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All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Removable, Sequestration Coatings for Mitigating Hazardous Contaminants Related to Deactivation and Decommissioning Activities

This project is a collaborative effort between InnoSense LLC (ISL) and Oak Ridge National Laboratory (ORNL) aimed at mitigating the mercury (Hg) contamination problem at the Y-12 National Security Complex (NSC). The report summarizes the research and technology development work of the Phase IIB Project, led by Dr. Uma Sampathkumaran at ISL for the period of July 31, 2017–October 31, 2021. The Y-12 site cleanup includes technologies for safe and cost-effective facility demolition, soil remediation, and on-site treatment and disposal of mercury bearing wastes. One of the technology demonstration goals was a reactive strippable coating for targeted pre-demolition and de-contamination to limit Hg mobilization and the volume of debris requiring treatment for disposal. Toward this, ISL has developed a water-based reactive strippable coating (Trap & See-Hg™) to sequester elemental Hg(0) and mercuric Hg(II) species in the coating. The coating provides multiple benefits including (1) Hg vapor suppression, (2) sealing in the hazardous contaminants, (3) visually locating the contaminant through color changes, and (4) remediating the contaminated surfaces upon coating removal. Through collaboration between ORNL and ISL in Phase II work, the team successfully demonstrated the Trap & See-Hg technology to (1) visually locate the presence of Hg on concrete, soil and drywall surfaces, (2) effectively sequester all mercury species (elemental, soluble and insoluble Hg) from lab-generated and ex-situ soil and brick/rubble samples collected from the Y 12 site with 80 to 95% efficiency to capture/reduce Hg vapor concentration, (3) be applied by manual and robotic spray applicators and cure at room ambient, (4) remain a cohesive and peelable coating upon drying, and (5) sequester Hg0 from walls in the alpha-2 building basement at Y-12 during a small scale in-situ field trial. In Phase IIB, ISL’s effort was focused on refining the coating formulations with additives containing passive and reactive sorbents, colorimetric indicator, and thixotropic agents to achieve the desired performance. The paints were then evaluated at ORNL for applicability to metal and concrete surfaces of different sizes and shapes, and soil rubble, Hg-sorption capacity and achieving sag-free coating on surfaces when applied by a manual spray applicator. Ambient cure of the coating resulted in a dry thickness of 16–20 mil. The coatings were removed from smooth or rough surfaces with low to moderate force. Both lab-generated Hg-contaminated samples and soil and brick/rubble samples containing a range of Hg concentrations (collected from the Y-12 site by UCOR) were used in this project. Optimized formulations were applied to these samples and evaluated for ability to suppress Hg vapors, sequester Hg 0 and Hg(II) species and color mapping of mercury species on the test surface. The ORNL team initially identified three to four potential sites at Y-12 and ORNL for potential demonstration. However, the pandemic closed any possible avenues for on-site demonstration of the robotic spray applicator. The metal and concrete samples with low to high Hg content provided by UCOR from an ongoing demolition were subsequently used for ex-situ sample characterization and analysis at ORNL over a period of 25 days. The coatings suppressed Hg vapors with an efficiency of 95–99% from heavily contaminated metal and 60% from concrete substrate. Analysis of total Hg in the peeled paints indicates sorption capacities ranging from 12 µg Hg/g of paint from concrete to 1.2 mg Hg/g of paint from the metal substrates while peeled paints from soil samples could capture a total Hg from 2.3 mg Hg/g to 66 mg/g paint. Toxicity characteristic leaching procedure (TCLP) tests recovered total mercury leached at 0.15±0.0008 µg/L for concrete to 126.81±0.67 µg/L and 377.25±5.67 µg/L for the two metal substrates, to allow for informed decisions on downstream disposal considerations. Together, this Phase IIB demonstrated the potential value of the Trap & See-Hg for Hg uptake, vapor suppression, and color mapping, and may thus be used to enhance worker safety during site cleanup, facility demolition, and downstream waste disposal at Y-12 NSC.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2023

Accelerating Additive Manufacturing Process Design for Energy Conversion Materials using In-situ Sensing and Machine Learning

One promising candidate for manufacturing of the bismuth Telluride thermoelectric legs is laser powder bed fusion (LPBF) additive Manufacturing (AM). AM processing parameters highly influence the material properties, however current processing parameter development methods in AM are costly and time consuming. In-situ sensors allow for the capture of physically relevant process information on a layer-by-layer basis and will be used to aide process development. To optimize the AM process for the best thermoelectric performance, process variables, in-situ process sensor data and ex-situ material characterization data are collected. Several different interpretable machine learning (ML) approaches are used, and the performance of each method are assessed. Significant input process variables include laser focus, hatch spacing and laser power. The best performing models are used to determine the manufacturing parameters that maximize the power factor. AM of bismuth telluride material provides the ability to create complex geometries enabling more efficient energy conversion.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2025

Chemical Analysis of Tantalum Thin Films compared to Niobium Thin Films using SIMS and XPS

Superconducting qubits are a leading platform for quantum computation. These circuits are typically made from superconducting materials like aluminum or niobium. However, the amorphous niobium oxide and aluminum oxide on the surface of these circuits introduce considerable RF loss due to the presence of two-level systems (TLS), which limits the maximum coherence times T1 to ~100 μs. Capping the niobium qubits with a tantalum layer leads to a 3- 5x improvement [Bal et al., 2024]. But even in this case, tantalum forms an amorphous surface oxide that introduces loss. In an effort to devise strategies to eliminate the presence of this oxide, we present a comprehensive study on the nature of Ta oxide using x-ray photoemission spectroscopy (XPS) and secondary ion mass spectrometry (ToF-SIMS) as a function of heat treatment. The thin films were annealed in ultra-high vacuum conditions and analyzed in situ to characterize the composition and evolution of the native tantalum oxide layer and oxide-metal interface. Our analysis reveals two critical differences between tantalum and niobium oxides: Nb2O5 completely dissolves at 400°C, while Ta2O5 persists even at 800°C. Additionally, tantalum oxide contains only a single suboxide (TaO), in contrast to niobium's two suboxides (NbO and NbO2). The suboxide of tantalum contributes minimally to the total oxide content and shows a relative increase with temperature. Understanding the oxide’s behavior will open new pathways for optimizing coherence times in tantalum qubits.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2022

Rotating Disk Electrode Standardization and Best Practices in Acidic Oxygen Evolution for Low-Temperature Electrolysis

Efforts in oxygen evolution catalyst development have significantly increased and often use rotating disk electrode half-cells to evaluate intrinsic kinetics and screen materials for short-term durability. Standardizing rotating disk electrode test protocols is critical to experimental accuracy, to realistically assess their potential impact at a device level and to assess how different catalyst approaches and concepts are prioritized. The goal of this study is to provide standardized test protocols and suggest best practices to help reduce variability in ex situ materials characterization in the broader community. Specifically, these protocols focus on test cleanliness and materials choices, including how electrodes are prepared and tested, and the impact on activity observations.

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

Understanding Selectivity in CO2 Hydrogenation to Methanol for MoP Nanoparticle Catalysts Using In Situ Techniques

Molybdenum phosphide (MoP) catalyzes the hydrogenation of CO, CO2, and their mixtures to methanol, and it is investigated as a high-activity catalyst that overcomes deactivation issues (e.g., formate poisoning) faced by conventional transition metal catalysts. MoP as a new catalyst for hydrogenating CO2 to methanol is particularly appealing for the use of CO2 as chemical feedstock. Herein, we use a colloidal synthesis technique that connects the presence of MoP to the formation of methanol from CO2, regardless of the support being used. By conducting a systematic support study, we see that zirconia (ZrO2) has the striking ability to shift the selectivity towards methanol by increasing the rate of methanol conversion by two orders of magnitude compared to other supports, at a CO2 conversion of 1.4% and methanol selectivity of 55.4%. In situ X-ray Absorption Spectroscopy (XAS) and in situ X-ray Diffraction (XRD) indicate that under reaction conditions the catalyst is pure MoP in a partially crystalline phase. Results from Diffuse Reflectance Infrared Fourier Transform Spectroscopy coupled with Temperature Programmed Surface Reaction (DRIFTS-TPSR) point towards a highly reactive monodentate formate intermediate stabilized by the strong interaction of MoP and ZrO2. This study definitively shows that the presence of a MoP phase leads to methanol formation from CO2, regardless of support and that the formate intermediate on MoP governs methanol formation rate.

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

In-Situ Calibrated Modeling of Residual Stresses Induced in Machining under Various Cooling and Lubricating Environments

Although many functional characteristics, such as fatigue life and damage resistance depend on residual stresses, there are currently no industrially viable ‘Digital Process Twin’ models (DPTs) capable of efficiently and quickly predicting machining-induced stresses. By leveraging advances in ultra-high-speed in-situ experimental characterization of machining and finishing processes under plane strain (orthogonal/2D) conditions, we have developed a set of physics-based semi-analytical models to predict residual stress evolution in light of the extreme gradients of stress, strain and temperature, which are unique to these thermo-mechanical processes. Initial validation trials of this novel paradigm were carried out in Ti-6Al4V and AISI 4340 alloy steel. A variety dry, cryogenically cooled and oil lubricated conditions were evaluated to determine the model’s ability to capture the tribological changes induced due to lubrication and cooling. The preliminarily calibrated and validated model exhibited an average correlation of better than 20% between the predicted stresses and experimental data, with calculation times of less than a second. Based on such fast-acting DPTs, the authors envision future capabilities in pro-active surface engineering of advanced structural components (e.g., turbine blades).

36 MATERIALS SCIENCE↗
NASA NTRS1988

Effect of substrate preparation on the structure and chemisorption properties of Pd/MgO model catalyst

Pd/MgO model catalysts are prepared by vapor deposition of Pd particles on MgO thin films which are deposited, at different temperatures, on UHV cleaved mica. MgO films and Pd particles are characterized in situ by Auger electron spectroscopy and energy-loss spectroscopy and ex situ by transmission electron microscopy. Succesive temperature programmed desorption (TPD) of CO shows a different evolution of the morphology of the Pd particles deposited on MgO films prepared at low and high temperature. In addition, on MgO prepared at low temperature, the smallest particles show a continuous decay of CO adsorption during TPD due to contamination by support species.

Henry, C. R.↗
NASA NTRS2000

In-Situ Planetary Chemical Analysis

Both, the search for evidence of life on Mars and the assessment of the Martian environment in respect to its compatibility with human explorers, will require the ability to measure and understand the aqueous chemistry of the Martian regolith. Direct in-situ chemical analysis is the only method by which chemical biosignatures can be reliably recognized and the toxicity of the regolith accurately assessed. Qualitative and quantitative determination of the aqueous ionic constituents and their concentrations is critical in developing kinetic and thermodynamic models that can be used to accurately predict the potential of the past or present Martian geochemical environment to have either generated or still sustain life. In-situ chemical characterization could provide evidence as to whether the chemical composition of the regolith or evaporates in suspected ancient water bodies have been biologically influenced.

Kounaves, S. P.↗
NASA NTRS1994

NASA Ultra-Sensitive Miniature Accelerometer

Using micro-machined silicon technology, an ultra-sensitive miniature acce.,rometer can be constructed which meets the requirements for microgravity experiments in the space environment.Such an accelerometer will have a full scale sensitivity of 1C2 g a resolution of lC8 g, low cross axis sensitivity, and low temperature sensitivity. Mass of the device is approximately five grams and its footprint is 2 cm x 2 cm. Innovative features of the accelerometer, which are patented, are: electrostatic caging to withstand handling shock up to 150 g, in-situ calibration, in situ performance characterization, and both static and dynamic compensation. The transducer operates on a force balance principle wherein the displacement of the proof mass is monitored by measuring tunneling electron current flow between a conductive tip, and a fixed platen. The four major parts of the accelerometer are tip die, incorporating the tunneling tip and four field plates for controlling pitch and roll of the proof mass; two proof mass dies, attached to the surrounding frame by sets of four leg" springs; and a force plate die. The four parts are fuse-bonded into a complete assembly. External electrical connections are made at bond pads on the front surface of the force plate die. Materials and processes used in the construction of the transducer are compatible with volume production.

Zavracky, Paul M.↗
NASA NTRS2007

SEM-EDS Analyses of Small Craters in Stardust Aluminum Foils: Implications for the Wild-2 Dust Distribution

Aluminium foils were used on Stardust to stabilize the aerogel specimens in the modular collector tray. Part of these foils were fully exposed to the flux of cometary grains emanating from Wild 2. Because the exposed part of these foils had to be harvested before extraction of the aerogel, numerous foil strips some 1.7 mm wide and 13 or 33 mm long were generated during Stardusts's Preliminary Examination (PE). These strips are readily accommodated in their entirety in the sample chambers of modern SEMs, thus providing the opportunity to characterize in situ the size distribution and residue composition - employing EDS methods - of statistically more significant numbers of cometary dust particles compared to aerogel, the latter mandating extensive sample preparation. We describe here the analysis of nearly 300 impact craters and their implications for Wild 2 dust.

Borg, J.↗
NASA NTRS2011

NASA Tech Briefs, December 2011

Topics covered include: 1) SNE Industrial Fieldbus Interface; 2) Composite Thermal Switch; 3) XMOS XC-2 Development Board for Mechanical Control and Data Collection; 4) Receiver Gain Modulation Circuit; 5) NEXUS Scalable and Distributed Next-Generation Avionics Bus for Space Missions; 6) Digital Interface Board to Control Phase and Amplitude of Four Channels; 7) CoNNeCT Baseband Processor Module; 8) Cryogenic 160-GHz MMIC Heterodyne Receiver Module; 9) Ka-Band, Multi-Gigabit-Per-Second Transceiver; 10) All-Solid-State 2.45-to-2.78-THz Source; 11) Onboard Interferometric SAR Processor for the Ka-Band Radar Interferometer (KaRIn); 12) Space Environments Testbed; 13) High-Performance 3D Articulated Robot Display; 14) Athena; 15) In Situ Surface Characterization; 16) Ndarts; 17) Cryo-Etched Black Silicon for Use as Optical Black; 18) Advanced CO2 Removal and Reduction System; 19) Correcting Thermal Deformations in an Active Composite Reflector; 20) Umbilical Deployment Device; 21) Space Mirror Alignment System; 22) Thermionic Power Cell To Harness Heat Energies for Geothermal Applications; 23) Graph Theory Roots of Spatial Operators for Kinematics and Dynamics; 24) Spacesuit Soft Upper Torso Sizing Systems; 25) Radiation Protection Using Single-Wall Carbon Nanotube Derivatives; 26) PMA-PhyloChip DNA Microarray to Elucidate Viable Microbial Community Structure; 27) Lidar Luminance Quantizer; 28) Distributed Capacitive Sensor for Sample Mass Measurement; 29) Base Flow Model Validation; 30) Minimum Landing Error Powered-Descent Guidance for Planetary Missions; 31) Framework for Integrating Science Data Processing Algorithms Into Process Control Systems; 32) Time Synchronization and Distribution Mechanisms for Space Networks; 33) Local Estimators for Spacecraft Formation Flying; 34) Software-Defined Radio for Space-to-Space Communications; 35) Reflective Occultation Mask for Evaluation of Occulter Designs for Planet Finding; and 36) Molecular Adsorber Coating

Source record↗
NASA NTRS2014

GeoLab: A Geological Workstation for Future Missions

The GeoLab glovebox was, until November 2012, fully integrated into NASA's Deep Space Habitat (DSH) Analog Testbed. The conceptual design for GeoLab came from several sources, including current research instruments (Microgravity Science Glovebox) used on the International Space Station, existing Astromaterials Curation Laboratory hardware and clean room procedures, and mission scenarios developed for earlier programs. GeoLab allowed NASA scientists to test science operations related to contained sample examination during simulated exploration missions. The team demonstrated science operations that enhance theThe GeoLab glovebox was, until November 2012, fully integrated into NASA's Deep Space Habitat (DSH) Analog Testbed. The conceptual design for GeoLab came from several sources, including current research instruments (Microgravity Science Glovebox) used on the International Space Station, existing Astromaterials Curation Laboratory hardware and clean room procedures, and mission scenarios developed for earlier programs. GeoLab allowed NASA scientists to test science operations related to contained sample examination during simulated exploration missions. The team demonstrated science operations that enhance the early scientific returns from future missions and ensure that the best samples are selected for Earth return. The facility was also designed to foster the development of instrument technology. Since 2009, when GeoLab design and construction began, the GeoLab team [a group of scientists from the Astromaterials Acquisition and Curation Office within the Astromaterials Research and Exploration Science (ARES) Directorate at JSC] has progressively developed and reconfigured the GeoLab hardware and software interfaces and developed test objectives, which were to 1) determine requirements and strategies for sample handling and prioritization for geological operations on other planetary surfaces, 2) assess the scientific contribution of selective in-situ sample characterization for mission planning, operations, and sample prioritization, 3) evaluate analytical instruments and tools for providing efficient and meaningful data in advance of sample return and 4) identify science operations that leverage human presence with robotic tools. In the first year of tests (2010), GeoLab examined basic glovebox operations performed by one and two crewmembers and science operations performed by a remote science team. The 2010 tests also examined the efficacy of basic sample characterization [descriptions, microscopic imagery, X-ray fluorescence (XRF) analyses] and feedback to the science team. In year 2 (2011), the GeoLab team tested enhanced software and interfaces for the crew and science team (including Web-based and mobile device displays) and demonstrated laboratory configurability with a new diagnostic instrument (the Multispectral Microscopic Imager from the JPL and Arizona State University). In year 3 (2012), the GeoLab team installed and tested a robotic sample manipulator and evaluated robotic-human interfaces for science operations.

Evans, Cynthia↗
NASA NTRS2013

In-Situ Transfer Standard and Coincident-View Intercomparisons for Sensor Cross-Calibration

There exist numerous methods for accomplishing on-orbit calibration. Methods include the reflectance-based approach relying on measurements of surface and atmospheric properties at the time of a sensor overpass as well as invariant scene approaches relying on knowledge of the temporal characteristics of the site. The current work examines typical cross-calibration methods and discusses the expected uncertainties of the methods. Data from the Advanced Land Imager (ALI), Advanced Spaceborne Thermal Emission and Reflection and Radiometer (ASTER), Enhanced Thematic Mapper Plus (ETM+), Moderate Resolution Imaging Spectroradiometer (MODIS), and Thematic Mapper (TM) are used to demonstrate the limits of relative sensor-to-sensor calibration as applied to current sensors while Landsat-5 TM and Landsat-7 ETM+ are used to evaluate the limits of in situ site characterizations for SI-traceable cross calibration. The current work examines the difficulties in trending of results from cross-calibration approaches taking into account sampling issues, site-to-site variability, and accuracy of the method. Special attention is given to the differences caused in the cross-comparison of sensors in radiance space as opposed to reflectance space. The results show that cross calibrations with absolute uncertainties lesser than 1.5 percent (1 sigma) are currently achievable even for sensors without coincident views.

Advanced Spaceborne Thermal Emission and Reflectio↗
NASA NTRS2016

Pre-Mission Input Requirements to Enable Successful Sample Collection by A Remote Field/EVA Team

The FINESSE (Field Investigations to Enable Solar System Science and Exploration) team, part of the Solar System Exploration Virtual Institute (SSERVI), is a field-based research program aimed at generating strategic knowledge in preparation for human and robotic exploration of the Moon, near-Earth asteroids, Phobos and Deimos, and beyond. In contract to other technology-driven NASA analog studies, The FINESSE WCIS activity is science-focused and, moreover, is sampling-focused with the explicit intent to return the best samples for geochronology studies in the laboratory. We used the FINESSE field excursion to the West Clearwater Lake Impact structure (WCIS) as an opportunity to test factors related to sampling decisions. We examined the in situ sample characterization and real-time decision-making process of the astronauts, with a guiding hypothesis that pre-mission training that included detailed background information on the analytical fate of a sample would better enable future astronauts to select samples that would best meet science requirements. We conducted three tests of this hypothesis over several days in the field. Our investigation was designed to document processes, tools and procedures for crew sampling of planetary targets. This was not meant to be a blind, controlled test of crew efficacy, but rather an effort to explicitly recognize the relevant variables that enter into sampling protocol and to be able to develop recommendations for crew and backroom training in future endeavors.

FINESSE↗
NASA NTRS2016

The Miniaturized Moessbauer Spectrometer MIMOS II for the Asteroid Redirect Mission(ARM): Quantative Iron Mineralogy And Oxidation States

The miniaturized Moessbauer spectrometer MIMOS II is an off‐the‐shelf instrument with proven flight heritage. It has been successfully deployed during NASA’s Mars Exploration Rover (MER) mission and was on‐board the UK‐led Beagle 2 Mars lander and the Russian Phobos‐Grunt sample return mission. A Moessbauer spectrometer has been suggested for ASTEX, a DLR Near-Earth Asteroid (NEA) mission study, and the potential payload to be hosted by the Asteroid Redirect Mission (ARM). Here we make the case for in situ asteroid characterization with Moessbauer spectroscopy on the ARM employing one of three available fully-qualified flight-spare Moessbauer instruments.

Schroeder, C.↗
NASA NTRS2016

The Miniaturized Mossbauer Spectrometer MIMOS II for the Asteroid Redirect Mission (ARM): Quantitative Iron Mineralogy and Oxidation States

The miniaturized Mossbauer spectrometer MIMOS II is an off-the-shelf instrument, which has been successfully deployed during NASA's Mars Exploration Rover (MER) mission and was on-board the ESA/UK Beagle 2 Mars lander and the Russian Phobos-Grunt sample return mission. We propose to use a fully-qualified flight-spare MIMOS II instrument available from these missions for in situ asteroid characterization with the Asteroid Redirect Robotic Mission (ARRM).

Schroder, Christian↗