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DOE OSTI2024

Model Development for Thermal-Hydrology Simulations of a Full-Scale Heater Experiment in Opalinus Clay

Disposal of commercial spent nuclear fuel in a geologic repository is studied. In situ heater experiments in underground research laboratories provide a realistic representation of subsurface behavior under disposal conditions. Here, this study describes process model development and modeling analysis for a full-scale heater experiment in opalinus clay host rock. The results of thermal-hydrology simulation, solving coupled nonisothermal multiphase flow, and comparison with experimental data are presented. The modeling results closely match the experimental data.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Rheo-Structural Spectroscopy: Fingerprinting the In Situ Response of Fluids to Arbitrary Flow Fields

The objectives of this project were to develop new sample environments, measurement methodologies and associated modeling tools for characterizing the structural response to arbitrarily complex processing flows using small angle scattering, and to apply these new tools for understanding the fundamental physics governing the structuring of anisotropic particulate and polymeric materials under flow histories and conditions relevant to industrial processing flows. The research resulted in the development and implementation of a new sample environment, the fluidic four roll mill (FFoRM), for in situ small angle neutron and X-ray scattering (SANS/SAXS) measurements. These measurements are capable of generating large data sets that “fingerprint” how a complex fluid responds to a wide range of flow histories involving time variations in deformation type and rate. New modeling tools were developed to extract detailed microstructural information from such data sets, including orientation distribution functions and interparticle correlation functions, as well as reduced-order parametric descriptors of these high-dimensional functions that can be used to readily map, visualize and interpret a fluid’s structural response to its flow history. These new tools were applied to a range of model materials involving elongated particle suspensions in order to provide new insights into the physics of how flow couples with orientational and structural order in complex flows, particularly under non-dilute conditions for which no accurate theories currently exist. Using these investigations, we elucidated a number of new insights into the fundamental phenomena driving such process-structure-property relationships. These findings provide guidance for the further development of rheological models, and ultimately can inform the rational and model-based design of flow processes to achieve optimized orientational ordering that is key to the properties and function of a wide range of energy-relevant materials.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Temperature‐Dependent Crystallization in Two‐Step Perovskite Deposition Revealed by In Situ GIWAXS and Machine Learning‐Guided Analysis

The performance and stability of perovskite solar cells are strongly governed by the crystallization behavior of their active layer. In two-step sequential deposition, early-stage film formation plays a decisive role in determining final phase purity and device quality. Guided by a data-driven analysis of nearly 39 000 devices in the FAIR perovskite database, we identified solvent-mediated quenching and thermal processing as key variables affecting power conversion efficiency (PCE), particularly in two-step fabrication. Here, to investigate these effects in real time, we designed and implemented a custom-built, temperature-controlled spin-coating system, enabling precise thermal modulation during precursor deposition. Using this platform, we performed in situ GIWAXS measurements to study the crystallization dynamics of FA 0.5 MA 0.5 PbI 3 films over a temperature range of 30°C–90°C. Our results reveal a non-monotonic relationship between spin-coating temperature and α-phase formation, governed by the interplay between precursor interdiffusion, PbI 2 crystallinity, and δ-phase suppression. The custom thermal control enabled us to isolate and quantify these competing effects during the earliest stages of film formation, providing mechanistic insight into how spin-coating temperature governs both phase purity and kinetic pathways in two-step perovskite systems. Temperature-dependent SEM and photovoltaic device measurements further demonstrate that early-stage crystallization pathways directly translate into differences in morphology, charge-transport continuity, and device performance. These findings inform targeted strategies for optimizing deposition protocols to balance rapid nucleation, phase stability, and device performance.

Saadawy, Ahmed [King Fahd University of Petroleum ↗

DOE OSTI2025

Evaluation of Hanford 200 West Area Tank Farms (241-S/241-SX-/241-U tank farms) Physical Properties Data for Use in Development of West Area Tank Treatment (WATT) Processing

With the recent acceptance of West Area Tank Treatment disposition alternative for 200 West Area tanks at the Hanford Site by the State of Washington and the U.S. Department of Energy, a review was initiated to identify the physical properties data available in the literature for the Hanford 241-S, 241-SX, and 241-U tank farms. The literature reviewed indicated that there is a relatively small set of useful data on physical properties of 200 West Area tanks, and the data that do exist are biased around a narrow range of tank samples. Much of the testing between the 1990s and mid-2010s was intended to support either enhanced sludge washing or feed delivery to the Pretreatment Facility at the Hanford Waste Treatment and Immobilization Plant. As such, some physical properties of 200 West Area samples were measured under conditions that are no longer relevant. Because of the distinctly different nature of many past processes at the 200 West Area compared to the 200 East Area, insight from waste testing in the 200 East Area waste should be used with caution, as there may be significantly different qualities in the physical properties data between these two areas (both in situ and as measured in laboratory analyses). Based on this assessment, there is a need to collect additional physical property data to support planning for 200 West Area retrievals.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

An Automatic Processing Framework for In Situ Determination of Ecohydrological Root Water Content by Ground-Penetrating Radar

This report concerns Root water content (RWC) as a vital component in water flux in soil-plant-atmosphere continuum. Knowledge of RWC helps to better understand the root function and the soil-root interaction and improves water cycle modeling. However, due to the lack of appropriate methods, field monitoring of RWC is seriously constrained. In this study, we used ground-penetrating radar (GPR), a common geophysical technique, to characterize RWC of coarse roots noninvasively. An automatic GPR data processing framework was proposed to (1) identify hyperbolic root reflections and locate roots in GPR images and (2) extract waveform parameters from the reflected wave of identified roots. These waveform parameters were then used to establish an empirical model and a semiempirical model to determine RWC. We validated the developed models using GPR root data at three antenna center frequencies (500 MHz, 900 MHz, and 2 GHz) that were produced from simulation experiments (with RWC ranging from 70% to 150%) and field experiments in sandy soils (with RWC ranging from 66% to 144%). Our results show that both the empirical and the semiempirical models achieved a good performance in estimating RWC with similar accuracy, i.e., the prediction error [root-mean-square error (RMSE)] was less than 8% for the simulation data and 12% for the field data. For both models, the accuracy of RWC estimation was the highest when applied to 2-GHz data. This study renders a new opportunity to determine RWC under field conditions that enhances the application of GPR for root study and the understanding and modeling of ecohydrology in the rhizosphere.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2007

Measuring a Precise Ultra-Lightweight Spaceflight Mirror on Earth: The Analysis of the SHARPI PM Mirror Figure Data during Mirror Processing at GSFC

The SHARPI (Solar High Angular Resolution Photometric Imager) primary mirror is a 5kg, 0.5m paraboloid, diffraction limited at FUV wavelengths when placed in a 0-G environment. The ULE sandwich honeycomb mirror and the attached mount pads were delivered by ITT (then Kodak) in 2003 to NASA s Goddard Space Flight Center (GSFC). At GSFC, we accepted, coated, mounted, and vibration tested this mirror in preparation for flight on the PICTURES (Planet Imaging Concept Testbed Using a Rocket Experiment) mission. At each step, the integrated analysis of interferometer data and FEA models was essential to quantify the 0-G mirror figure. This task required separating nanometer sized variations from hundreds of nanometers of gravity induced distortion. The ability to isolate such features allowed in-situ monitoring of mirror figure, diagnosis of perturbations, and remediation of process errors. In this paper, we describe the technical approach used to achieve these measurements and overcome the various difficulties maintaining UV diffraction-limited performance with this aggressively lightweighted mirror.

Antonille, Scott↗

NASA NTRS2022

Predicting Antarctic Net Snow Accumulation at the Kilometer Scale and Its Impact on Observed Height Changes

Sub-grid-scale processes occurring at or near the surface of an ice sheet have a potentially large impact on local and integrated net accumulation of snow via redistribution and sublimation. Given observational complexity, they are either ignored or parameterized over large-length scales. Here, we train random forest (RF) models to predict variability in net accumulation over the Antarctic Ice Sheet using atmospheric variables and topographic characteristics as predictors at 1 km resolution. Observations of net snow accumulation from both in situ and airborne radar data provide the input observable targets needed to train the RF models. We find that local net accumulation deviates by as much as 172% of the atmospheric model mean. The correlation in space between the predicted net accumulation variability and satellite-derived surface-height change indicates that surface processes operate differently through time, driven largely by the seasonal anomalies in snow accumulation.

Antarctic↗

NASA NTRS2006

Floating the Ball: Advances in the Technology of Electrostatic Levitation

Electrostatic Levitation (ESL) is an emerging technology. The MSFC ESL is a NASA facility that supports investigations of refractory solids and melts. The facility can be used to process a wide variety of materials including metals, alloys, ceramics, glasses and semiconductors. Containerless processing via ESL provides a high-purity environment for the study of high temperature materials and access to metastable states. Scientific topics investigated in the facility include nucleation, undercooling, metastable state formation and metallic glass formation. Additionally, the MSFC ESL provides data for the determination of phase diagrams, time-temperature-transition diagrams, viscosity, surface tension, density, heat capacity and creep resistance. In order to support a diverse research community, the MSFC ESL facility has developed a number of technical capabilities, including a portable system for in situ studies of structural tran$hrmations during processing at the high-energy X-ray beamline at the Advanced Photon Source of Argonne National Laboratory. The capabilities of the MSFC ESL facilities will be discussed and selected results of materials processing and characterization studies will be presented.

Rogers, Jan R.↗

DOE OSTI2026

Evaluation of daily gridded climate products using in situ FLUXNET data and tree growth modeling

Gridded climate data products have facilitated research in climate and ecology by providing meteorological data continuously across large spatial scales. However, the sensitivity of scientific outcomes to dataset choice remains poorly understood, and evaluation using station-based records can favor datasets built heavily on weather stations. Here, we evaluate seven high-resolution daily gridded datasets covering the contiguous United States using independent meteorology from the FLUXNET2015 dataset, with a focus on the implications of dataset choice for process-based tree growth modeling. We find that gridded products tend to capture temperature accurately while consistently overestimating the magnitude and frequency of precipitation and its extremes. Moreover, datasets vary in how they define a ‘day,’ which significantly affects temporal alignment with FLUXNET2015 observations. Despite differences among the datasets, the interannual variability in tree ring simulations is insensitive to dataset choice, likely because daily-scale biases are averaged out through accumulated growth across several months. However, inaccuracies in temperature and precipitation can significantly bias modeled xylem cell production, with systematically higher annual precipitation in the gridded datasets leading to greater xylem production compared to simulations using in situ data. Our results suggest that model applications, especially those that integrate to time scales longer than one day, are likely insensitive to climate dataset choice, but applications that are sensitive to daily climate variations or to absolute climate values need to carefully consider biases in gridded climate products.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2011

Next-Generation Aura/OMI NO2 and SO2 Products

The measurement of both SO2 and NO2 gases are recognized as an essential component of atmospheric composition missions. We describe current capabilities and limitations of the operational Aura/OMI NO2 and SO2 data that have been used by a large number of researchers. Analyses of the data and validation studies have brought to light a number of areas in which these products can be expanded and improved. Major improvements for new NASA standard (SP) NO2 product include more accurate tropospheric and stratospheric column amounts, along with much improved error estimates and diagnostics. Our approach uses a monthly NO2 climatology based on the NASA Global Modeling Initiative (GMI) chemistry-transport model and takes advantage of OMI data from cloudy scenes to find clean areas where the contribution from the trap NO2 column is relatively small. We then use a new filtering, interpolation and smoothing techniques for separating the stratospheric and tropospheric components of NO2, minimizing the influence of a priori information. The new algorithm greatly improves the structure of stratospheric features relative to the original SP. For the next-generation OMI SO2 product we plan to implement operationally the offline iterative spectral fitting (ISF) algorithm and re-process the OMI Level-2 SO2 dataset using a priori SO2 and aerosol profiles, clouds, and surface reflectivity appropriate for observation conditions. This will improve the ability to detect and quantify weak tropospheric SO2 loadings. The new algorithm is validated using aircraft in-situ data during field campaigns in China (2005 and 2008) and in Maryland (Frostburg, 2010 and DISCOVER-AQ in July 2011). The height of the SO2 plumes will also be estimated for high SO2 loading cases (e.g., volcanic eruptions). The same SO2 algorithm will be applied to the data from OMPS sensor to be launched on NPP satellite later this year. The next-generation NO2 and SO2 products will provide critical information (e.g., averaging kernels) for evaluation of chemistry-transport models, for data assimilation, and to impose top-down constraints on the SO2 and NO2 emission sources.

Krotkov, Nickolay↗

DOE OSTI2022

An Investigation of Chemo-Mechanical Phenomena and Li Metal Penetration in All-Solid-State Lithium Metal Batteries Using In Situ Optical Curvature Measurements

Solid-electrolytes (SEs) can provide a pathway to increase energy-density in lithium metal batteries. However, lithium metal penetration through garnet based LLZO solid electrolytes has been identified as a critical failure process. This phenomenon is related to chemo-mechanical processes which are difficult to probe. In particular, characterizing the dynamic mechanical deformations that occur in electrode-SE structures is very challenging. Here study reports in situ curvature measurements that are thus designed to probe chemo-mechanical phenomena that occur during lithium plating. The novel experimental cell configuration created for this work shows that pressure builds up in the Li metal during plating, up until the point where short circuits occur. The resulting data are analyzed with a detailed finite element model (FEM) to quantitatively evaluate stress evolution. The results show that Li metal plating within a surface flaw can produce stress build-up prior to short-circuiting. The combined results from both the experiments and the FEM suggest that it is critical to minimize surface defects and flaws during the manufacturing processes.

25 ENERGY STORAGE↗

DOE OSTI2021

Portable quantitative confocal Raman spectroscopy: Non-destructive approach of the carbonation chemistry and kinetics

Highlights: • Raman spectroscopy was used to monitor carbonation of portlandite • The approach was non-destructive, continuous, and performed within the material • Carbonation was identified coupling Raman spectroscopy and chemometrics • Kinetics was calculated for one portlandite thickness at different CO{sub 2}-percentages Carbonation is one major alteration process of cementitious materials. It can be monitored through several methods, all destructive. In this study, some preliminary investigations were conducted to monitor the carbonation process of pure portlandite with an in situ and non-destructive spectroscopic method. This complementary approach was motivated by a literature review indicating the benefits of Raman spectroscopy, but requiring innovative approaches for data acquisition and analysis. The material was selected to validate this spectroscopic monitoring, coupled with chemometrics tools to allowing an early detection of the carbonation reaction through a structure identified in the spectra data population. The carbonation occurred abruptly, and spectra analysis indicated the occurrence of phases synonymous of microstructural evolutions. Varying the atmospheric percentage of CO{sub 2} (0.04% - 4%) conducted to an appreciation of the kinetics of the carbonation front through the same thickness of portlandite.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Massive all-atom analysis of 2D materials with quantum properties (Final report)

Improvements in microscopy have enabled the acquisition of data at a scale that is difficult to process manually, making automated machine learning approaches to analyzing experimental images essential. In this project, we developed and applied machine learning (ML) workflows for atomic resolution scanning transmission electron microscopy (STEM) images. This development included improving both methodology as well as generating user-friendly codes. We developed machine learning architectures which, after training, automatically identify the location and types of defects throughout a material. We used these data to produce class-averaged images of 2D atomic coordinates with up to 0.3 pm precision, uncovering the structure and oscillations of long-range strain fields around point defects in WSe 2-2x Te 2x . We also resolved a long-standing problem in this field in the training of ML models, a lack of labeled experimental data, by developing a cycle-GAN that transformed simulated-generated labeled data into labeled data indistinguishable from experiment and therefore suitable for training. This removed the remaining parts of the ML data processing workflow where human intervention was still critical and therefore a bottleneck to working at scale. Codes have been developed and released for this full machine learning workflow. ML approaches to partially automate STEM acquisition were also developed. Finally we applied ML and other advanced data processing methods to several materials science problems in two-dimensional materials, including studying the evolution of hyperuniformity with defect concentration in WSe2, understanding phase transformations in transition metal dichalcogenides during in-situ heating in the STEM, and exploring how 2D interfaces transform from twisted into aligned structures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS2001

ECC Ozonesonde Reliability, Observations, and Comparisons with Satellite Ozone Instruments

Electrochemical Concentration Cell (ECC) ozone instruments depend on the quality of care exercised in their pre-flight preparation. The ozone-measuring project conducted at Goddard Space Flight Center's Wallops Flight Facility uses a number of mechanisms designed to inspect the ECC for anomalies that may interfere with the reception of valid ozone profiles. Complete electronic testing of the instrument, individually and when coupled to its radiosonde has led to exceptional monitoring of ozone for detecting long-term atmospheric changes. A number of factors are considered when preparing an ECC instrument for flight. These basically are specific calibrations of pump efficiency, volumetric flow rate, temperature of the air entering the pump, and background current. The concentration of the potassium iodide solution is also important. Wallops is the only site using a UV photometer (Dasibi) to compare ECC ozone output at various concentrations of ozone that allows adjustment to be made to offsets that may appear in the balloon-borne instrument prior to release. All of the above procedures allow identification of potential problems before release of the ECC instrument. Procedures followed at Wallops also are employed in Brazil, and Ascension Island where NASA has cooperative agreements in place to obtain ozonesondes data. All ECC instruments are prepared 3-4 weeks prior to the day of observation. We will briefly describe the instrumental tests employed. These tests have included simultaneous dual observations to compare the effect of different solution concentrations, comparison of sensors of different manufacturers, and comparisons with surface- and space-based instrumentation such as the Dobson Spectrophotometer and satellites. Vertical profiles of ozone from Arctic, mid-latitudes, and Antarctica will be discussed. Although not unusual, the data reveals ozone structure that correlate well with typical atmospheric temperatures and possibly relative humidity. Finally, vertical ozone distribution, compared with remotely measured ozone from lidar and satellite, will be discussed. Specific comparisons between ECC and HALOE measurements, integrated ECC total ozone overburden with the EP-TOMS and the Dobson, as well as comparisons with lidar are discussed. Results show agreement and some disagreement between the in situ measurements of the ECC and the remote instruments. We postulate reasons for the differences, or biases, which in spite of the excellent ECC quality control during pre-flight preparation and data analysis processes, may be due to uncertainties in both measuring systems.

Schmidlin, F. J.↗

NASA NTRS2002

Decadal Changes in Global Ocean Annual Primary Production

The Sea-viewing Wide Field-of-View Sensor (SeaWiFS) has produced the first multi-year time series of global ocean chlorophyll observations since the demise of the Coastal Zone Color Scanner (CZCS) in 1986. Global observations from 1997-present from SeaWiFS combined with observations from 1979-1986 from the CZCS should in principle provide an opportunity to observe decadal changes in global ocean annual primary production, since chlorophyll is the primary driver for estimates of primary production. However, incompatibilities between algorithms have so far precluded quantitative analysis. We have developed and applied compatible processing methods for the CZCS, using modern advances in atmospheric correction and consistent bio-optical algorithms to advance the CZCS archive to comparable quality with SeaWiFS. We applied blending methodologies, where in situ data observations are incorporated into the CZCS and SeaWiFS data records, to provide improvement of the residuals. These re-analyzed, blended data records provide maximum compatibility and permit, for the first time, a quantitative analysis of the changes in global ocean primary production in the early-to-mid 1980's and the present, using synoptic satellite observations. An intercomparison of the global and regional primary production from these blended satellite observations is important to understand global climate change and the effects on ocean biota. Photosynthesis by chlorophyll-containing phytoplankton is responsible for biotic uptake of carbon in the oceans and potentially ultimately from the atmosphere. Global ocean annual primary decreased from the CZCS record to SeaWiFS, by nearly 6% from the early 1980s to the present. Annual primary production in the high latitudes was responsible for most of the decadal change. Conversely, primary production in the low latitudes generally increased, with the exception of the tropical Pacific. The differences and similarities of the two data records provide evidence of how the Earth's climate may be changing and how ocean biota respond. Furthermore, the results have implications for the ocean carbon cycle.

Gregg, Watson↗

NASA NTRS2013

Petrologic and In Situ Geochemical Constraints on Diogenite Genesis

Diogenites, members of the howardite, eucrite and diogenite (HED) clan, are orthopyroxenite, harzburgite and dunite meteorites [1-3]. Most are breccias, but remnant textures indicate they were originally coarse-grained rocks, with grain sizes of order of cm. Their petrography and compositions support an origin as crustal cumulates from a differentiated asteroid. Astronomical observations, and surface mineralogy and composition of Vesta determined by the Dawn spacecraft suggest that asteroid (4) Vesta is the parent object for HED meteorites [4-6]. The origin of diogenites is an unsettled issue. It is difficult to fit their bulk compositional characteristics into global magma ocean models that successfully describe the compositions of basaltic and cumulate eucrites [7]. Compositional analyses of acid-leached bulk samples have led to the hypothesis that many diogenites were formed late by interaction of their parent melts with a eucritic crust [8]. Those observations may alternatively be explained by subsolidus equilibration of trace elements between orthopyroxene and minor/ accessory phases in the rocks such as plagioclase and phosphate [7]. These competing hypotheses can be tested through in situ measurements of trace and minor elements in orthopyroxene. Our new petrologic observations and in situ minor and trace element data for a suite of diogenites are used to discuss the petrologic evolution of diogenites. Our preliminary data on two diogenites are consistent with the hypothesis that subsolidus element mobilization processes caused unusual trace element signatures seen in some diogenites [7]. We cannot stress strongly enough, however, that the sample set is too small and that additional data are required before definitive conclusions can be made.

Mittlefehldt, David W.↗

NASA NTRS2012

Mar's Science Laboratory : Qualification Model Dirty Testing (QMDT) Support

The Martian missions of Spirit, Opportunity, and many others have sparked high interest in Mars which has led to Curiosity to answer questions that we have sought after for years. Has life ever existed on Mars? Through the collection and analyzation of samples, it will help to answer questions about the possibilities of life that may have existed on Mars, and we will gain valuable data about the planet Mars.

Qualification Model Dirty Testing (QMDT)↗

NASA NTRS2002

Clues to Coral Reef Health: Integrating Radiative Transfer Modeling and Hyperspectral Data

An important contribution to coral reef research is to improve spectral distinction between various health states of coral species in areas subject to harmful anthropogenic activity and climate change. New insights into radiative transfer properties of corals under healthy and stressed conditions can advance understandings of ecological processes on reefs and allow better assessments of the impacts of large-scale bleaching and disease events, Our objective was to examine the spectral and spatial properties of hyperspectral sensors that may be used to remotely sense changes in reef community health. We compare in situ reef environment spectra (healthy coral, stressed coral, dead coral, algae, and sand) with airborne hyperspectral data to identify important spectral characteristics and indices. Additionally, spectral measurements over a range of water depths, relief, and bottom types are compared to help quantify bottom-water column influences. In situ spectra were collected in July and August 2002 at the Long Rock site in the Andros Island, Bahamas coastal zone coral reef. Our primary emphasis was on Acropora palmata (or elkhorn coral), a major reef building coral, which is prevalent in the study area, but is suffering from white band disease. A. palmata is currently being, proposed as an endangered species because its populations have severely declined in many areas of the Caribbean. In addition to the A. palmata biotope, we have collected spectra of at least seven other coral biotopes that exist within the study area, each with different coral community composition, density of corals, relief, and size of corals. Coral spectral reflectance was then input into a radiative transfer model, CORALMOD (CM1), which is based on a leaf radiative transfer model. In CM1, input coral reflectance measurements produce modeled reflectance through an inversion at each visible wavelength to provide the absorption spectrum. Initially, we imposed a scattering baseline that is the same regardless of the coral condition and that coral is optically thick and no light is transmitted through coral. Here we will focus on methodology, experimental design, and initial findings of the in situ spectral measurements and preliminary output from the radiative transfer model.

Guild, Liane↗