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DOE OSTI2026

Pulsed radio frequency power modulation for profile control in cryogenic reactive ion etching of silicon gratings

Cryogenic silicon etching with SF 6 /O 2 plasmas enables vertical sidewalls and smooth surfaces for high–aspect-ratio structures, yet precise control of etched profiles (sidewall angle, lateral etching, and linewidth retention) remains challenging under continuous-wave excitation due to coupling among radical fluxes, ion energy distributions, and in situ passivation dynamics. In this work, we investigated pulsed radio frequency bias delivery as a process knob for profile control during cryogenic silicon etching. Systematic experiments on 500 nm-wide, 1 μm-pitch gratings etched to 0.8–1.1 μm depth at 0.5–2 kHz pulsing frequency and 25%–75% duty cycle revealed strong dependencies of etch rate, linewidth, and sidewall angle on modulation conditions. We proposed a conceptual kinetic picture combined with feature-scale electrostatic analysis to understand the alternation of ion-driven etching and passivation recovery between on/off segments and local electric field shaping and modulation of ion trajectories within the trench. Moderate duty cycles (50%–75%) near 1 kHz achieved a balance between anisotropy and etch rate. These results demonstrate pulsed-bias modulation can be utilized to tune directionality and sidewall preservation in cryogenic SF 6 /O 2 etching, which are relevant to photonic, metrology, and quantum device fabrication.

36 MATERIALS SCIENCE↗

NASA NTRS2014

Hot Hydrogen Testing of Tungsten-Uranium Dioxide (W-UO2) CERMET Fuel Materials for Nuclear Thermal Propulsion

CERMET fuel materials are being developed at the NASA Marshall Space Flight Center for a Nuclear Cryogenic Propulsion Stage. Recent work has resulted in the development and demonstration of a Compact Fuel Element Environmental Test (CFEET) System that is capable of subjecting depleted uranium fuel material samples to hot hydrogen. A critical obstacle to the development of an NCPS engine is the high-cost and safety concerns associated with developmental testing in nuclear environments. The purpose of this testing capability is to enable low-cost screening of candidate materials, fabrication processes, and further validation of concepts. The CERMET samples consist of depleted uranium dioxide (UO2) fuel particles in a tungsten metal matrix, which has been demonstrated on previous programs to provide improved performance and retention of fission products1. Numerous past programs have utilized hot hydrogen furnace testing to develop and evaluate fuel materials. The testing provides a reasonable simulation of temperature and thermal stress effects in a flowing hydrogen environment. Though no information is gained about radiation damage, the furnace testing is extremely valuable for development and verification of fuel element materials and processes. The current work includes testing of subscale W-UO2 slugs to evaluate fuel loss and stability. The materials are then fabricated into samples with seven cooling channels to test a more representative section of a fuel element. Several iterations of testing are being performed to evaluate fuel mass loss impacts from density, microstructure, fuel particle size and shape, chemistry, claddings, particle coatings, and stabilizers. The fuel materials and forms being evaluated on this effort have all been demonstrated to control fuel migration and loss. The objective is to verify performance improvements of the various materials and process options prior to expensive full scale fabrication and testing. Post test analysis will include weight percent fuel loss, microscopy, dimensional tolerance, and fuel stability.

Hickman, Robert↗

NASA NTRS1982

Progress in ceramic component fabrication technology

Net shape techniques have been used in the production of rotating and static vehicular engine high-temperature components composed of sintered Alpha-SiC (SASC). Injection-molded rotors have been cold spin tested, as well as a slip-cast combustor assembly hot rig. SASC pistons and cylinder liners have also been constructed for an opposed piston, two-cycle diesel test rig while test results are presented. An uncooled, minimum-friction internal combustion engine with multi-fuel capability due to its elevated combustion temperatures appears to be achievable in the near term by means of SASC techniques. The flexural strength of SASC at 1500 C is 446 MPa, identical to that at room temperature, and excellent strength retention has been demonstrated after 3500 hours of cyclic exposure.

Storm, R. S.↗

NASA NTRSDate not supplied

Advanced eLectrical Bus (ALBus) CubeSat: From Build to Flight

Advanced eLectrical Bus (ALBus) CubeSat is a technology demonstration mission of a 3-U CubeSat with an advanced digitally controlled electrical power system and novel use of Shape Memory Alloy (SMA) technology for reliable deployable solar array mechanisms. The primary objective was to advance the power management and distribution (PMAD) capabilities to enable future missions requiring more flexible and reliable power systems with higher output power capabilities. Goals included demonstration of 100W distribution to a target electrical load, response to continuous and fast transient power requirements, and exhibition of reliable deployment of solar arrays and antennas utilizing re-settable SMA mechanisms. The power distribution function of the ALBus PMAD system is unique in the total power to target load capability, as power is distributed from batteries to provide 100W of power directly to a resistive load. The deployable solar arrays utilize NASA’s Nickel-Titanium-Palladium-Platinum (NiTiPdPt) high-temperature SMAs for the retention and release mechanism, and a superelastic binary NiTi alloy for the hinge component. The project launched as part of the CubeSat Launch Initiative (CLI) Educational Launch of Nanosatellites (ELaNa) XIX mission on Rocket Lab’s Electron in December 2018. This paper summarizes the final launched design and the lessons learned from build to flight.

Deboshri Sadhukhan↗

NASA NTRSDate not supplied

Advanced eLectrical Bus (ALBus) CubeSat: From Build to Flight

The Advanced eLectrical Bus (ALBus) CubeSat project is a technology demonstration mission of a 3-U CubeSat with an advanced, digitally controlled electrical power system capability and novel use of Shape Memory Alloy (SMA) technology for reliable deployable solar array mechanisms. The objective of the project was to advance the state of power management and distribution (PMAD) capabilities to enable future missions requiring flexible and reliable power systems with higher output power capabilities. The goals of the mission were to demonstrate 100W distribution to a target electrical load, respond to continuous and fast transient power requirements, and show reliable deployment of solar arrays and antennas utilizing re-settable SMA mechanisms. The power distribution function of the ALBus PMAD system is unique in the total power to target load capability. Power is distributed from batteries to provide 100W of power directly to a resistive load. The deployable solar arrays utilize NASA Glenn Research Center’s Nickel-Titanium-Palladium-Platinum high-temperature SMAs for the retention and release mechanism, and a super-elastic binary NiTi alloy for the hinge component. The deployable solar array hinge design features the utilization of SMA material properties for a dual purpose. First, the hinge uses the super-elastic SMA properties to provide the spring force to deploy the arrays. Second, the electrical conductivity properties of the SMA enables the design to provide clean conduits for power transfer from the deployable arrays to the power management system. This eliminates the need for electrical harnesses between the arrays and the PMAD system in the ALBus system design. The uniqueness of the SMA retention and release mechanism design is the ability to reset the mechanism and reuse the same hardware. This allow functional tests of the mechanisms before flight with no degradation of performance and flying the hardware that is tested. The project launched as part of the CubeSat Launch Initiative Educational Launch of Nanosatellites (ELaNa) XIX mission on Rocket Lab’s Electron in December 2018. This paper summarizes the final launched design of ALBus and lessons learned from the technology and overall project from development through flight.

Deboshri Sadhukhan↗

NASA NTRS2002

New High-Performance SiC Fiber Developed for Ceramic Composites

Sylramic-iBN fiber is a new type of small-diameter (10-mm) SiC fiber that was developed at the NASA Glenn Research Center and was recently given an R&D 100 Award for 2001. It is produced by subjecting commercially available Sylramic (Dow Corning, Midland, MI) SiC fibers, fabrics, or preforms to a specially designed high-temperature treatment in a controlled nitrogen environment for a specific time. It can be used in a variety of applications, but it currently has the greatest advantage as a reinforcement for SiC/SiC ceramic composites that are targeted for long-term structural applications at temperatures higher than the capability of metallic superalloys. The commercial Sylramic SiC fiber, which is the precursor for the Sylramic-iBN fiber, is produced by Dow Corning, Midland, Michigan. It is derived from polymers at low temperatures and then pyrolyzed and sintered at high temperatures using boron-containing sintering aids (ref. 1). The sintering process results in very strong fibers (>3 GPa) that are dense, oxygen-free, and nearly stoichiometric. They also display an optimum grain size that is beneficial for high tensile strength, good creep resistance, and good thermal conductivity (ref. 2). The NASA-developed treatment allows the excess boron in the bulk to diffuse to the fiber surface where it reacts with nitrogen to form an in situ boron nitride (BN) coating on the fiber surface (thus the product name of Sylramic-iBN fiber). The removal of boron from the fiber bulk allows the retention of high tensile strength while significantly improving creep resistance and electrical conductivity, and probably thermal conductivity since the grains are slightly larger and the grain boundaries cleaner (ref. 2). Also, as shown in the graph, these improvements allow the fiber to display the best rupture strength at high temperatures in air for any available SiC fiber. In addition, for CMC applications under oxidizing conditions, the formation of an in situ BN surface layer creates a more environmentally durable fiber surface not only because a more oxidation-resistant BN is formed, but also because this layer provides a physical barrier between contacting fibers with oxidation-prone SiC surface layers (refs. 3 and 4). This year, Glenn demonstrated that the in situ BN treatment can be applied simply to Sylramic fibers located within continuous multifiber tows, within woven fabric pieces, or even assembled into complex product shapes (preforms). SiC/SiC ceramic composite panels have been fabricated from Sylramic-iBN fabric and then tested at Glenn within the Ultra-Efficient Engine Technology Program. The test conditions were selected to simulate those experienced by hot-section components in advanced gas turbine engines. The results from testing at Glenn demonstrate all the benefits expected for the Sylramic-iBN fibers. That is, the composites displayed the best thermostructural performance in comparison to composites reinforced by Sylramic fibers and by all other currently available high-performance SiC fiber types (refs. 3 and 5). For these reasons, the Ultra-Efficient Engine Technology Program has selected the Sylramic-iBN fiber for ongoing efforts aimed at SiC/SiC engine component development.

DiCarlo, James A.↗

DOE OSTI2024

Biopolymer-supramolecular polymer hybrids for photocatalytic hydrogen production

Solar generation of H 2 is a promising strategy for dense energy storage. Supramolecular polymers composed of chromophore amphiphile monomers containing perylene monoimide (PMI) have been reported as crystalline light-harvesting assemblies for aqueous H 2 -evolving catalysts. Gelation of these supramolecular polymers with multivalent ions creates hydrogels with high diffusivity but insufficient mechanical stability and catalyst retention for reusability. We report here on using sodium alginate (SA) biopolymer to both induce supramolecular polymerization of PMI and co-immobilize them with catalysts in a robust hydrogel with high diffusivity that can also be 3D-printed. Faster mass transfer was achieved by controlling the material macrostructure by reducing gel diameter and microstructure by reducing biopolymer loading. Optimized gels produce H 2 at rates rivaling solution-based PMI and generate H 2 for up to 6 days. The PMI assemblies in the SA matrix create a percolation network capable of bulk-electron transfer under illumination. These PMI–SA materials were then 3D-printed on conductive substrates to create 3D hydrogel photoelectrodes with optimized porosity. The design of these versatile hybrid materials was bioinspired by the soft matter environment of natural photosynthetic systems and opens the opportunity to carry out light-to-fuel conversion within soft matter with arbitrary shapes and particular local environments.

36 MATERIALS SCIENCE↗

NASA NTRS1991

Tiltrotor research aircraft composite blade repairs: Lessons learned

The XV-15, N703NA Tiltrotor Research Aircraft located at the NASA Ames Research Center, Moffett Field, California, currently uses a set of composite rotor blades of complex shape known as the advanced technology blades (ATBs). The main structural element of the blades is a D-spar constructed of unidirectional, angled fiberglass/graphite, with the aft fairing portion of the blades constructed of a fiberglass cross-ply skin bonded to a Nomex honeycomb core. The blade tip is a removable laminate shell that fits over the outboard section of the spar structure, which contains a cavity to retain balance weights. Two types of tip shells are used for research. One is highly twisted (more than a conventional helicopter blade) and has a hollow core constructed of a thin Nomex-honeycomb-and-fiberglass-skin sandwich; the other is untwisted with a solid Nomex honeycomb core and a fiberglass cross-ply skin. During initial flight testing of the blades, a number of problems in the composite structure were encountered. These problems included debonding between the fiberglass skin and the honeycomb core, failure of the honeycomb core, failures in fiberglass splices, cracks in fiberglass blocks, misalignment of mated composite parts, and failures of retention of metal fasteners. Substantial time was spent in identifying and repairing these problems. Discussed here are the types of problems encountered, the inspection procedures used to identify each problem, the repairs performed on the damaged or flawed areas, the level of criticality of the problems, and the monitoring of repaired areas. It is hoped that this discussion will help designers, analysts, and experimenters in the future as the use of composites becomes more prevalent.

Espinosa, Paul S.↗

NASA NTRS1992

Tiltrotor Research Aircraft composite blade repairs - Lessons learned

Espinosa, Paul S.↗

NASA NTRS2013

Process Optimization of Bismaleimide (BMI) Resin Infused Carbon Fiber Composite

Bismaleimide (BMI) resins are an attractive new addition to world-wide composite applications. This type of thermosetting polyimide provides several unique characteristics such as excellent physical property retention at elevated temperatures and in wet environments, constant electrical properties over a vast array of temperature settings, and nonflammability properties as well. This makes BMI a popular choice in advance composites and electronics applications [I]. Bismaleimide-2 (BMI-2) resin was used to infuse intermediate modulus 7 (IM7) based carbon fiber. Two panel configurations consisting of 4 plies with [+45deg, 90deg]2 and [0deg]4 orientations were fabricated. For tensile testing, a [90deg]4 configuration was tested by rotating the [0deg]4 configirration to lie orthogonal with the load direction of the test fixture. Curing of the BMI-2/IM7 system utilized an optimal infusion process which focused on the integration of the manufacturer-recommended ramp rates,. hold times, and cure temperatures. Completion of the cure cycle for the BMI-2/IM7 composite yielded a product with multiple surface voids determined through visual and metallographic observation. Although the curing cycle was the same for the three panellayups, the surface voids that remained within the material post-cure were different in abundance, shape, and size. For tensile testing, the [0deg]4 layup had a 19.9% and 21.7% greater average tensile strain performance compared to the [90deg]4 and [+45deg, 90deg, 90deg,-45degg] layups, respectively, at failure. For tensile stress performance, the [0deg]4 layup had a 5.8% and 34.0% greater average performance% than the [90deg]4 and [+45deg, 90deg, 90deg,-45deg] layups.

Ehrlich, Joshua W.↗

DOE OSTI2022

Soil pore network response to freeze-thaw cycles in permafrost aggregates

This dataset contains data used for the paper "Pore network response to freeze-thaw cycles in permafrost aggregates". The Related References field will be updated with a full citation when available.Climate change in Arctic landscapes may increase freeze-thaw frequency within the active layer as well as newly thawed permafrost. A highly disruptive process, freeze-thaw can deform soil pores and alter the architecture of the soil pore network with varied impacts to water transport and retention, redox conditions, and microbial activity. Our objective was to investigate how freeze-thaw cycles impacted the pore network of newly thawed permafrost aggregates to improve understanding of what type of transformations can be expected from warming Arctic landscapes. We measured the impact of freeze-thaw on pore morphology, pore throat diameter distribution, and pore connectivity with X-ray computed tomography (XCT) using six permafrost aggregates with sizes of 2.5 cm3 from a mineral soil horizon (Bw; 28-50 cm depths) in Toolik, Alaska. Freeze-thaw cycles were performed using a laboratory incubation consisting of five freeze-thaw cycles (-10˚C to 20˚C) over five weeks. Our findings indicated decreasing spatial connectivity of the pore network across all aggregates with higher frequencies of singly connected pores following freeze-thaw. Water-filled pores that were connected to the pore network decreased in volume while the overall connected pore volumetric fraction was not affected. Shifts in the pore throat diameter distribution were mostly observed in pore throats ranges of 100 microns or less with no corresponding changes to the pore shape factor of pore throats. Responses of the pore network to freeze-thaw varied with aggregate, suggesting that initial pore morphology may play a role in driving freeze-thaw response. Our research suggests that freeze-thaw alters the microenvironment of permafrost aggregates during the incipient stage of deformation following permafrost thaw, impacting soil properties and function in Arctic landscapes undergoing transition. This dataset contains a compressed (.zip) archive of the data and R scripts used for this manuscript. The dataset includes files in .csv format, which can be accessed and processed using MS Excel or R. This archive can also be accessed on GitHub at https://github.com/Erin-Rooney/XCT-freezethaw (DOI: 10.5281/zenodo.5816355).

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Assessing the potential of composite confining systems for secure and long-term CO 2 retention in geosequestration

A potential geologic target for CO 2 storage should ensure secure containment of injected CO 2 . Traditionally, this objective has been achieved by targeting reservoirs with overlying seals-regionally extensive, low permeability units that have been proven capable of retaining buoyant fluid accumulations over geologic time. However, considering that the amount of CO 2 is limited by a decadal injection period, vertical migration of CO 2 can be effectively halted by a composite system of discontinuous shale/silt/mudstone barriers in bedded sedimentary rocks. Here, we studied the impact of depositional architectures in a composite confining system on CO 2 migration and confinement at reservoir scale. We stochastically generated lithologically heterogeneous reservoir models containing discontinuous barriers consistent with statistical distributions of net-sand-to-gross-shale ratio (NTG) and horizontal correlation lengths derived from well log data and observations of producing hydrocarbon fields in Southern Louisiana. We then performed an extensive suite of reservoir simulations of CO 2 injection and post-injection to evaluate the sensitivity of CO 2 plume migration and pressure response of the composite system to a series of geologic and fluid parameters including the lateral continuity of barriers, NTG, permeability anisotropy within the sand body, and capillary pressure contrast between the sand and shale facies. The results indicate that lateral continuity of barriers and NTG are the dominant controls on CO 2 plume geometry and pressure build-up in the reservoir, while the impact of NTG is particularly pronounced. The significance of intraformational barriers becomes apparent as they facilitate the local capillary trapping of CO 2 . Those barriers improve the pore space occupancy by promoting a more dispersed shape of the plume and ultimately retard the buoyancy-driven upward migration of the plume post injection.

58 GEOSCIENCES↗

NASA NTRS2018

Probing Supraglacial Debris on Mars 2: Crater Morphology

Lobate debris aprons (LDA), lineated valley fill (LVF), and concentric crater fill (CCF) on Mars, interpreted to bedebris-covered glaciers, possess craters with a suite of distinct interior landforms (called "ring-mold craters")that have been attributed to the presence of glacial ice at depth or surface modification processes. We testedcurrent hypotheses for the formation of ring-mold craters by conducting a comprehensive analysis of the size andmorphology of 16,457 impact craters 125m in diameter formed within glacial deposits in DeuteronilusMensae. Two major groups, bowl-shaped craters and ring-mold craters, are found, with at least nine distinctcrater types. While there is statistical difference in median diameters between these crater types, this differenceis relatively small and is within the estimated uncertainty in diameter measurements and may be related to moreenhanced erosion of the rims of ring-mold craters. Clear degradation sequences are observed, supporting a rolefor post-impact modification in producing at least some of the diversity in crater landforms. The spatial densityof ring-mold craters is also directly correlated with the development of LDA, LVF, and CCF surface textures. Flowlineations cross-cut two ring-mold crater types but they maintain their circular planforms in some cases, suggestingthat the craters initially formed completely within mantling layers deposited after glacial flow hadceased. We also find analogous craters in non-glacial units; glacial ice is therefore not required to form theobserved morphologic diversity. Our observations are most consistent with formation of crater landforms byemplacement and modification of at least two depositional episodes of icy dust (i.e., "mantle"). This mantle wasinitially tens of meters in thickness to support crater formation, and has experienced much downwasting anderosion since emplacement. Derived crater retention ages of 460 Ma for LDA, LVF, and CCF features in the regiontherefore reflect deposition of mantle units and only give a very minimum age for the formation of LDA, LVF, andCCF

Geological↗

DOE OSTI2020

Erratum to: Soft- and reactive landing of ions onto surfaces: concepts and applications

Soft- and reactive landing of mass-selected ions is gaining attention as a promising approach for the precisely-controlled preparation of materials on surfaces that are not amenable to deposition using conventional methods. A broad range of ionization sources and mass filters are available that make ion soft-landing a versatile tool for surface modification using beams of hyperthermal (<100?eV) ions. The ability to select the mass-to-charge ratio of the ion, its kinetic energy and charge state, along with precise control of the size, shape, and position of the ion beam on the deposition target distinguishes ion soft landing from other surface modification techniques. Soft- and reactive landing have been used to prepare interfaces for practical applications as well as precisely-defined model surfaces for fundamental investigations in chemistry, physics, and materials science. For instance, soft- and reactive landing have been applied to study the surface chemistry of ions isolated in the gas-phase, prepare arrays of proteins for high-throughput biological screening, produce novel carbon-based and polymer materials, enrich the secondary structure of peptides and the chirality of organic molecules, immobilize electrochemically-active proteins and organometallics on electrodes, create thin films of complex molecules, and immobilize catalytically active organometallics as well as ligated metal clusters. In addition, soft landing has enabled investigation of the size-dependent behavior of bare metal clusters in the critical subnanometer size regime where chemical and physical properties do not scale predictably with size. The morphology, aggregation, and immobilization of larger bare metal nanoparticles, which are directly relevant to the design of catalysts as well as improved memory and electronic devices, have also been studied using ion soft landing. This review article begins in section 1 with a brief introduction to the existing applications of ion soft- and reactive landing. Section 2 provides an overview of the ionization sources and mass filters that have been used to date for soft landing of mass-selected ions. A discussion of the competing processes that occur during ion deposition as well as the types of ions and surfaces that have been investigated follows in section 3. Section 4 discusses the physical phenomena that occur during and after ion soft landing, including retention and reduction of ionic charge along with factors that impact the efficiency of ion deposition. The influence of soft landing on the secondary structure and biological activity of complex ions is addressed in section 5. Lastly, an overview of the structure and mobility as well as the catalytic, optical, magnetic, and redox properties of bare ionic clusters and nanoparticles deposited onto surfaces is presented in section 6. © 2015 Wiley Periodicals, Inc. Mass Spec Rev 35:439–479, 2016.

Johnson, Grant E.↗

DOE OSTI2025

Modeling the microplastic distribution along the Delaware River Estuary: Accumulation patterns and hydrodynamic influences

Microplastic pollution is an escalating environmental concern, particularly in densely populated estuary regions, where it poses significant threats to aquatic life and human health. The dispersion patterns of microplastic particles along estuaries are influenced and complicated by multiple environmental factors such as river flow, tidal mixing, salt intrusion, and estuarine circulation. This study examines the accumulation and dispersion patterns by modeling three typical classes of microplastics in the Delaware River Estuary: synthetic fibers, sinking plastic films, and rising plastic pellets. Our findings reveal specific areas with high microplastic accumulation for each type. Notably, the upper estuary regions exhibit significant retention of rising microplastics, associated with a region with reduced along-thalweg velocities downstream of Trenton, NJ and upstream of Philadelphia, PA. Conversely, synthetic fibers and sinking plastic films accumulate in the flow convergence zone near the bottom salinity front, typically downstream of Philadelphia. All of the microplastic accumulation hot spot locations are controlled by the balance of river discharge and salinity intrusions. During the dry season, microplastic accumulation hot spots shift upstream in the estuary, whereas in the wet season, the strong river discharge pushes them downstream. Furthermore, on the other hand, tidal mixing, settling, and resuspension processes strongly impact the spreading of microplastics along the river.

Delaware River Estuary↗