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All sourcesNASA NTRSDOE OSTI
NASA NTRS2019

Durability Characterization of Mechanical Interfaces in Solar Sail Membrane Structures

The construction of a solar sail from commercially available metallized film presents several challenges. The solar sail membrane is made by seaming together strips of metallized polymer film. This requires seaming together a preselected width and thickness of a base material into the required geometry, and folding the assembled sail membranes into a small stowage volume prior to launch. The sail membranes must have additional features for connecting to rigid structural elements (e.g., sail booms) and must be electrically grounded to the spacecraft bus to prevent charge build up. Space durability of the material and mechanical interfaces of the sail membrane assemblies will be critical for the success of any solar sail mission. In this study, interfaces of polymer/metal joints in a representative solar sail membrane assembly were tested to ensure that the adhesive interfaces and the fastening grommets could withstand the temperature range and expected loads required for mission success. Various adhesion methods, such as surface treatment, commercial adhesives, and fastening systems, were experimentally evaluated and will be discussed.

Interface↗
NASA NTRS2021

Sample Return Containerization and Planetary Protection Using Brazing for Breaking the Chain of Contact to Mars

Planetary protection of Mars samples returned to Earth in a future NASA mission is a critical part of preventing uncontrolled biological materials being released from the samples. The planetary protection process requires addressing the potential risks and would involve “breaking the chain of contact (BTC)”, where any returned material reaching Earth for further analysis would have to be sealed inside a container with extremely high confidence. The sterilization process would require destroying any potential biological materials that may contaminate the external surface of the container. A novel process for containing the returned samples has been conceived and developed at JPL. The process consists of using induction heated brazing to synchronously sterilize, separate, seam and seal the container. In this case. the braze material is heated to the level of melting at temperatures higher than 500°C to assure sterilizing exposed areas since carbon bonds are broken above this temperature. The container that encloses the samples consists of double walls with interstitial space that is Earth-clean. The process consists of two-steps, where one was intended to be prepared on Earth and the second potentially executed on orbit around Mars. The latest results of this study that established the needed capability are described and discussed in this manuscript.

Shirajian, Nareg↗
DOE OSTI2020

Surface and bulk characterization of reservoir and cap-rocks: Past, present, and future

Geologic formations provide potentially some of the largest volume capacities for CO 2 storage or sequestration. Potential storage sites can be deep saline aquifers, depleted oil reservoirs, and coal seams, surrounded by sealing layers to prevent CO 2 from leaking. It is therefore critical to understand mechanisms contributing to CO 2 trapping and CO 2 leaks. Both phenomena are governed by reactions at the interfaces of the reservoir and cap-rocks and are controlled by the complex chemistry and pore structures of rocks. Mechanisms at the macroscale are affected by the processes occurring at the nanoscale. This review highlights the necessity of multitechnique, multiscale characterization of rocks and points to the importance of surface analysis and surface science studies. Two shale rocks (seals) from Niobrara and Agardhfjellet formations with complex surface chemistry are used as examples throughout the paper. Typically, evaluation of rocks with x-ray diffraction, thermogravimetric analysis, Rock-Eval pyrolysis, gas adsorption, and electron microscopy combined with energy dispersive x-ray spectroscopy is conducted to provide valuable information about the bulk mineralogy, elemental composition, pore volume, and adsorbed species on the sample surface. These studies are necessary prior to designing surface sensitive experiments with x-ray photoelectron spectroscopy (XPS), guiding both sample preparation and sample analysis. XPS has been widely used to study the surface composition of rocks during the investigations of their fine-scale wettability, and the main findings are highlighted here. This paper also reviews the existing literature on ambient-pressure XPS, which provides new opportunities to study in situ chemical alteration due to interactions with CO 2 and offers recommendations for adapting this technique to study rock-fluid interactions, allowing for the identification of fundamental interactions during CO 2 sequestration and guide selection of formation sites for improved storage.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRSDate not supplied

Status of the 3-MDCP, the 3-D Woven TPS enabling MSR Earth Entry System Development

While the HEEET project established the dual-layer, 3-D Woven TPS at TRL 6 for extreme entry environment missions such as Saturn and Ice-Giant Probe missions, subsequent to the completion of HEEET project in 2018, further development was undertaken to assess the viability of a variant of the 3-D Woven, a single, insulating layer alone as a viable TPS for Mars Sample Return mission. MSR Earth Entry System (EES) baselined it and named the TPS as 3D, mid-density, carbon-phenolic (3MDCP). MSR program invested in building a new loom and the weaver T.E.A.M. Inc is currently weaving 80” wide 1.2” thick insulating layer. Unlike HEEET, where a set of tiles and seams are integrated to form the heat-shield, 3MDCP is a seamless heatshield by wrapping and shaping a flat panel into the heatshield shape and then rigidizing the preform through resin infusion. MSR EES is investing in technology maturation of 3MDCP for the current mission launch in 2027. This lighting talk will provide key developments and time line for 3MDCP technology maturation to show that 3MDCP will be ready to support future UOP or Saturn Probe mission. In addition, the limitations of the capability will be presented so that Saturn mission proposers as well as UOP flagship mission study can be fully informed as to the 3MDCP capability.

HEEET↗
DOE OSTI2022

Permutation invariant polynomial neural network based diabatic ansatz for the ( E + A ) × ( e + a ) Jahn–Teller and Pseudo-Jahn–Teller systems

In this work, the permutation invariant polynomial neural network (PIP-NN) approach is employed to construct a quasi-diabatic Hamiltonian for system with non-Abelian symmetries. It provides a flexible and compact NN-based diabatic ansatz from the related approach of Williams, Eisfeld, and co-workers. The example of $H^3_+$ is studied, which is an (E + A) × (e + a) Jahn–Teller and Pseudo-Jahn–Teller system. The PIP-NN diabatic ansatz is based on the symmetric polynomial expansion of Viel and Eisfeld, the coefficients of which are expressed with neural network functions that take permutation-invariant polynomials as input. This PIP-NN-based diabatic ansatz not only preserves the correct symmetry but also provides functional flexibility to accurately reproduce ab initio electronic structure data, thus resulting in excellent fits. Further, the adiabatic energies, energy gradients, and derivative couplings are well reproduced. A good description of the local topology of the conical intersection seam is also achieved. Therefore, this diabatic ansatz completes the PIP-NN based representation of DPEM with correct symmetries and will enable us to diabatize even more complicated systems with complex symmetries.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1995

Development of LaRC (TM): IA thermoplastic polyimide coated aerospace wiring

NASA Langley has invented LaRC(exp TM) IA and IAX which are thermoplastic polyimides with good melting, thermal and chemical resistance properties. It was the objective of this contract to prepare and extrude LaRC (exp TM) polyimide onto aircraft wire and evaluate the polymers performance in this critical application. Based on rheology and chemical resistance studies at Imitec, LaRC (exp TM) IAX melts readily in an extruder, facilitating the manufacture of thin wall coatings. The polyimide does not corode the extruder, develop gel particles nor advance in viscosity. The insulated wire was tested according to MiL-W-22759E test specifications. The resulting wire coated with LaRC (exp TM) IAX displayed exceptional properties: surface resistance, non blocking, non burning, hot fluid resistance, impulse dielectric, insulation resistance, low temperature flexibility, thermal aging, wire weight, dimensions, negligible high temperature shrinkage and stripability. The light weight and other properties merit its application in satellites, missiles and aircraft applications. The extruded IAX results in a polyimide aircraft insulation without seams, outstanding moisture resistance, continuous lengths and abrasion resistance.

Keating, Jack↗
NASA NTRS2018

Mechanisms of Oxide Formation in the Self-Reacting Friction Stir Weld Process

The initial objective of this study was to evaluate the effect of an extended delay time between preweld cleaning and the completion of a self-reacting friction stir welding (SRFSW) process on the resulting quality of various thickness panels of AA2219-T87. The current NASA standard specifies no more than a 48 hour delay between preweld cleaning and actual welding. The concern is whether increasing the cleaning delay time results in development of the residual oxide defect (ROD) in SRFSW. This concern emanates from the possibility of increased time correlating with increased oxide layer thickness on the faying surfaces. Oxide content on the faying surfaces has been reported to correlate with the occurrence of the ROD which reduces mechanical properties. When the SRFSW process was first adopted by the NASA Marshall Space Flight Center (MSFC), unexpected low tensile values that resulted were attributed to oxides within the weld that appeared to follow the former faying surface contours. Mitigation of the ROD was achieved through a combination of modifications to the processing parameters, tool designs, and incorporation of a weld seam offset. Two operations are involved in preweld cleaning: the first is removal of oil and grease, and the second is removal of surface oxides. In arc welding, improper cleaning of the faying surfaces of aluminum welded joints can increase the sensitivity toward development of defects. As the aluminum is locally melted, these contaminants contribute toward the development of porosity, inclusions, entrapped oxides, and other discontinuities which can degrade the strength of the weld joint. For weldment of large structures, the weld joint is typically cleaned, fit-up, and tack welded prior to the final full penetration welding pass. Because of the stringent joint fit-up requirements for mismatch and peaking for launch vehicle structures, the joint fit-up can sometimes contribute to lengthy delays between cleaning and tack welding, especially for circumferential weld joints on large diameter components. When the conventional friction stir welding (CFSW) process was introduced at the NASA MSFC, there was no procedure for cleaning prior to the solid-state joining process. As the process expanded to include SRFSW, preparation of the faying, crown, and root surfaces were implemented to overcome the ROD. Although the solid-state process is not expected to reach temperatures high enough for dissociation of the native oxide layer, concern remained regarding the redeposition of the native oxide layer within the stir zone. NASA has previously established the allowable time at 48 hours between preweld cleaning and a SRFSW process. The effect of potential 2 contamination resulting from an extended delay to 188 hours was subsequently evaluated for SRFSWs using tensile testing and metallographic imaging. Tensile specimens were tested at room temperature (RT), and at cryogenic conditions of liquid nitrogen (LN2) and liquid hydrogen. No detrimental effect on weld quality, as determined by weld strength, was reported for cleaning delays of 48, 120, 168, 240 or 288 hours. While no trends were established in this study, which extended the delay from 48 to 188 hours, there were a few outliers in terms of ultimate tensile strength (UTS). According to M. Fisher's 2014 Boeing Company Memo no. EYBF-MAF-14-029, all outliers were above the minimum acceptance criteria, but out of family with respect to the average values. As the robustness and reliability of any process ultimately depends on the average values as well as the outliers, an understanding of the cause of these outliers will ultimately improve the process. This report examines those outliers and their possible causes.

Schneider, J. A.↗
NASA NTRS2011

NASA's Integrated Instrument Simulator Suite for Atmospheric Remote Sensing from Spaceborne Platforms (ISSARS) and Its Role for the ACE and GPM Missions

Forward simulation is an indispensable tool for evaluation of precipitation retrieval algorithms as well as for studying snow/ice microphysics and their radiative properties. The main challenge of the implementation arises due to the size of the problem domain. To overcome this hurdle, assumptions need to be made to simplify compiles cloud microphysics. It is important that these assumptions are applied consistently throughout the simulation process. ISSARS addresses this issue by providing a computationally efficient and modular framework that can integrate currently existing models and is also capable of expanding for future development. ISSARS is designed to accommodate the simulation needs of the Aerosol/Clouds/Ecosystems (ACE) mission and the Global Precipitation Measurement (GPM) mission: radars, microwave radiometers, and optical instruments such as lidars and polarimeter. ISSARS's computation is performed in three stages: input reconditioning (IRM), electromagnetic properties (scattering/emission/absorption) calculation (SEAM), and instrument simulation (ISM). The computation is implemented as a web service while its configuration can be accessed through a web-based interface.

real-aperture instruments↗
NASA NTRS2012

The Evolution of Friction Stir Welding Theory at Marshall Space Flight Center

From 1995 to the present the friction stir welding (FSW) process has been under study at Marshall Space Flight Center (MSFC). This is an account of the progressive emergence of a set of conceptual tools beginning with the discovery of the shear surface, wiping metal transfer, and the invention of a kinematic model and making possible a treatment of both metallurgical structure formation and process dynamics in friction stir welding from a unified point of view. It is generally observed that the bulk of the deformation of weld metal around the FSW pin takes place in a very narrow, almost discontinuous zone with high deformation rates characteristic of metal cutting. By 1999 it was realized that this zone could be treated as a shear surface like that in simple metal cutting models. At the shear surface the seam is drawn out and compressed and pressure and flow conditions determine whether or not a sound weld is produced. The discovery of the shear surface was followed by the synthesis of a simple 3- flow kinematic model of the FSW process. Relative to the tool the flow components are: (1) an approaching translational flow at weld speed V, (2) a rotating cylindrical plug flow with the angular velocity of the tool , and (3) a relatively slow ring vortex flow (like a smoke ring) encircling the tool and driven by shoulder scrolls and pin threads. The rotating plug flow picks up an element of weld metal, rotates it around with the tool, and deposits it behind the tool ( wiping metal transfer ); it forms plan section loops in tracers cut through by the tool. Radially inward flow from the ring vortex component retains metal longer in the rotating plug and outward flow expels metal earlier; this interaction forms the looping weld seam trace and the tongue and groove bimetallic weld contour. The radial components of the translational and ring vortex flows introduce parent metal intrusions into the small grained nugget material close to the tool shoulder; if this feature is pronounced, nugget collapse may result. Certain weld features, in particular internal banding seen in transverse section as onion rings and associated surface ridges called tool marks , have long implied an oscillation flow component, but have only recently been attributed in the literature to tool eccentricity. Rotating plug shape, typically a hollow cylinder flared at the end where it sticks to the shoulder, varies as pressure distribution on the tool determines where sticking occurs. Simplified power input estimates balanced against heat loss estimates give reasonable temperature estimates, explain why the power requirement changes hardly at all over a wide range of RPM s, and yield isotherms that seem to fall along boundaries of parameter windows of operation.

Nunes, Arthur C.↗
NASA NTRSDate not supplied

Sustaining Thermal Protection Systems Needed for Uranus Probes

Summary: Achieving Uranus in-situ science objectives through deploying probes in the atmosphere requires thermal protection systems capable of withstanding extreme entry environments. NASA’s 3-D Woven based thermal protection systems (TPS), developed specifically to meet this challenge, are mature, efficient, and capable of withstanding such entry. These science-enabling capabilities need to be sustained, otherwise mission implementation risk may increase to the point that the mission is untenable. The heatshield technology has been developed in concert with industry, and manufacturing processes have been technology transferred. Current technology readiness does not guarantee future availability. Sustainment requires maintaining expertise within NASA as well as ensuring that proven industrial expertise and capabilities will be readily available in the future. A constant awareness and risk assessment followed by risk mitigation are required. The scientific community needs to be aware of these challenges. It needs to engage NASA to ensure these capabilities will be available when needed. As was the case with the atrophy of heritage carbon phenolic that led to developing the 3-D Woven capabilities, our vigilance is again needed to sustain these enabling TPS capabilities for Uranus and for other missions. Background: NASA invested in and developed Heatshield for Extreme Entry Environment Technology (HEEET) TPS that was matured to TRL 6 in 2019 as a tiled system with seams and gap-fillers. Manufacturing readiness included development of specialized looms, molding, and infusion processes using commercial partners. In support of the Mars Sample Return mission, a single-layer, seamless, single-piece variant referred to as 3MDCP (3-D woven Mid-Density Carbon-Phenolic) was developed and is limited to a 1.3m maximum diameter scale due to weaving width limitations of 80”. Molding techniques developed to transform a flat, 2”-thick 3-D woven preform into a sphere-cone shape prior to phenolic resin infusion has been demonstrated. A team at NASA Ames is currently working with industry to demonstrate infusion at full-scale. By 2026, 3MDCP will be at a high level of maturity in technical, manufacturing, and integration readiness as well as material characterization. HEEET and 3MDCP for Uranus Entry: Several system studies have evaluated and baselined 3-D Woven TPS for Uranus entry, both HEEET as well as 3MDCP. If the aeroshell carrying the descent probe is 1.3m or less, then 3MDCP is a very capable and the most mass-efficient choice. If the aeroshell is bigger than 1.3m diameter, then HEEET can meet the mission need as it allows for an aeroshell of any diameter. HEEET and 3MDCP are capable of Saturn in-situ science missions prioritized in the New Frontiers-5 draft Announcement of Opportunity (AO) and if Saturn is the mission of choice, there is a pathway for sustaining the capability. Capability Sustainment: Given NASA’s current budgetary constraints, the postponement of the next New Frontiers AO to no earlier than 2026 and the unknown delay in starting the UOP flagship effort point to potential gap years for the HEEET and 3MDCP capabilities. The first step in capability sustainment is to understand the risks as they emerge, assess those risks, and develop plans to mitigate them. Keeping the science community, who are interested in UOP as well as the larger Giant Planet missions, informed of the emerging challenges requires continuous risk assessment/mitigation. Without these steps, atrophy is more likely within the industrial partners with which NASA has partnered. This presentation will provide more details as well as steps NASA can take to minimize the impact to the UOP mission.

Ethiraj Venkatapathy↗
DOE OSTI2026

Utilization of Unmanned Aircraft Systems for Environmental Purposes at the Savannah River Site – 26578

Born in the 1950s, the Savannah River Plant was constructed as a plutonium and tritium production plant. As the Cold War era came and went, a change of direction was signaled when the name of the facility changed from Savannah River Plant to Savannah River Site (1989) – the main mission at Savannah River shifted from “production” to “cleanup.” The Department of Energy is responsible for managing the 310 square miles of land that is the Savannah River Site and the cleanup/remediation activities that occur. The Savannah River National Laboratory utilizes unmanned aircraft systems to assist with some of those environmental monitoring and remediation activities. One function of unmanned aircraft systems at the Savannah River National Laboratory is conducting aerial photography and videography. Various infrastructure evaluations have been performed with unmanned aircraft – facility rooftop inspections, water tower lock verifications, earthen dam surveys, etc. An unmanned aircraft system has been used for progress footage of remediation projects – Dunbarton Bay remediation, Saltstone Disposal Unit construction, etc. Thermal cameras on an unmanned aircraft system are used to help identify cracks/leaks in structures from vantage points not readily accessible by personnel. Virtual tours of different waste units are conducted with unmanned aircraft systems for Site groups and federal/state regulators to save costs and travel time. Additionally, advanced remote sensing technologies are used on unmanned aircraft systems at the Savannah River Site. Light Detection and Ranging uses laser pulses to measure distances to the Earth's surface or other targets to create highly detailed topographic maps that accurately portray terrain (e.g., elevation changes, slopes, and contours). Data collection with a Light Detection and Ranging unit mounted on an unmanned aircraft system is quick and efficient – large-area surveys are conducted in shorter time frames. Because Light Detection and Ranging can penetrate through foliage and vegetation to ground level, it is being used in conjunction with a watershed model to study the General Separations Area of the Site to determine stormwater flow volume and direction, monitor stream stability, and forecast river flow behavior. A hyperspectral camera captures a wide spectrum of electromagnetic wavelengths across numerous narrow bands, beyond what the human eye can see. It provides detailed spectral information about the objects or surfaces in an image, which can be used to identify and analyze materials based on their spectral signatures. A hyperspectral camera mounted on an unmanned aircraft system has been used at the Savannah River Site for non-destructive evaluation of concrete and concrete structures. Unmanned aircraft systems at the Savannah River Site are also used for the application of herbicide on identified rooftops. P-Reactor and R-Reactor are entombed nuclear reactors at the Savannah River Site. Unwanted vegetation is often present on these rooftops – over time roots can penetrate seams, cracks, and joints of the general roof and concrete caps, leading to water ingress and deterioration of the structural components. For time and cost efficiencies as well as in the interest of personnel safety, an unmanned aircraft is used to dispense herbicide on rooftop areas where vegetation is noticed to help alleviate the issues/hazards.

Lorier, Troy [Savannah River National Laboratory (↗
DOE OSTI2026

Cybersecurity Workforce Training for SMR Integration into Distribution Grids: A Competency Framework and Containerized Hands-On Lab for the SMR/DER/Microgrid Boundary

Small modular reactors (SMRs) and microreactors are entering the U.S. distribution grid as synchronous generation on feeders designed for loads and inverter-based distributed energy resources (DERs). No existing cybersecurity training program addresses this intersection of nuclear operations, DER management, and operational technology security. As subcontractor to Iowa State University on the CyDERMS Center, Argonne analyzed the relevant standards and training landscape, translated the resulting gaps into a twelve-objective competency framework across distribution-operator and graduate-analyst role tracks, and built a containerized training lab using a ∼400-bus composite grid model behind a realistically simulated Modbus TCP SCADA stack. The analysis isolates the balance-of-plant / energy-management-system (BOP/EMS) boundary as the critical jurisdictional seam where, as of March 2026, neither NRC nor NERC CIP cleanly claims cybersecurity responsibility for distribution-connected SMRs. The framework maps each objective across NIST CSF 2.0, ISA/IEC 62443, NIST NICE Task–Knowledge–Skill statements, and NRC RG 5.71 awareness-and-training controls. The training lab implements operator-recognition assessment scenarios spanning grid-side disturbances and telemetry-layer anomalies.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
NASA NTRS1998

Large Scale Testing of a Foam/Multilayer Insulation Thermal Control System (TCS) for Cryogenic Upper Stages

The development of high energy cryogenic upper stages is essential for the efficient delivery of large payloads to various destinations envisioned in future programs. A key element in such upper stages is cryogenic fluid management (CFM) advanced development/technology. Due to the cost of and limited opportunities for orbital experiments, ground testing must be employed to the fullest extent possible. Therefore, a system level test bed termed the Multipurpose Hydrogen Test Bed (MHTB), which is representative in size and shape (3 meter diameter by 3 meter long with a volume of 18 cubic meters) of a fully integrated space transportation vehicle liquid hydrogen propellant tank has been established. To date, upper stage studies have often baselined the foam/multilayer insulation (FMLI) combination concept; however, hardware experience with the concept is minimal and was therefore selected for the MHTB. The foam element (isofoam SS-1 171 with an average thickness of 3.5 centimeters) is designed to protect against ground hold/ascent flight environments, and allows for the use of a dry nitrogen purge as opposed to the more complex/heavy helium purge subsystem normally required with MLI in cryogenic applications. The MLI (45 layers of Double Aluminized Mylar with Dacron spacers) provides protection in the vacuum environment of space and is designed for an on-orbit storage period of 45 days. Several unique features were incorporated in the MLI concept and included: variable density MLI (reduces weight and radiation losses by changing the layer density), larger but fewer DAM perforations for venting during ascent to orbit (reduces radiation losses), and roll wrap installation of the MLI with a commercially established process to lower assembly man-hours and reduce seam heat leak. Thermal performance testing of the MHTB TCS was conducted during three test series conducted between September 1995 and May 1996. Results for the ground hold portion of the tests were as expected producing an average heat leak of 63 WattS/M2 at an average foam surface temperature of 170 K. The results of the simulated orbit hold test interval produced heat leaks ranging from 0.085 to 0.22 Watts/squareM at warm boundary temperatures of 164K and 305K, respectively. When compared to the performance for a traditional MLI system, a 60% reduction in orbital heat leak or boiloff was measured. Overall, the MHTB TCS demonstrated satisfactory performance for all mission phases required of a cryogenic upper stage.

Hastings, Leon↗
DOE OSTI2021

Interferometric SAR modelling of near surface data to improve geological model in the Surat Basin, Australia

Here we present a study on geophysical inverse modelling for subsurface structural properties of an unconventional hydrocarbon site that was monitored previously by Interferometric Synthetic Aperture Radar (InSAR) technology for surface deformation. A static three-dimensional geomodel along with extracted property maps replicates the depth of each underlying stratigraphic unit and structural feature with the density of each geological layer. We examine the hypothesis that integration of elastic properties of each formation layer with InSAR observations in a stratified elastic medium will lead to a viscoelastic geophysical inverse problem that can be solved to estimate fractional volume change at the reservoir level. Moreover, we examine synthetic scenarios in which the elastic properties of the formations are perturbed before determining the resulting impact on the rate of surface deformation. The results show that although the slope of underlying formations, their density and depth can define the extent and pattern of a deformation signal, their properties have a marginal impact on volumetric change compared to the dense network of shallow depth Coal Seam Gas (CSG) mining wells. Besides, it is also demonstrated that the inversion of InSAR deformation maps can resolve the uncertainties associated with low-resolution seismic interpretation as well as filling the data gaps within seismic acquisitions. A significant contribution of this investigation to the geological basin modelling involves a) introducing a remote and non-invasive technology such as InSAR to improve geophysical mapping of subsurface structures such as faults in areas with sparse or no reflective seismic information, and b) applying a multi-layer viscoelastic geophysical source model for an unconventional hydrocarbon reservoir such as CSG.

58 GEOSCIENCES↗
NASA NTRS2017

Synchronous Separation, Seaming, Sealing and Sterilization (S4) using Brazing for Sample Containerization and Planetary Protection

The potential return of samples back to Earth from other planetary bodies would be based on planetary protection requirements that vary depending on the type of body [1]. Potential Mars Sample Return would require the protection of our planet from backward contamination. To fulfill this requirement, it would be necessary to implement “break the chain of contact (BTC)” process, where any material reaching Earth would have to be inside a container that is sealed with an extremely high level of confidence. In order to accomplish this, it would be necessary to contain the acquired samples and destroy any potential biological materials that may have contaminated the external surface of the container, while protecting the samples for further analysis. Using brazing, a novel synchronous separation, seaming, sealing and sterilization (S4) process for sample containerization and planetary protection has been conceived and demonstrated. A prototype double-wall container with inner and outer shells and Earth clean interstitial space was used for this demonstration. For potential Mars sample return, the double wall container would be consist of two halves and prepared on Earth. The on-orbit execution would consist of inserting the sample into one of the halves and then mating to the other half and melt the braze material to perform the S4 process. The use of brazing material that melts at temperatures higher than 500OC would assure sterilization of the exposed areas due to pyrolysis since carbon bonds are broken at this temperature. The process consists of two-steps, Step-1: the double wall container halves are fabricated and brazed on Earth; and Step-2: Assembly and brazing the samples on orbit. To prevent potential jamming during the process of mating the two halves of the double-wall container and the extraction of the brazed inner container, a double cone-within-cone approach has been conceived. The results of this study are described and discussed in this manuscript.

Bar-Cohen, Yoseph↗
DOE OSTI2023

AN ACID BAKING APPROACH TO ENHANCE RARE EARTH ELEMENT RECOVERY FROM BITUMINOUS COAL SOURCES

Rare earth elements (REE) are a group of 17 elements typically classified as light and heavy rare earth elements, which play a crucial role in developing the latest technologies for energy, defense, and medical sectors. Even though REEs have been found in more than 200 minerals, only bastnaesite, monazite and xenotime are commercially exploited for REE extraction. However, the recent exponential increase in REE demand has spurred countries such as the United States into research for the extraction of REEs from secondary sources such as coal, acid mine drainage, and coal ash. Several coal sources (e.g., Fire Clay seam coal) across the United States have been identified to contain elevated concentrations of rare earth elements (>600 ppm), and various researchers have investigated the feasibility of both physical and hydrometallurgical extraction techniques for rare earth concentration and subsequent extraction. However, both physical and direct leaching were concluded to be inefficient for RE beneficiation and extraction due to low recoveries. Alternatively, thermal treatment provides promising means for RE recovery from bituminous coal sources. The positive impact of thermal treatment/calcination was established to be due to the decarbonization and dehydroxylation of the clays, which released entrapped rare earth elements within the dominant minerals and converted them into an acid-soluble form. Nonetheless, the improvement in recovery was limited to the light REEs (LREEs) with an insignificant increase in the heavy REEs (HREE). It was demonstrated that the light and heavy REEs in the material were associated with difficult-to-leach minerals such as monazite, xenotime, and zircon, which were not decomposed by simple calcination due to their high thermal stability. Hence, roasting in the presence of chemicals was necessary to ensure the decomposition of those REE-containing minerals. As such, this study was focused on the acid baking treatment of bituminous coals with an aim to enhance REE recovery, especially HREEs. Based on the presence of REE minerals like monazite and xenotime, three pre-leach treatment methods, i.e., 1) roasting, 2) direct acid baking, and 3) acid baking after roasting were investigated. Roasting tests at 600 ⁰C revealed that the recovery of light REEs (LREEs) was enhanced while the recovery of HREEs remained relatively unaffected. LREE and HREE recovery values of 38.3% and 21.3%, respectively, were achieved using a 50 g/L sulfuric acid solution at 5% solid concentration and a solution temperature of 75 ⁰C for 2 hours. Comparatively, direct acid baking at 250 °C provided substantial increased LREE and HREE recovery values to approximately 49.4% and 53.0%, respectively, using an equivalent acid dosage. Recoveries were maximized to 77.0% and 79.6% for LREE and HREE, respectively, by roasting followed by acid baking. Similar results were obtained from the treatment of a second bituminous coal source. Due to strong correlations between REE and Al recovery values, tests were performed on kaolinite and illite, which were prominent clay minerals within the source coals. These experiments revealed that the REE recovery improvements were likely a result of dehydroxylation of clays and subsequent release and decomposition of REE-bearing minerals such as monazite, xenotime and zircon. Subsequently, a parametric study was conducted to identify the impact of acid baking parameters on rare earth element recovery. The factors investigated using a three-level statistical experimental program were acid baking time, acid solution concentration, baking temperature, and acid solution-to-solids ratio which were found to significantly impact REE and contaminant element (Al, Fe, and Ca) recovery. An increase in baking temperature up to around 250 ⁰C improved the light and heavy REE recovery values by more than 50 absolute percentage points relative to performances achieved when direct leaching. As aforementioned, acid baking was needed to both decompose the clay minerals and liberate the REE minerals, which allowed access for the acid to solubilize the REEs. Acid concentration of the solution used for acid baking was studied as a means of minimizing the amount of acid needed to achieve a target REE recovery. However, thermo-gravimetric and differential scanning calorimetry analysis (TGA-DSC) of sulfuric acid under oxidizing atmosphere revealed that the addition of water decreased the evaporation temperature, which explains the lower REE recovery values obtained when using acid concentrations less than 100%. Using pure sulfuric acid at an acid-to-solid ratio of 0.8:1 resulted in recovery values of around 70% for both LREEs and HREEs. The decomposition reaction time was relatively quick with 65% of the TREEs recovered within the first 10 minutes. Following the identification of optimum operating conditions through the parametric study, a systematic leaching study was carried out to examine the impact of leaching parameters, such as solid-to-liquid (S/L) ratio, temperature, and time, on REE recovery using acid baking conditions of 1:1 acid to solids ratio at 250 °C for 30 minutes. The solid-to-liquid ratio was varied from 1-20% by weight at 25 °C, 50 °C, and 75 °C solution temperatures. The results indicated that reaction time and solution temperature considerably impacted the recovery of heavy and light REEs. Interestingly, LREE recovery reduced from 68% at 5% S/L to 58% at 20%S/L, whereas HREE recovery of 78% remained unaffected. The decrease in the LREE recovery was determined to be due to La and Ce precipitation, likely through isomorphic substitution with calcium in gypsum. The kinetic data indicated that 67% LREE and 77% HREE recovery could be obtained within the first 15 minutes of the reaction, suggesting fast reaction kinetics. Furthermore, raising the solution temperature from 25 °C to 75 °C increased the LREE and HREE recovery from 60% and 32% to 67% and 79%, respectively. The kinetic modeling results demonstrated that the rate-limiting step in the LREE dissolution was diffusion and chemical reaction, whereas the HREE extraction was controlled by only chemical reaction. The leaching study concluded that using 20% S/L at 75 °C for 15 minutes maximized LREE and HREE recovery. The lab-scale precipitation study showed that Fe and Al in solution could be removed at pH 4.5 followed by REE precipitation at pH 6.0 using 6 mol/L NaOH. Finally, the bench-scale data was used to develop a process flowsheet for REE recovery from low-grade bituminous coal sources using acid baking. Finally, based on the proposed flowsheet, a concentrated RE-cake obtained through selective precipitation at pH 6.5 was re-leached using HCl at pH 1.5. The resultant leachate was used to identify the impact of various operating parameters on REE recovery and purity with an aim to maximize REE precipitation efficiency while minimizing the oxalic acid dosage. The operating parameters for this investigation were oxalic acid dosage, iron (III) contamination, solution pH and temperature. The resultant model suggested that oxalic acid dosage and reaction pH are the most significant factors for the REE precipitation efficiency, followed by the interaction of oxalic dosage and Fe concentration. Test results indicated that increasing the oxalic acid concentration from 0g/L to 80g/L improved the REE precipitation efficiency from approximately 4.2% to 95.0%. Furthermore, raising the solution pH from 0.5 to 2.5 considerably enhanced the precipitation efficiency from 0.0% to 98.9%. A solution temperature elevation decreased REE recovery, which indicated an exothermic reaction between REEs and oxalate anions. Finally, a high level of Fe contamination adversely impacted REE precipitation efficiency. The speciation analysis revealed that the dominant iron species in the solution system were Fe-(C₂O₄)₃³⁻, Fe-(C₂O₄)²⁻, and Fe-(C₂O₄)⁺, which consumed the majority of the oxalate anions

rare earth elements, acid baking, high-temperature↗
NASA NTRSDate not supplied

Improvements to Stitching Controls for Manufacturing Advanced Stitched Composites

Stitched composites have been extensively studied and have been shown to have benefits over unstitched composites for stiffened structures, including improved damage tolerance, reduced weight, and fewer fasteners. These benefits make stitched composites attractive from a performance perspective, however, the nature of stitching the preforms prior to infusion includes additional manufacturing steps and equipment compared to conventional resin infusion. Stitching of composite material structures at NASA Langley Research Center (LaRC) is performed at the Integrated Structural Assembly of Advanced Composites (ISAAC) facility using control algorithms developed by the lead author. Two deficiencies have been identified in the current control algorithms, and mitigations for these deficiencies were developed within the Hi-Rate Composite Aircraft Manufacturing (HiCAM) project and are presented herein. First, decoupling stitch translation and rotation takes more time for stitching since two robot operation control steps are executed for each stitch. Therefore, a method was developed to determine when to decouple the translation and rotation for stitching, which reduces stitch time by decoupling the operation control steps only when necessary to execute the stitch properly. Second, a correction to the sideslip stitching approach that eliminates a significant portion of the pre- and post-stitching activities was developed. The developed method adjusts the sideslip stitch angle based on the rotations of previous stitches to ensure that the width of the stitching seam remains constant along its length. Constant seam width eliminates observed overlap of the insertion and catcher thread portions for highly curved paths, which maintains the desired uniformity of through-the-thickness architecture along the seam and eliminates the local degradation of properties where the insertion needle is too close to, or crosses, the catcher needle portion of the seam.

stitching↗
DOE OSTI2025

Resolving femtosecond photoinduced energy flow: capture of nonadiabatic reaction pathway topography and wavepacket dynamics from photoexcitation through the conical intersection seam (Final Technical Report)

The dynamics that take place within just tens to hundreds of femtoseconds following the absorption of light by a molecule can play a critical role in how the absorbed energy is directed, allowing it to be used for a specific function or dissipated harmlessly. The form of chemical change that occurs rapidly in these molecules is called a “nonadiabatic electronic transition.” Such transitions are known to mediate energy flow in natural biological systems such as the ultraviolet photoprotection mechanism of DNA and the first step of the human vision response. Understanding how these mechanisms work precisely may help scientists achieve controlled manipulation of solar energy or optical control of a wide range of energy management functions in artificial systems. Experimental methods, however, have not yet allowed a precisely resolved and complete measurement of nonadiabatic electronic transitions. This constitutes a major obstacle to progress in the field. For progress to occur that would inform a wide body of research aiming to efficiently harness the energy of light for practical purposes, it is especially important to benchmark computational models of the molecules undergoing these rapid changes with experimental measurements, in order to learn which models are accurate. With Dept. of Energy funding, we have made strong progress towards establishing a new optical method for experimentally detecting the full nonadiabatic electronic transition. This requires having coordinated pulses of light covering the visible through the mid-infrared range of the electromagnetic spectrum that last only ten femtoseconds. We have developed a new, relatively simple approach for generating such pulses of laser light, and have incorporated them into a time-resolved spectrometer for measuring rapid changes in molecules. These tools can provide the greater precision and new types of data that are needed to benchmark computational models of molecular change and thus to make progress in the field. Our tools were tested on graphene, an excellent solid-state sample for verifying the capabilities and limitations of our instrumentation. The investment made in these tools by the Dept. of Energy Office of Science will allow new fundamental scientific understanding of energy dynamics in molecules in future studies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗