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DOE OSTI2025

Aging studies on chemical vapor deposition and mechanically exfoliated molybdenum disulfide flakes heated in ambient air

The structural integrity of atomically thin two-dimensional molybdenum disulfide (MoS 2 ) is crucial for high-temperature applications, including nanoelectronics and optoelectronics. This study explores the structural stability and electrical performance, under extended thermal exposure in air, of MoS 2 flakes synthesized via chemical vapor deposition (CVD) and mechanical exfoliation. The MoS 2 flakes, both CVD-grown and mechanically exfoliated, were subjected to heating at 200 °C with a relative humidity of 60(±5)% for a prolonged period and investigated with atomic force microscopy and Raman spectroscopy. This study shows that CVD-grown flakes developed noticeable cracks after prolonged heating, whereas mechanically exfoliated flakes mostly retained their structural integrity. Also, both types of flakes showed a decrease in layer thickness and lateral size over time, with mechanically exfoliated flakes exhibiting a comparatively smaller reduction in substrate coverage area. In addition, MoS 2 -based two-terminal devices were subjected to heating at 150 °C for approximately 1100 h, and their electrical characterization revealed a steady rise in current during constant voltage (5 V) conditions. This study enhances our understanding of MoS 2 stability and provides guidance for improving the reliability of MoS 2 -based devices in high-temperature electronic applications.

2D materials↗

NASA NTRS1978

Accelerated/abbreviated test methods for predicting life of solar cell encapsulants to Jet Propulsion Laboratory California Institute of Technology for the encapsulation task of the low-cost solar array project

An important principle is that encapsulants should be tested in a total array system allowing realistic interaction of components. Therefore, micromodule test specimens were fabricated with a variety of encapsulants, substrates, and types of circuitry. One common failure mode was corrosion of circuitry and solar cell metallization due to moisture penetration. Another was darkening and/or opacification of encapsulant. A test program plan was proposed. It includes multicondition accelerated exposure. Another method was hyperaccelerated photochemical exposure using a solar concentrator. It simulates 20 year of sunlight exposure in a short period of one to two weeks. The study was beneficial in identifying some cost effective encapsulants and array designs.

Kolyer, J. M.↗

NASA NTRS1990

X-ray/VUV transmission gratings for astrophysical and laboratory applications

This paper describes the techniques used to fabricate deep-submicron-period transmission gratings for astrophysical and laboratory applications, with special attention given to the major steps involved in the transmission grating fabrication. These include the holographic lithography procedure used to pattern the master transmission grating, the fabrication of X-ray mask, the X-ray lithography step used to transfer the X-ray mask pattern into a substrate, and the electroplating of the substrate to form the final grating pattern. The various ways in which transmission gratings can be used in X-ray and VUV spectroscopy are discussed together with some examples of experiments reported in the literature.

Schattenburg, M. L.↗

DOE OSTI2025

Biosynthesis of bioprivileged, linear molecules via novel carboligase reactions

Over the award period, we made progress on the three aims. We screened twenty-five carboligases for activity coupling twenty-one possible -keto acids (Aim 1). The carboligases were selected across a diverse set of protein sequences. Using Q-Exactive UHPLC-MS, we tested a total of 210 coupled products per enzyme and generated a dataset of 5250 enzyme-substrate activity relationships. We identified multiple enzymes that had activity for synthesizing suberic acid and heptanoic acid (Aim 2). We built a random forest model for predicting the activity of each enzyme toward substrates on which it was not tested using the data from Aim 1. Finally, we evaluated growth defects that occurred due to expression of different carboligases in E. coli (Aim 3). We were able to identify specific metabolites and putative pathways that, when supplemented in the media, recovered the growth defect associated with the presence of specific carboligases. We are in the process of publishing two manuscript describing the methods for high-throughput screening of enzyme promiscuity, using machine learning to predict activity on untested substrates, and enzyme activity data we collected. This project has produced enabling data for biosynthesis of a range of new-to-nature compounds to support biomanufacturing.

60 APPLIED LIFE SCIENCES↗

NASA NTRSDate not supplied

RGB Imaging as a Tool to Monitor Indoor Crop Plant Production

Future crop production in space will require robust monitoring technologies that can optimize crop yield, reduce waste, and generate data for an automated plant growth design. Imaging has been suggested as a tool for measuring plant health, yet imaging systems for indoor crops have not been tested in spaceflight. Fortunately, RGB images of crop plants growing inside the Advanced Plant Habitat (APH) aboard the ISS have already been captured. In ground-based studies, the Kennedy Space Center (NASA, KSC) is collaborating with the United States Department of Agriculture (USDA ARS) to develop an imaging system for monitoring indoor crop plant health. In one study, we applied a drought stress to ‘Dragoon’ lettuce plants over a period of 14 days and captured RGB images in 24 h increments. Images were analyzed, and by applying a difference index, the images were able to be used to detect the drought stress in lettuce. This difference index was then applied to RGB images collected inside the APH ground unit for a pre-flight experiment growing ‘Outredgous’ lettuce under different substrate moisture conditions, and results showed that the RGB camera was capable of detecting drought stress inside the spaceflight plant growth hardware. These results suggest that RGB cameras already deployed to space may offer valuable information for monitoring plant production in extraterrestrial environments. This research was supported by NASA’s space biology program.

Rachel Tucker↗

DOE OSTI2026

Do Flashing and Sealant Materials Need to be Exposed to Extreme Cycling?

In the U.S., over 50% of homes were built before 1980, when minimal building codes existed. The aging of building envelopes can significantly contribute to the air leakage, moisture intrusion, and durability of buildings leading to higher energy demands. Although the durability of building materials and envelope systems has been studied extensively, the durability of specific components like window-wall flashing and sealants remains underexplored. Current standards such as ASTM, NIST, and AAMA primarily focus on durability testing considering the high temperatures only and require sealant testing on anodized aluminum panels, leaving questions about performance in cold or fluctuating temperatures unanswered. Current ASTM and AAMA standards provide guidelines for durability testing but predominantly focus on exposure to higher temperature conditions. It remains unclear how exposure to cold temperatures, or cycles of both hot and cold conditions, affect the durability of these materials. Furthermore, AAMA standards mandate that flashing materials be tested on anodized aluminum panels, which may not reflect real-world applications. Therefore, this initial study aims to explore this concern through testing by constructing two window-wall interface prototypes and applying five different flashing and sealant materials to their joints. These samples were subjected to extreme temperatures, ranging from −34 ℃ (−30 °F) to 50 ℃ (122 °F), over a 28-day period (fourteen cycles of 24 hours), with daily visual inspections to document any signs of deterioration such as wrinkling, distortion, or warping. The study has two main objectives: (1) to determine whether flashing and sealant materials lose their durability and strength when exposed to varying climate conditions, specifically cold climates, and (2) to assess whether the interaction of these materials with different substrates (e.g., lumber, PVC, insulation) affects their durability and strength under varying climate conditions. The findings demonstrate how aging impacts the durability of window-wall systems interfaces, justifying future research that potentially could lead to the development of new testing protocols if significant defects are identified.

Palani, Hevar [ORNL] (ORCID:0000000220211994)↗

NASA NTRS1993

Design and testing of a unique randomized gravity, continuous flow bioreactor

A rotating, null gravity simulator, or Couette bioreactor was successfully used for the culture of mammalian cells in a simulated microgravity environment. Two limited studies using Lipomyces starkeyi and Streptomyces clavuligerus were also conducted under conditions of simulated weightlessness. Although these studies with microorganisms showed promising preliminary results, oxygen limitations presented significant limitations in studying the biochemical and cultural characteristics of these cell types. Microbial cell systems such as bacteria and yeast promise significant potential as investigative models to study the effects of microgravity on membrane transport, as well as substrate induction of inactive enzyme systems. Additionally, the smaller size of the microorganisms should further reduce the gravity induced oscillatory particle motion and thereby improve the microgravity simulation on earth. Focus is on the unique conceptual design, and subsequent development of a rotating bioreactor that is compatible with the culture and investigation of microgravity effects on microbial systems. The new reactor design will allow testing of highly aerobic cell types under simulated microgravity conditions. The described reactor affords a mechanism for investigating the long term effects of reduced gravity on cellular respiration, membrane transfer, ion exchange, and substrate conversions. It offers the capability of dynamically altering nutrients, oxygenation, pH, carbon dioxide, and substrate concentration without disturbing the microgravity simulation, or Couette flow, of the reactor. All progeny of the original cell inoculum may be acclimated to the simulated microgravity in the absence of a substrate or nutrient. The reactor has the promise of allowing scientists to probe the long term effects of weightlessness on cell interactions in plants, bacteria, yeast, and fungi. The reactor is designed to have a flow field growth chamber with uniform shear stress, yet transfer high concentrations of oxygen into the culture medium. The system described allows for continuous, on line sampling for production of product without disturbing fluid and particle dynamics in the reaction chamber. It provides for the introduction of substrate, or control substances after cell adaptation to simulated microgravity has been accomplished. The reactor system provides for the nondisruptive, continuous flow replacement of nutrient and removal of product. On line monitoring and control of growth conditions such as pH and nutrient status are provided. A rotating distribution valve allows cessation of growth chamber rotation, thereby preserving the simulated microgravity conditions over longer periods of time.

Lassiter, Carroll B.↗

NASA NTRS2009

Suppressing Ghost Diffraction in E-Beam-Written Gratings

A modified scheme for electron-beam (E-beam) writing used in the fabrication of convex or concave diffraction gratings makes it possible to suppress the ghost diffraction heretofore exhibited by such gratings. Ghost diffraction is a spurious component of diffraction caused by a spurious component of grating periodicity as described below. The ghost diffraction orders appear between the main diffraction orders and are typically more intense than is the diffuse scattering from the grating. At such high intensity, ghost diffraction is the dominant source of degradation of grating performance. The pattern of a convex or concave grating is established by electron-beam writing in a resist material coating a substrate that has the desired convex or concave shape. Unfortunately, as a result of the characteristics of electrostatic deflectors used to control the electron beam, it is possible to expose only a small field - typically between 0.5 and 1.0 mm wide - at a given fixed position of the electron gun relative to the substrate. To make a grating larger than the field size, it is necessary to move the substrate to make it possible to write fields centered at different positions, so that the larger area is synthesized by "stitching" the exposed fields.

Wilson, Daniel↗

DOE OSTI2025

Control over Banded Morphologies and Circular Dichroism in Chiral Halide Perovskites

Chiral halide perovskites (c-HPs) merge the chirality of organic cations with the semiconducting properties of metal halide frameworks, creating a family of chiral semiconductors with tunable chiroptoelectronic behavior. Here, we describe the impact of periodic banded morphologies of textured c-HP ( R/S -NEA) 2 PbBr 4 films (NEA = 1- (1-naphthyl)ethylammonium) on their chiroptical behavior. Due to the interplay between the crystalline and glassy phases, the c-HP film growth is driven by rhythmic precipitation, producing a distinctive controllable radial banded pattern with the ( R/S -NEA) 2 PbBr 4 inorganic planes oriented parallel to the substrate. The banded morphology can be controlled, as evidenced by the growth temperature dictating the ridge-to-ridge spacing as well as the density of banded regions. The resulting circular dichroism (CD) spectral shape, intensity, and polarity vary in a seemingly random manner across processing conditions. However, these spectral features can be explained by considering key features of the banded morphology, such as refraction of the incident light due to surface morphology, birefringence, and stacked, rotated crystallites. These effects cannot be canceled by averaging front and back CD spectra of c-HP films, and our model incorporating these effects reproduces all observed CD spectra remarkably well. The control over the c-HP morphology and prediction capabilities of our CD modeling leads to further understanding of this class of semiconductors and the possibility of exploiting structural features for light polarization control akin to enhanced metamaterials.

14 SOLAR ENERGY↗

NASA NTRS1968

Feasibility Study 30 Watts per Pound Rollup Solar Array

Principal efforts in this reporting period were applied to preparation of the detail design of the array structure and mechanisms and to manufacturing drawings for a demonstration model of the selected design concept. Analytical support focused on substantiation of the detail design. Additional studies were performed of dynamic criteron effects on components of the wrap drum. Thermal studies were extended to evaluate another thin film (preferred) material for the substrate and its influence on solar cell temperatures. Electrical design considerations included feasibility studies and ramifications of using a new, larger size, solar cell and a new coverglass application concept. Preliminary evaluations suggest improvement in the array power to weight characteristic and net savings in the estimated cost of cell installation. Weight estimates have been up-dated in keeping with refinements in detail design. Performance of this contractor's rollout solar array design is now projected as capable of producing 31.6 watts per pound of weight; excludes estimated improvements from use of new solar cell design.

Source record↗

NASA NTRS2007

Arc Testing of a Mockup Cable in a Simulated Space Radiation Environment

A mockup cable was irradiated with electrons of 25-100 keV energy in a vacuum chamber. The m'ockup cable consisted of insulated wires on a kapton substrate, overlaid with a metallized teonex shield. Voltages induced on the wires and shield by the electron beam during irradiation were monitored, and voltage changes were used, along with video, to detect arcs due to the charge built-up in the cable. The cable was also cooled with liquid nitrogen to very low temperatures, to simulate cables kept in the dark for long periods of time. Arcing was common at fluences typical of long space missions. Occasionally an arc would occur some time after the electron beam was turned off. The conductivity of the wires and shield was monitored as a function of temperature, and behaved as expected, with lower conductivities at lower temperatures. Arcs from the wires and shield to ground and from the wires to the shield were measured. Sympathetic arcs were also seen, wherein an arc from the shield to ground or from the wires to ground was followed in a short period of time by another arc of a different type. Implications of these results for real cables on long space missions will be discussed, and recommendations given for arc mitigation.

Ferguson, D. C.↗

NASA NTRS2001

Fabrication of poly(ethylene glycol) hydrogel microstructures using photolithography

The fabrication of hydrogel microstructures based upon poly(ethylene glycol) diacrylates, dimethacrylates, and tetraacrylates patterned photolithographically on silicon or glass substrates is described. A silicon/silicon dioxide surface was treated with 3-(trichlorosilyl)propyl methacrylate to form a self-assembled monolayer (SAM) with pendant acrylate groups. The SAM presence on the surface was verified using ellipsometry and time-of-flight secondary ion mass spectrometry. A solution containing an acrylated or methacrylated poly(ethylene glycol) derivative and a photoinitiator (2,2-dimethoxy-2-phenylacetophenone) was spin-coated onto the treated substrate, exposed to 365 nm ultraviolet light through a photomask, and developed with either toluene, water, or supercritical CO2. As a result of this process, three-dimensional, cross-linked PEG hydrogel microstructures were immobilized on the surface. Diameters of cylindrical array members were varied from 600 to 7 micrometers by the use of different photomasks, while height varied from 3 to 12 micrometers, depending on the molecular weight of the PEG macromer. In the case of 7 micrometers diameter elements, as many as 400 elements were reproducibly generated in a 1 mm2 square pattern. The resultant hydrogel patterns were hydrated for as long as 3 weeks without delamination from the substrate. In addition, micropatterning of different molecular weights of PEG was demonstrated. Arrays of hydrogel disks containing an immobilized protein conjugated to a pH sensitive fluorophore were also prepared. The pH sensitivity of the gel-immobilized dye was similar to that in an aqueous buffer, and no leaching of the dye-labeled protein from the hydrogel microstructure was observed over a 1 week period. Changes in fluorescence were also observed for immobilized fluorophore labeled acetylcholine esterase upon the addition of acetyl acholine.

NASA Discipline Life Sciences Technologies↗

NASA NTRS1985

Microbial ecology of extreme environments: Antarctic yeasts and growth in substrate-limited habitats

The high, dry valleys of the Ross Desert of Antarctic, characterized by extremely low temperatures, aridity and a depauperate biota, are used as an analog of the postulated extreme climates of other planetary bodies of the Solar System to test the hypothesis that if life could be supported by Ross, it might be possible where similar conditions prevail. The previously considered sterility of the Ross Desert soil ecosystem has yielded up an indigenous yeast, Cryptoccus vishniacci, which is able to resist the extremes of cold, wet and dry freezing, and long arid periods, while making minimal nutritional demands on the soil.

Vishniac, H. S.↗

DOE OSTI2021

Durable graphene oxide membranes

Embodiments described herein relate generally to durable graphene oxide membranes for fluid filtration. For example, the graphene oxide membranes can be durable under high temperatures non-neutral pH, and/or high pressures. One aspect of the present disclosure relates to a filtration apparatus comprising: a support substrate, and a graphene oxide membrane disposed on the support substrate. The graphene oxide membrane has a first lactose rejection rate of at least 50% with a first 1 wt % lactose solution at room temperature. The graphene oxide membrane has a second lactose rejection rate of at least 50% with a second 1 wt % lactose solution at room temperature after the graphene oxide membrane is contacted with a solution that is at least 80° C. for a period of time.

Frayne, Stephen↗

DOE OSTI2022

Durable graphene oxide membranes

Frayne, Stephen↗

DOE OSTI2020

Ferroelastic Hysteresis in Thin Films of Methylammonium Lead Iodide

Mechanical strain can modify the structural and electronic properties of methylammonium lead iodide MAPbI 3 . The consequences of ferroelastic hysteresis, which involves the retention of structural memory upon cycles of deformation, are reported for polycrystalline thin films of MAPbI 3 . Repeatedly bent films were examined using grazing incidence wide-angle X-ray scattering (GIWAXS) to quantitatively characterize the strains and proportions of twin domains. Approximate locations for the coercive stress and saturation on the ferroelastic stress–strain curve are identified, and changes to the stress–strain curve with cyclic strain are characterized. Notably, an external stress source, such as thermal stress from the substrate or a roll-to-roll printing setup, must apply at least |50| MPa to modify the proportions of different twins. The presence of specific twin domains is found to correlate to previously reported strain and defect heterogeneity in MAPbI 3 films. Domains from differently strained twin sets interact with each other. Long-term stability testing reveals that the domain walls are highly immobile over extended periods. Nucleation of new domain walls occurs for specific mechanical strains and correlates closely with degradation. Furthermore, these results help to explain the behavior of ion migration, degradation rate, and photoluminescence in thin films under compressive and tensile strain.

Defects↗

DOE OSTI2024

Reactor wall effects in Si–Cl 2 –Ar atomic layer etching

This work complements our previous manuscript [J. Vac. Sci. Technol. A41, 062602 (2023)] where predictions from molecular dynamics (MD) simulations of silicon–chlorine–argon (Si–Cl 2 –Ar) atomic layer etching (ALE) are compared to experiments. When etch product distributions for atomic chlorine (Cl) and silicon chlorides were initially compared to optical emission spectroscopy (OES) signals, it appeared that there was a discrepancy between the MD predictions and experimental results at higher ion fluences. Experiments showed a relatively long period of nearly constant Cl-containing etch products released from the ion-bombarded surface (referred to as the “plateau”) but this effect was not observed in MD simulations. In this report, we demonstrate that the “plateau” observed in the OES signals is most likely due to the desorption of Cl-containing etch products from the walls of the reactor and subsequent adsorption on the Si substrate. Experiments varying the gas residence time in the chamber while keeping incoming gas concentrations and pressure constant support this interpretation. We also conducted experiments with an additional Ar-only flow in the chamber to reduce the concentration of Cl-containing species on the chamber walls. For both sets of flow modification experiments, we observe results consistent with the hypothesis that Cl-containing species desorbing from chamber walls are a significant cause of the observed discrepancy between MD predictions and experimental observations. If the measured OES signals are corrected for this “additional” source of Cl-containing species at the surface, the MD predictions and measured OES signals are in excellent agreement. This further supports the predictive capability of MD simulations to accurately capture the relevant physical and chemical processes in plasma-assisted ALE processes. We provide an order of magnitude estimate of the required density of Cl-containing species that would account for the additional etch products observed. Finally, we discuss the implications of this effect on ALE in plasma nanofabrication.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Surface plasmon-cavity hybrid state and its graphene modulation at THz frequencies

Fabry–Pérot (F–P) cavity and metal hole array are classic photonic devices. Integrating F–P cavity with holey metal typically enhances interfacial reflection and dampens wave transmission. In this work, a hybrid bound surface state is found within rectangular metal holes on a silicon substrate by merging an extraordinary optical transmission (EOT) mode and a high-order F–P cavity mode both spatially and spectrally. Transmission, Q-factor, and bandwidth can be enhanced significantly with respect to the classical EOT and F–P interference by simply sweeping the cavity length. This state can provide EOT properties and ten times broader EOT bandwidth well below the effective plasma frequency of the periodic metal holes, where the metal holes typically show evanescent properties and do not support EOT in theory. Furthermore, a large modulation range of 25 % and 39 % is demonstrated with various graphene patterns for the transmittance of this hybrid state at 500 and 582 GHz, respectively.

36 MATERIALS SCIENCE↗