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At least 757 records · Page 42
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Building Intelligent Cyberinfrastructure to Learn Iteratively from both Observations and Models for Understanding Watershed Dynamics

Focal Area(s): Predictive modeling through the use of AI techniques and AI-derived model components; the use of AI and other tools to design a prediction system comprising of a hierarchy of models (e.g., AI-driven model/component/parameterization selection). Science Challenge: Watershed processes, such as the fate and transport of sediment, carbon and nutrients across landscapes and their fluxes to water bodies (e.g., streams, rivers and lakes), have important implications for global and regional carbon and nutrient dynamics, biogeochemical functioning of terrestrial ecosystems, and soil functions. The magnitude of lateral surface/subsurface transport and fluxes of sediment, carbon and nutrients are key factors controlling the vulnerability of watersheds to climate extremes such as droughts, wildfires, and floods. Recent field observations and other scientific evidence suggest that the magnitudes of lateral transport and fluxes of sediment, carbon and nutrients are governed primarily by the spatial and vertical heterogeneity of landscape and soil properties and by pedogenic processes. However, the current generation of land surface and watershed models do not mechanistically couple the terrestrial and hydrologic systems, nor do they represent sufficiently the spatial and vertical heterogeneity of land surface and subsurface properties. On the other hand, increasing complexity of coupled watershed and land surface models requires more data to parameterize, calibrate and validate. Remote sensing (RS) provides a means to acquire spatial data and characterize their heterogeneity at the watershed scale, overcoming a major limitation associated with conventional point measurements. To improve the representation of land-surface and surface/subsurface process coupling and sub-grid heterogeneity in watershed models, it is essential to build our predictive understanding by learning from both the multi-scale multi-process modeling and diverse multi-scale data while leveraging powerful artificial intelligence (AI) techniques.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2017

Active Cryovolcanism on Europa?

Evidence for plumes of water on Europa has previously been found using the Hubble Space Telescope using two different observing techniques. Roth et al. found line emission from the dissociation products of water. Sparks et al. found evidence for off-limb continuum absorption as Europa transited Jupiter. Here, we present a new transit observation of Europa that shows a second event at the same location as a previous plume candidate from Sparks et al., raising the possibility of a consistently active source of erupting material on Europa. This conclusion is bolstered by comparison with a nighttime thermal image from the Galileo Photopolarimeter-Radiometer that shows a thermal anomaly at the same location, within the uncertainties. The anomaly has the highest observed brightness temperature on the Europa nightside. If heat flow from a subsurface liquid water reservoir causes the thermal anomaly, its depth is ≈1.8–2 km, under simple modeling assumptions, consistent with scenarios in which a liquid water reservoir has formed within a thick ice shell. Models that favor thin regions within the ice shell that connect directly to the ocean, however, cannot be excluded, nor modifications to surface thermal inertia by subsurface activity. Alternatively, vapor deposition surrounding an active vent could increase the thermal inertia of the surface and cause the thermal anomaly. This candidate plume region may offer a promising location for an initial characterization of Europa’s internal water and ice and for seeking evidence of Europa’s habitability.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS2013

A Mars Sample Return Sample Handling System

We present a sample handling system, a subsystem of the proposed Dragon landed Mars Sample Return (MSR) mission [1], that can return to Earth orbit a significant mass of frozen Mars samples potentially consisting of: rock cores, subsurface drilled rock and ice cuttings, pebble sized rocks, and soil scoops. The sample collection, storage, retrieval and packaging assumptions and concepts in this study are applicable for the NASA's MPPG MSR mission architecture options [2]. Our study assumes a predecessor rover mission collects samples for return to Earth to address questions on: past life, climate change, water history, age dating, understanding Mars interior evolution [3], and, human safety and in-situ resource utilization. Hence the rover will have "integrated priorities for rock sampling" [3] that cover collection of subaqueous or hydrothermal sediments, low-temperature fluidaltered rocks, unaltered igneous rocks, regolith and atmosphere samples. Samples could include: drilled rock cores, alluvial and fluvial deposits, subsurface ice and soils, clays, sulfates, salts including perchlorates, aeolian deposits, and concretions. Thus samples will have a broad range of bulk densities, and require for Earth based analysis where practical: in-situ characterization, management of degradation such as perchlorate deliquescence and volatile release, and contamination management. We propose to adopt a sample container with a set of cups each with a sample from a specific location. We considered two sample cups sizes: (1) a small cup sized for samples matching those submitted to in-situ characterization instruments, and, (2) a larger cup for 100 mm rock cores [4] and pebble sized rocks, thus providing diverse samples and optimizing the MSR sample mass payload fraction for a given payload volume. We minimize sample degradation by keeping them frozen in the MSR payload sample canister using Peltier chip cooling. The cups are sealed by interference fitted heat activated memory alloy caps [5] if the heating does not affect the sample, or by crimping caps similar to bottle capping. We prefer cap sealing surfaces be external to the cup rim to prevent sample dust inside the cups interfering with sealing, or, contamination of the sample by Teflon seal elements (if adopted). Finally the sample collection rover, or a Fetch rover, selects cups with best choice samples and loads them into a sample tray, before delivering it to the Earth Return Vehicle (ERV) in the MSR Dragon capsule as described in [1] (Fig 1). This ensures best use of the MSR payload mass allowance. A 3 meter long jointed robot arm is extended from the Dragon capsule's crew hatch, retrieves the sample tray and inserts it into the sample canister payload located on the ERV stage. The robot arm has capacity to obtain grab samples in the event of a rover failure. The sample canister has a robot arm capture casting to enable capture by crewed or robot spacecraft when it returns to Earth orbit

Wilson, David↗
NASA NTRSDate not supplied

3D Modeling of Solar-Type Stars to Characterize Stellar Jitter

Detection of Earth-mass planets requires measurements of radial velocity with extreme precision. To capture the tiny disturbances caused by a planet's motion, it is necessary to understand and characterize the host star’s turbulent dynamics in order to apply proper filtering to the observational data. We take advantage of current computational and technological capabilities to develop 3D realistic models of the stellar subsurface convection and atmospheres and thereby estimate the photospheric jitter. We have identified an initial set of target stars, obtained initial conditions using the MESA code, and obtained initial 3D radiative models of the stellar surfaces and atmospheres with a spatial resolution of 50km. We present initial 3D radiative hydrodynamic model results of the planet-hosting star HD209458.

SMD↗
DOE OSTI2021

Biogeochemical dynamics and microbial community development under sulfate- and iron-reducing conditions based on electron shuttle amendment

Iron reduction and sulfate reduction are two of the major biogeochemical processes that occur in anoxic sediments. Microbes that catalyze these reactions are therefore some of the most abundant organisms in the subsurface, and some of the most important. Due to the variety of mechanisms that microbes employ to derive energy from these reactions, including the use of soluble electron shuttles, the dynamics between iron- and sulfate-reducing populations under changing biogeochemical conditions still elude complete characterization. Here, we amended experimental bioreactors comprised of freshwater aquifer sediment with ferric iron, sulfate, acetate, and the model electron shuttle AQDS (9,10-anthraquinone-2,6-disulfonate) and monitored both the changing redox conditions as well as changes in the microbial community over time. The addition of the electron shuttle AQDS did increase the initial rate of Fe III reduction; however, it had little effect on the composition of the microbial community. Our results show that in both AQDS- and AQDS+ systems there was an initial dominance of organisms classified as Geobacter (a genus of dissimilatory Fe III -reducing bacteria), after which sequences classified as Desulfosporosinus (a genus of dissimilatory sulfate-reducing bacteria) came to dominate both experimental systems. Furthermore, most of the ferric iron reduction occurred under this later, ostensibly “sulfate-reducing” phase of the experiment. This calls into question the usefulness of classifying subsurface sediments by the dominant microbial process alone because of their interrelated biogeochemical consequences. To better inform models of microbially-catalyzed subsurface processes, such interactions must be more thoroughly understood under a broad range of conditions.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2018

Biochemical Mechanisms and Associated Biomolecular Signatures Underlying Energy Strategies of Geobacter Sulfurreducens

To provide the scientific understanding required to allow DOE sites to incorporate relevant biological, chemical, and physical processes into decisions concerning environmental remediation, a fundamental understanding of the controls on micro-organism growth in the subsurface is necessary. Specifically, mobility of metals in the environment, including chromium, technetium and uranium, is greatly affected by the process of dissimilatory metal reduction (DMR). DMR has been shown to be an important biological activity controlling contaminant mobility in the subsurface at many DOE sites. Long-term maintenance of DMR at constant rates must rely upon steady fluxes of electron donors to provide the maintenance energy needed by organisms such as Geobacter sulfurreducens to maintain steady state populations in the subsurface. At present, much effort has been put forth to develop biomolecular signatures which inform on the relevant biological processes at DOE field sites. These signatures are also being developed in defined laboratory conditions to which the field data can be compared to. These signatures include metagenomic, metatranscriptomic and proteomic characterization. While the relevant processes involve reduction of metal contaminants, we suggest that the predominant biochemistry that impacts the biomolecular signature is nutrient availability/limitation. As such, the present proposal aims at characterizing the survival strategy of Geobacter and obtaining biomolecular signatures that would reflect on its energy flux status. In addition, we lack the fundamental knowledge needed to answer fundamental questions such as these: What influxes of electron donors are required to maintain a growing versus a non-growing population of Geobacter? How do changes in nutrient availability or other environmental conditions such as pH and ionic strength affect such required electron-donor influxes? How are these electron-donor influxes controlled by availability and nature of electron acceptors? Under survival conditions, where availability of electron acceptors and nutrients are extremely low, what physiological and genetic modifications occur in Geobacter to enable long-term survival? How do these changes affect the required electron-donor influxes? Is it possible to relate the metabolic activities of Geobacter living under survival mode to the required fluxes of electron donors? What conceptual models can be used to predict maintenance energies of Geobacter under different phases of growth when measured under different environmental conditions? How can these models help the DOE predict the long-term evolution of contaminated sites? We outline a strategy to tackle these questions and lay the framework for DOE to make long-term predictions concerning DMR in the subsurface. We will test the following hypothesis: Geobacter requires different fluxes of substrate for metabolism when existing under growth, stationary, or survival modes, and these substrate fluxes can be related to specific metabolic activities utilized under different geochemical conditions. Our project has two specific objectives: i) Determine the survival characteristics of Geobacter under long-term stationary phase by characterize the physiological response of Geobacter in growth, stationary, and survival phases using genomic sequencing, DNA microarray chips and iTRAQ (proteomics) and relate these responses to the measured substrate fluxes; ii) Determination of growth yield and maintenance energy. While site-specific studies are necessary for site-specific remediation, our work will provide the fundamental knowledge necessary for long-term stewardship of all DOE sites where contaminant mobility is affected by dissimilatory metal reduction.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Key Learnings from Hydraulic Fracturing Test Site - 2 (HFTS-2), Delaware Basin

Hydraulic fractures (HF) play a dominant role in oil and gas production from unconventional reservoirs, fracture characteristics, geometry, and extent are generally not well known and are typically inferred from various monitoring methods or subsurface models. The Hydraulic Fracturing Test Site-2 (HFTS-2) is a field-based research experiment performed in the Wolfcamp formation of the Permian (Delaware) Basin. HFTS-2, a unique joint industry program (JIP) that brings together government, academia, and industry, focused on field data acquisition and interpretation. The project has built a comprehensive HF research dataset that includes microseismic (MS), 1,500 ft of core, diagnostic formation injection tests (DFIT), fluid characterization, advanced logs, geochemistry, downhole gauges, varying completions, and permanent fiber optic (FO) cable in vertical and horizontal wells. These data were integrated and used to characterize HF geometry/dimensions and resulting depletion profiles, gain insights for completion design, and achieve a better understanding of parent well depletion effects on child well performance. The analysis and integration of the comprehensive HFTS-2 diagnostics dataset provide insights for optimal well placement and completions and improves understanding about the effects of parent well depletion. Furthermore, this dataset can be used to blind test and develop subsurface workflows for unconventional resources. Key learnings from HFTS-2 and the new technologies tested can easily be transferred to other unconventional plays.

58 GEOSCIENCES↗
DOE OSTI2018

Metagenomic evaluation of a Utah tar sand microbiota suggests the predominant hydrocarbonoclastic role of Actinobacteria

Background: Occurrences of tar sands have been reported in 22 states in the United States; however, the largest deposit is located in southwestern Utah. It has been suggested that tar sands were created by the microbial degradation of immobile subsurface oil over several million years; however, little is known about the indigenous microbial communities in the bituminous tar sands. Methods: This study identified Utah tar sand microbiota using next-generation sequencing technology and characterized the functional diversity using community-level physiological profile (CLPP). Results: Microbiota identified in these tar sands are mainly affiliated with the Gram-positive Actinobacteria and representatives of genera that have also been previously shown to degrade aromatic hydrocarbons, including Arthrobacter , Dietzia , Janibacter , Nocardioides , Microbacterium , Agrococcus and Salinibacterium , suggesting that these microbes likely play roles in the biodegradation of oil-hydrocarbons. CLPP analysis revealed less than 24 h was needed for the first color development in the microplate wells containing the polymers, whereas the duration of the lag phase of the carboxylic acids was prolonged. Conclusions: The quick utilization of the polymers suggests that the indigenous microbial community, especially the actinomycetes in the tar sand habitat, are poised and primed to degrade these recalcitrant compounds.

Lewis, Dawn E. (ORCID:0000000206931768)↗
DOE OSTI2018

Sensitivity Analysis of Contaminant Transport from Vadose Zone Sources to Groundwater

Remedy selection and implementation in the Central Plateau of the Hanford Site will be facilitated by a technically defensible description of vadose zone sources and their spatial and temporal impacts on groundwater. To this end, a case study approach is used to assess impacts to groundwater associated with uncertainties in source terms and hydraulic and sorption parameters for the B-Complex at Hanford. Several unplanned releases of wastes occurred in the tanks in the B-Complex. Several planned liquid waste discharges also occurred to cribs, trenches, tile fields, and French drains within the B-Complex, creating a significant inventory of contaminants in the vadose zone whose downward migration in the subsurface pose a potential threat to groundwater. Given the uncertainty in multiple source locations, volumes and intensities, and uncertainties in hydraulic and sorption properties, an integrated assessment of their combined effects is needed to guide characterization, support selection of appropriate remedies, and design appropriate monitoring for vadose zone source areas and the underlying aquifer.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2016

Proteomic Stable Isotope Probing Reveals Biosynthesis Dynamics of Slow Growing Methane Based Microbial Communities

Marine methane seep habitats represent an important control on the global flux of methane between the subsurface and water column reservoirs. Meta-omics studies have begun to outline community-wide metabolic potential, but expression patterns of proteins that enact sulfate-mediated anaerobic methane oxidation in seeps are poorly characterized. Proteomic stable isotope probing (proteomic SIP) offers an additional layer of information for characterizing phylogenetically specific, functionally relevant activity in mixed microbial communities. Here we applied proteomic SIP to 15NH4+ and CH4 amended seep sediment microcosms in an attempt to track the protein synthesis of slow-growing, low-energy microbial systems. Across all samples, 3495 proteins were identified, 21% of which were 15N-labeled. We observed active synthesis (15N enrichment) of all proteins believed to be involved in sulfate reduction and reverse methanogenesis including methylenetetrahydromethanopterin reductase (Mer). The abundance and phylogenetic range of methyl-coenzyme M reductase (Mcr) orthologs produced during incubation experiments suggests that seeps provide sufficient niches for multiple organisms performing analogous metabolisms. Twenty-eight previously unreported post-translational modifications of McrA were measured, indicating dynamic enzymatic machinery and offering a dimension of functional diversity beyond gene-dictated sequence. RNA polymerase associated with putative sulfur-oxidizing Epsilonproteobacteria and aerobic Gammaproteobacteria were more abundant among pre-incubation proteins, suggesting diminished metabolic activity in long-term anoxic, sulfidic experimental incubations. Twenty-six proteins of unknown function were detected in all proteomic experiments and actively expressed in labeled experiments, suggesting that they play important roles in methane seep ecosystems. The addition of stable isotope probing to environmental proteomics experiments provides a mechanism to begin to assess the degree to which diagnostic meatbolic proteins are long-lived or acively synthesized in complex, slow-growing microbial communities. Our work here demonstrates that sediment-hosted microbial assemblages in marine methane seeps are dynamic, heterogeneous systems with broad functional diversity.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS1993

The distribution of ground ice on Mars

A wealth of geologic evidence indicates that subsurface water ice has played an important role in the evolution of Martian landforms. Theoretical models of the stability of ground ice show that in the near-surface regolith ice is currently stable at latitudes poleward of about +/- 40 deg and below a depth of a few centimeters to a meter, with some variations with longitude. If ice is not previously present at a particular location where it is stable, atmospheric water will diffuse into the regolith and condense as ice, driven by the annual subsurface thermal oscillations. The lower boundary of this ice deposit is found to occur at a depth (typically a few meters) where the annual thermal oscillations give way to the geothermal gradient. In the equatorial regions near-surface ice is currently not stable, resulting in the sublimation of any existing ice and subsequent loss to the atmosphere. However, subliming ice might be maintained at a steady-state depth, where diffusion and loss to the atmosphere are balanced by resupply from a possible deeper source of water (either deeper, not yet depleted, ice deposits or ground water). This depth is typically a few tens to hundreds of meters and depends primarily on the surface temperature and the nature of the geothermal gradient, being deeper for a higher surface temperature and a lower geothermal gradient. Such an equatorial deposit is characterized by the regolith ice content being low nearer the surface and increasing with depth in the deposit. Oscillations in the orbit will affect this picture of ground ice in two ways: by causing periodic changes in the pattern of near-surface stability and by producing subsurface thermal waves that may be capable of driving water ice deeper into the regolith.

Mellon, M. T.↗
DOE OSTI2024

Variations in Bedrock and Vegetation Cover Modulate Subsurface Water Flow Dynamics of a Mountainous Hillslope

Abstract Predicting the hydrological response of watersheds to climate disturbances requires a detailed understanding of the processes connecting hillslopes and streams. Using a network of soil moisture and temperature sensors, electrical resistivity tomography monitoring, and a weather station we assess the above and below‐ground processes driving the hydrological response of a hillslope during snowmelt and summer monsoon. The transect covers bedrock and vegetation gradients, with a steep upper part characterized by shallow bedrock, and gentle lower part underlain by colluvium. The main vegetation cover is conifers on the upper, and grass and veratrum on the lower part. Combined with a simplified hydrological model, we show that the thin soil layer of the steep slope acts as a preferential flow path, leading to mostly shallow lateral flow, interrupted by vertical flow, mostly at tree locations, and likely facilitated by flow along fractures and roots. Vertical flow and upstream‐driven groundwater dynamics are prevailing at the colluvium, presenting a very different hydrological behavior compared to the upper part. These results show that subsurface structure and features have a strong control on the hydrological response of a hillslope and that those can create considerably varying hydrological dynamics across small spatial scales.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

Calcium Silicate Crystal Structure Impacts Reactivity with CO 2 and Precipitate Chemistry

The reaction of CO 2(aq) with calcium silicates creates precipitates that can impact fluid flow in subsurface applications such as geologic CO 2 storage and geothermal energy. These reactions nominally produce calcium carbonate (CaCO 3 ) and amorphous silica (SiO x ). Here we report evidence that the crystal structure of the parent silicate determines the way in which it reacts with CO 2 and the resulting structures of the reaction products. Batch experiments were carried out using two polymorphs of a model calcium silicate (CaSiO 3 ), wollastonite (chain-structured) and pseudowollastonite (ring-structured), at elevated temperatures and CO 2(aq) concentrations. Reaction of CO 2(aq) with wollastonite produced CaCO 3 and SiO x , whereas reaction of CO 2(aq) with pseudowollastonite produced numerous plate-like crystalline calcium silicate phases, along with CaCO 3 and SiO x . A reaction mechanism is proposed that explains the observations in relation to dissolution rates of ions from the parent silicate, the pH of the solution, and the presence of nucleation sites. The mechanism is supported with ICP-OES measurements of the aqueous phase and SEM/TEM-SAED characterization of solid products. As a result, these findings are important for a number of reasons among them the fact that the crystalline silicate precipitates are more stable than CaCO 3 at low pH conditions, which would be very valuable for creating permanent seals in subsurface applications.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2013

Characterization and Transcription of Arsenic Respiration and Resistance Genes During In Situ Uranium Bioremediation

The possibility of arsenic release and the potential role of Geobacter in arsenic biogeochemistry during in situ uranium bioremediation was investigated because increased availability of organic matter has been associated with substantial releases of arsenic in other subsurface environments. In a field experiment conducted at the Rifle, CO study site, groundwater arsenic concentrations increased when acetate was added. The number of transcripts from arrA, which codes for the alpha subunit of dissimilatory As(V) reductase, and acr3, which codes for the arsenic pump protein Acr3, were determined with quantitative RT-PCR. Most of the arrA (> 60%) and acr3-1 (> 90%) sequences that were recovered were most similar to Geobacter species, while the majority of acr3-2 (>50%) sequences were most closely related to Rhodoferax ferrireducens. Analysis of transcript abundance demonstrated that transcription of acr3-1 by the subsurface Geobacter community was correlated with arsenic concentrations in the groundwater. In contrast, Geobacter arrA transcript numbers lagged behind the major arsenic release and remained high even after arsenic concentrations declined. This suggested that factors other than As(V) availability regulated transcription of arrA in situ even though the presence of As(V) increased transcription of arrA in cultures of G. lovleyi, which was capable of As(V) reduction. These results demonstrate that subsurface Geobacter species can tightly regulate their physiological response to changes in groundwater arsenic concentrations. The transcriptomic approach developed here should be useful for the study of a diversity of other environments in which Geobacter species are considered to have an important influence on arsenic biogeochemistry.

arsenic resistance↗
DOE OSTI2023

NNSA-IAEC Area: Workshop on Nuclear Waste Management and Subsurface Science (8-10 November 2022)

The 7 th workshop of the NNSA-IAEC collaboration was conducted on November 8-10 2022. The workshop was held at the geologic survey of Israel, Jerusalem. The IAEC hosted the workshop. The main topic of the workshop evolved around the results of the characterization borehole drilled in the Yamin plain during 2022 and associated experimental work and modeling results. The new data will be integrated for the applicability analysis of intermediate depth borehole (IDB) disposal for spent fuel in the Yamin plain. The first day of the workshop (November 8 th ) was dedicated to a geological field trip in the Judea desert depicting a similar cross section to that found in the Yamin plain. During the 9 th and 10 th of November the characterization BH results were presented, results of new work on the Miocene Hazeva fm. were presented, and this year’s outcome of the different collaboration groups were given.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Quantitative Studies of Machining-Induced Microstructure Alteration and Plastic Deformation in AISI 316 Stainless Steel Using EBSD

Surface machining can result in a heavily plastic deformed layer in the subsurface. The microstructure alterations and the extent of plastic deformation of a milled 316 austenitic stainless steel were investigated using electron backscatter diffraction (EBSD) technique in this study. The microstructure alteration of the deformed layer was characterized by the generation of grain and subgrain boundaries. The plastic deformation was evaluated by kernel average misorientation (KAM) and grain average misorientation (GAM). The local deformation within grains was assessed by the misorientation from adjacent point (MFAP). The EBSD results indicated gradients of microstructure and plastic deformation along the depth direction. High-angle grain boundaries were generated within the depth of 40 μm, and subgrain boundaries were produced up to the depth of 150 μm. Estimated by KAM and GAM, the plastic strain was about 0.7 at the depth of 25 μm and decreased to 0.1 at the depth of 115 μm The MFAP analysis revealed that the local deformation varied within individual grains. Additionally, the change of micro-hardness along the depth direction showed a strong correlation with KAM and GAM values.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Argon Milling of Bulk and Post-FIB Specimens for Multi-Length Scale Analyses by EBSD, TEM, and APT under Controlled Environments

Correlative investigations involve structural characterization by transmission electron microscopy (TEM) combined with compositional analysis by atom probe tomography (APT) using the same specimen. A critical component of successful correlative analyses is specimen preparation; probing individual atoms requires a surface and subsurface with minimal defects, beginning with the bulk material through to the prepared specimen for TEM or APT analysis. Our previous work showed that low-energy concentrated ion beam Ar ion milling improves TEM [1] and APT [2,3] specimen quality by removing surface oxides and Ga damage caused by focused ion beam (FIB) preparation. Further enhancement in specimen quality of APT specimens is achieved in the established workflow under controlled environments, as shown in [4]. In this work, we present specimen preparation using Ar ion milling techniques not only for the APT specimen, but also the bulk sample for subsequent multi-length scale analyses by electron backscatter diffraction (EBSD), TEM, and APT under controlled environments. The removal of surface damage and oxidation, which is crucial for probing atomic layer specimens by broad and concentrated Ar ion beam milling techniques under controlled environments, is highlighted.

36 MATERIALS SCIENCE↗