small as 250 nm [12], depending on the fabrication parameters, and grain boundary fission product precipitates can be nano-sized, the TEM-based PED orientation data collection method is preferred to determine an accurate representation of the relative fractions of low angle, high angle and CSL-related grain boundaries. It was concluded that although the resolution of the PED data is better by more than an order of magnitude, data acquisition times may be significantly longer or the number of areas analyzed significantly larger than the SEM-based method to obtain a statistically relevant distribution. Also, grain size could be accurately determined but significantly larger analysis areas than those used in this study would be required.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Analysis of fission product distribution and composition in the TRISO layers of AGR-2 fuel

The Advanced Gas Reactor Fuel Qualification and Development Program's second irradiation experiment focuses on the performance of fuel particles produced in an industrial-scale coating system. Ongoing post-irradiation examination efforts include exploration of tristructural-isotropic (TRISO)-coated particle fuel in the as-irradiated state and subjected to elevated temperatures to simulate accident conditions (safety testing). Scanning electron microscopy (SEM) analysis with energy dispersive x-ray spectroscopy (EDS) was used to show the distribution of fission products within the TRISO layers. The SEM analysis showed a variation of fission product distribution within the TRISO layers based on irradiation temperature, burnup, individual particle fission product inventory retention, safety testing history and kernel composition. Finally, a key observation is that particles which likely experienced higher temperature showed a greater diversity and distribution of fission products and actinides in the IPyC and SiC layers, implying that temperature is a dominant variable influencing the transport of radionuclides in TRISO particles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Electron microscopy techniques employed to explore mitochondrial defects in the developing rat brain following ketamine treatment

Ketamine, an FDA-approved N-methyl-D-aspartate (NMDA) receptor antagonist, is commonly used for general pediatric anesthesia. Accumulating evidence has indicated that prolonged exposure to ketamine induces widespread apoptotic cell death in the developing brains of experimental animals. Although mitochondria are known to play a pivotal role in cell death, little is known about the alterations in mitochondrial ultrastructure that occur during ketamine-induced neurotoxicity. The objective of this pilot study was to utilize classic and contemporary methods in electron microscopy to study the impact of ketamine on the structure of mitochondria in the developing rat brain. While transmission electron microscopy (TEM) was employed to comprehensively study mitochondrial inner membrane topology, serial block-face scanning electron microscopy (SBF-SEM) was used as a complementary technique to compare the overall mitochondrial morphology from a representative treated and untreated neuron. In this study, postnatal day 7 (PND-7) Sprague-Dawley rats were treated with ketamine or saline (6 subcutaneous injections × 20 mg/kg or 10 ml/kg, respectively, at 2-h intervals with a 6-h withdrawal period after the last injection, n=6 each group). Samples from the frontal cortex were harvested and analyzed using TEM or SBF-SEM. While classic TEM revealed that repeated ketamine exposure induces significant mitochondrial swelling in neurons, the newer technique of SBF-SEM confirmed the mitochondrial swelling in three dimensions (3D) and showed that ketamine exposure may also induce mitochondrial fission, which was not observable in the two dimensions (2D) of TEM. Furthermore, 3D statistical analysis of these reconstructed mitochondria appeared to show that ketamine-treated mitochondria had significantly larger volumes per unit surface area than mitochondria from the untreated neuron. The ultrastructural mitochondrial alterations demonstrated here by TEM and SBF-SEM support ketamine’s proposed mechanism of neurotoxicity in the developing rat brain.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2022

Confined Growth of DNA-Assembled Superlattice Films

Here, we study the assembly of DNA-functionalized nanocubes under lateral confinement in microscale square trenches on a DNA-functionalized substrate. Microfocus small-angle X-ray scattering (SAXS) and scanning electron microscopy (SEM) are used to characterize the superlattices (SLs). The results indicate that nanocubes form simple-cubic SLs with square-prism morphology and a (100) out-of-plane orientation to maximize DNA bonding. In-plane, SLs align with the template, exposing their {100} side facets, and the degree of alignment depends on trench size. Interestingly, the distribution of in-plane orientations determined from SAXS and SEM do not agree, indicating that the internal and external structures of the SLs differ. To understand this discrepancy, X-ray ptychography is employed to image the internal structures of the SLs, revealing that SLs which appear to be single-crystalline in SEM may have subsurface grain boundaries, depending on trench size. SEM reveals that the SLs grow via nucleation and growth of randomly oriented domains, which then coalesce; this mechanism explains the observed dependence of alignment and defect structure on size. Interestingly, crystallization occurs via an unusual growth mode, whereby continuous SL layers grow on top of several misoriented islands. Overall, this work elucidates the effect of lateral confinement on the crystallization of DNA-functionalized nanoparticles and shows how X-ray ptychography can be used to gain insight into nanoparticle crystallization.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Dielectric property of NiTiO{sub 3} doped substituted ortho-chloropolyaniline composites

Ortho-chloropolyaniline (OCP)-NiTiO{sub 3} composites have been synthesized via in-situ polymerization of ortho-chloroaniline with various weight percentages of NiTiO{sub 3.} Fourier Transform Infrared spectroscopic studies of Ortho-chloropolyaniline and its composites indicated the formation of composites as a result of Vander Waal's interaction between OCP and NiTiO{sub 3} particles. Surface morphology of OCP and OCP-NiTiO{sub 3} composites were studied using Scanning Electron Microscope (SEM). The SEM micrographs indicated a modified morphology after the composite formation. Dielectric properties and electric modulus of OCP and OCP-NiTiO{sub 3} composites have been investigated in the frequency range of 50 Hz – 5 MHz. It has been noticed that electrical resistance decreases with increase in weight percentage of NiTiO{sub 3} particles in polymer matrix as well as with applied frequency. The display of semicircular arcs in Cole-Cole plots indicates the formation of series resistor and capacitor in network causing a decrease in the relaxation time and as a result conductivity enhances in these composites. The facile and cost effective synthesis process and excellent dielectric and conductivity response of these materials makes them promising materials for practical applications.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Growth of graphene underlayers by chemical vapor deposition

We present a simple and very convincing approach to visualizing that subsequent layers of graphene grow between the existing monolayer graphene and the copper catalyst in chemical vapor deposition (CVD). Graphene samples were grown by CVD and then transferred onto glass substrates by the bubbling method in two ways, either direct-transfer (DT) to yield poly (methyl methacrylate) (PMMA)/graphene/glass or (2) inverted transfer (IT) to yield graphene/PMMA/glass. Field emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM) were used to reveal surface features for both the DT and IT samples. The results from FE-SEM and AFM topographic analyses of the surfaces revealed the underlayer growth of subsequent layers. The subsequent layers in the IT samples are visualized as 3D structures, where the smaller graphene layers lie above the larger layers stacked in a concentric manner. The results support the formation of the so-called “inverted wedding cake” stacking in multilayer graphene growth.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effects of rapid thermal annealing on the structural and local atomic properties of ZnO: Ge nanocomposite thin films

We have investigated the structural and local atomic properties of Ge nanocrystals (Ge-ncs) embedded ZnO (ZnO: Ge) thin films. The films were deposited by sequential sputtering of ZnO and Ge thin film layers on z-cut quartz substrates followed by an ex-situ rapid thermal annealing (RTA) at 600 °C for 30, 60, and 90 s under forming gas atmosphere. Effects of RTA time on the evolution of Ge-ncs were investigated by x-ray diffraction (XRD), scanning electron microscopy (SEM), hard x-ray photoelectron spectroscopy (HAXPES), and extended x-ray absorption fine structure (EXAFS). XRD patterns have clearly shown that fcc diamond phase Ge-ncs of sizes ranging between 18 and 27 nm are formed upon RTA and no Ge-oxide peak has been detected. However, cross-section SEM images have clearly revealed that after RTA process, Ge layers form varying size nanoclusters composed of Ge-ncs regions. EXAFS performed at the Ge K-edge to probe the local atomic structure of the Ge-ncs has revealed that as prepared ZnO:Ge possesses Ge-oxide but subsequent RTA leads to crystalline Ge structure without the oxide layer. In order to study the occupied electronic structure, HAXPES has been utilized. The peak separation between the Zn 2p and Ge 3d shows no significant change due to RTA. This implies little change in the valence band offset due to RTA.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Novel comparison of microscopy and diffraction techniques on the structure of iron oxide nanoparticle monolayers transferred by Langmuir-Schaefer method

Iron oxide nanoparticles undergo self-assembly into well-ordered monolayer films of macroscopic size at the air-water interface. This self-assembly process is the result of the van der Waals forces between the constituent particles. For roughly spherical particles, this monolayer is a 2D hexagonal close packed lattice. With Grazing Incidence X-Ray Diffraction (GID), one can obtain global statistical information about the film’s spacing and correlation length. Herein, we demonstrate that comparable structural information can be obtained by a novel Fourier transform analysis method applied to Scanning Electron Microscopy (SEM) images taken of the film after it has been transferred to a silicon substrate. This consists of using numerical methods to isolate the lattice structure of the monolayer in the SEM image to which a 2D discrete Fourier Transform is applied and the result integrated. This results in Bragg peak information akin to that obtained from GID, whose structure shows the same hexagonal close packed lattice with similar spacing and of greater peak contrast. Furthermore, this analysis technique may prove to be a suitable alternative or compliment to GID for many applications.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Environmentally induced chemical and morphological heterogeneity of zinc oxide thin films

Zinc oxide (ZnO) thin films have been reported to suffer from degradation in electrical properties, when exposed to elevated heat and humidity, often leading to failures of electronic devices containing ZnO films. This degradation appears to be linked to water and oxygen penetration into the ZnO film. However, a direct observation in the ZnO film morphological evolution detailing structural and chemical changes has been lacking. Here, we systematically investigated the chemical and morphological heterogeneities of ZnO thin films caused by elevated heat and humidity, simulating an environmental aging. X-ray fluorescence microscopy, X-ray absorption spectroscopy, grazing incidence small angle and wide angle X-ray scattering, scanning electron microscopy (SEM), ultra-high-resolution SEM, and optical microscopy were carried out to examine ZnO and Al-doped ZnO thin films on two different substrates—silicon wafers and flexible polyethylene terephthalate (PET) films. In the un-doped ZnO thin film, the simulated environmental aging is resulting in pin-holes. In the Al-doped ZnO thin films, significant morphological changes occurred after the treatment, with an appearance of platelet-shaped structures that are 100–200 nm wide by 1μm long. Synchrotron x-ray characterization further confirmed the heterogeneity in the aged Al-doped ZnO, showing the formation of anisotropic structures and disordering. X-ray diffraction and X-ray absorption spectroscopy indicated the formation of a zinc hydroxide in the aged Al-doped films. In conclusion, utilizing advanced characterization methods, our studies provided information with an unprecedented level of details and revealed the chemical and morphologically heterogeneous nature of the degradation in ZnO thin films.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Three-Dimensional Ultrastructure of Arabidopsis Cotyledons Infected with Colletotrichum higginsianum

We used serial block-face scanning electron microscopy (SBF-SEM) to study the host–pathogen interface between Arabidopsis cotyledons and the hemibiotrophic fungus Colletotrichum higginsianum. By combining high-pressure freezing and freeze-substitution with SBF-SEM, followed by segmentation and reconstruction of the imaging volume using the freely accessible software IMOD, we created 3D models of the series of cytological events that occur during the Colletotrichum–Arabidopsis susceptible interaction. We found that the host cell membranes underwent massive expansion to accommodate the rapidly growing intracellular hypha. As the fungal infection proceeded from the biotrophic to the necrotrophic stage, the host cell membranes went through increasing levels of disintegration culminating in host cell death. Intriguingly, we documented autophagosomes in proximity to biotrophic hyphae using transmission electron microscopy (TEM) and a concurrent increase in autophagic flux between early to mid/late biotrophic phase of the infection process. Occasionally, we observed osmiophilic bodies in the vicinity of biotrophic hyphae using TEM only and near necrotrophic hyphae under both TEM and SBF-SEM. Overall, we established a method for obtaining serial SBF-SEM images, each with a lateral ( x-y) pixel resolution of 10 nm and an axial ( z) resolution of 40 nm, that can be reconstructed into interactive 3D models using the IMOD. Application of this method to the Colletotrichum–Arabidopsis pathosystem allowed us to more fully understand the spatial arrangement and morphological architecture of the fungal hyphae after they penetrate epidermal cells of Arabidopsis cotyledons and the cytological changes the host cell undergoes as the infection progresses toward necrotrophy. [Formula: see text] Copyright © 2024 The Author(s). This is an open access article distributed under the CC BY 4.0 International license .

Biochemistry & Molecular Biology↗
DOE OSTI2017

Applying Pattern Recognition to High-Resolution Images to Determine Cellular Signaling Status

Two frequently used tools to acquire high-resolution images of cells are scanning electron microscopy (SEM) and atomic force microscopy (AFM). The former provides a nanometer resolution view of cellular features rapidly and with high throughput, while the latter enables visualizing hydrated and living cells. In current practice, these images are viewed by eye to determine cellular status, e.g. activated versus resting. Automatic and quantitative data analysis is lacking. This work develops an algorithm of pattern recognition that works very effectively for AFM and SEM images. Using rat basophilic leukemia (RBL) cells, our approach creates a support vector machine (SVM) to automatically classify resting and activated cells. 10-fold cross-validation with cells that are known to be activated or resting gives a good estimate of the generalized classification results. The pattern recognition of AFM images achieves 100% accuracy, while SEM reaches 95.4% for our images as well as images published in prior literature. This outcome suggests that our methodology could become an important and frequently used tool for researchers utilizing AFM and SEM for structural characterization as well as determining cellular signaling status and function.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2019

Oncologic Outcomes of Self-Expandable Metallic Stent as a Bridge to Surgery and Safety and Feasibility of Minimally Invasive Surgery for Acute Malignant Colonic Obstruction

Background: Although self-expandable metal stents (SEMS) are widely used as a bridge to surgery (BTS) in patients with malignant colorectal cancer obstruction, there has been some debate about their effect on long-term oncological outcomes. Furthermore, data on the safety and feasibility of minimally invasive surgery (MIS) combined with stent placement are scarce. We aimed to determine the long-term oncological outcomes of SEMS as a BTS, and the short-term outcomes of SEMS used with minimally invasive colorectal surgery. Methods: Data from patients who were admitted with malignant obstructing colon cancer between January 2006 and December 2015 were retrospectively reviewed; 71 patients underwent direct surgery and 182 patients underwent SEMS placement as a BTS. Long-term and short-term outcomes of the groups were compared. In a subgroup analysis of the BTS group, the short-term outcomes of conventional open surgery and MIS were compared. Results: There were no differences in long-term oncologic outcomes between groups. The primary anastomosis rate was higher in the stent group than in the direct surgery group. In the stent group, postoperative complication rates were lower in the minimally invasive group than in the open surgery group. Time to flatus and time to soft diet resumption were shorter in the minimally invasive group, as was length of hospital stay. Conclusions: Elective surgery after stent insertion does not adversely affect long-term oncologic outcomes. Furthermore, MIS combined with stent insertion for malignant colonic obstruction is safe and feasible.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2014

Carbon Dioxide Sealing Capacity: Textural or Compositional Controls? (Final Scientific/Technical Report)

This research project is aiming to assess the carbon dioxide sealing capacity of most common seal-rocks, such as shales and non-fractured limestones, by analyzing the role of textural and compositional parameters of those rocks. We hypothesize that sealing capacity is controlled by textural and/or compositional parameters of caprocks. In this research, we seek to evaluate the importance of textural and compositional parameters affecting the sealing capacity of caprocks. The conceptual framework involves two testable end-member hypotheses concerning the sealing capacity of carbon dioxide reservoir caprocks. Better understanding of the elements controlling sealing quality will advance our knowledge regarding the sealing capacity of shales and carbonates. Due to relatively low permeability, shale and non-fractured carbonate units are considered relatively impermeable formations which can retard reservoir fluid flow by forming high capillary pressure. Similarly, these unites can constitute reliable seals for carbon dioxide capture and sequestration purposes. This project is a part of the comprehensive project with the final aim of studying the caprock sealing properties and the relationship between microscopic and macroscopic characteristics of seal rocks in depleted gas fields of Oklahoma Panhandle. Through this study we examined various seal rock characteristics to infer about their respective effects on sealing capacity in special case of replacing reservoir fluid with super critical carbon dioxide (scCO 2 ). To assess the effect of textural and compositional properties on scCO 2 maximum retention column height we collected 30 representative core samples in caprock formations in three counties (Cimarron, Texas, Beaver) in Oklahoma Panhandle. Core samples were collected from various seal formations (e.g., Cherokee, Keys, Morrowan) at different depths. We studied the compositional and textural properties of the core samples using several techniques. Mercury Injection Porosimetry (MIP), Scanning Electron Microscopy SEM, and Sedigraph measurements are used to assess the pore-throat-size distribution, sorting, texture, and grain size of the samples. Also, displacement pressure at 10% mercury saturation (Pd) and graphically derived threshold pressure (P c ) were determined by MIP technique. SEM images were used for qualitative study of the minerals and pores texture of the core samples. Moreover, EDS (Energy Dispersive X-Ray Spectrometer), BET specific surface area, and Total Organic Carbon (TOC) measurements were performed to study various parameters and their possible effects on sealing capacity of the samples. We found that shales have the relatively higher average sealing threshold pressure (P c ) than carbonate and sandstone samples. Based on these observations, shale formations could be considered as a promising caprock in terms of retarding scCO 2 flow and leakage into above formations. We hypothesized that certain characteristics of shales (e.g., 3 fine pore size, pore size distribution, high specific surface area, and strong physical chemical interaction between wetting phase and mineral surface) make them an efficient caprock for sealing super critical CO 2 . We found that the displacement pressure at 10% mercury saturation could not be the ultimate representative of the sealing capacity of the rock sample. On the other hand, we believe that graphical method, introduced by Cranganu (2004) is a better indicator of the true sealing capacity. Based on statistical analysis of our samples from Oklahoma Panhandle we assessed the effects of each group of properties (textural and compositional) on maximum supercritical CO 2 height that can be hold by the caprock. We conclude that there is a relatively strong positive relationship (+.40 to +.69) between supercritical CO 2 column height based on P c and hard/ soft mineral content index (ratio of minerals with Mohs hardness more than 5 over minerals with Mohs hardness less than 5) in both shales and limestone samples. Average median pore radius and porosity display a strong negative correlation with supercritical CO 2 retention column height. Also, increasing bulk density is positively correlated with the supercritical CO 2 retention column height. One of the most important factors affecting sealing capacity and consequently the height of supercritical CO 2 column is sorting of the pore throats. We observed a strong positive correlation between pore throat sorting and height of CO 2 retention column, especially in shales. This correlation could not be observed in limestone samples. It suggests that the pore throat sorting is more controlling the sealing capacity in shales and shales with well sorted pore throats are the most reliable lithology as seal. We observed that Brunauer–Emmett–Teller (BET) surface area shows a very strong correlation with CO 2 retention column height in limestone samples while BET surface area did not display significant correlation in shales. Pore structure based on SEM micrographs exhibits strong correlation with CO 2 retention column height in limestones. Both intercrystalline and vuggy structures have negative correlations while intergranular texture has positive correlation in limestone with respect to CO 2 retention column height. Textural effects observed on SEM micrographs did not show statistically significant correlation with supercritical CO 2 retention column height in shale samples. Finally, we showed that increasing hard/soft mineral index is strongly correlated with the displacement pressure in limestone samples. Vuggy texture displays a relatively strong and negative correlation with displacement pressure values at 10% mercury saturation in shale samples.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2016

Morphological Comparison of U3O8 Ore Concentrates from Canada Key Lake and Namibia Sources

Uranium ore concentrates from two different sources were examined using scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The ore powders are referred to as Namibia (id. no. 90036, LIMS id. no. 18775) and Canada Key Lake (id. no. 90019, LIMS id. no. 18774). Earlier work identified the ores as the U₃O₈ phase of uranium oxide using x-ray diffraction. Both sets of powders were in the form of dark brown to black powder fines. However, the Canada Key Lake concentrates contained larger chunks of material on the millimeter scale that were easily visible to the unaided eye. The powders were mounted for SEM examination by hand dispersing a small amount onto conductive sticky tape. Two types of applicators were used and compared: a fine-tipped spatula and a foam-tipped applicator. The sticky tape was on a standard SEM “tee” mount, which was tapped to remove loose contamination before being inserted into the SEM.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗