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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 415 records · Page 23

Anti-Fog Coatings For Spacesuit Helmets

A permanent and robust anti-fog coating was developed that is applied to the interior of polycarbonate spacesuit helmets. The coating is a mechanically resilient and permanent superhydrophilic (SHPL) layer produced by a two-step process consisting of a plasma processing pre-etch followed by the deposition of an optically transparent Diamond Like Carbon (DLC) coating to achieve an anti-fog, SHPL-DLC layer with Water Contact Angle (WCA) < 10°. The all-dry vacuum process consists of an oxygen plasma etching to engineer the surface of the polycarbonate, creating a well-controlled nanotextured morphology, which is key to the superhydrophilic properties, followed by vacuum deposited Plasma Enhanced Chemical Vapor Deposition (PECVD) DLC coating with high surface energy. The process is carried out at low temperatures compatible with polycarbonate materials and the two steps are performed back-to-back without breaking vacuum between steps. The process is readily scalable and compatible with large scale production volumes. The SHPL-DLC coating was tested for > 200 hours exposure using a breath simulator with no detrimental effect on the coating performance. The coating was also tested for exposure to cleaning fluids, IPA chemical exposure, adhesion testing per ASTM D3359, and abrasion resistance per MIL-E-12397 with no detrimental effects.

Spacesuit↗

MPCVD-Grown Nanodiamond Microelectrodes with Oxygen Plasma Activation for Neurochemical Applications

Nanodiamonds (NDs) are a carbon nanomaterial that has a diamond core with heteroatoms and defects at the surface. The large surface area, defect sites, and functional groups on NDs make them a promising material for electrochemical sensing. Previously, we dip-coated ND onto carbon-fiber microelectrodes (CFMEs) and found increases in sensitivity, but the coating was sparse. Here, for this work, we directly grew thin films of ND on niobium wires using microwave plasma chemical vapor deposition (MP-CVD) to provide full surface coverage. ND microelectrodes show a reliable performance in neurotransmitter detection with good antifouling properties. To improve sensitivity, we oxygen plasma etched ND films to activate the surface and intentionally add defects and oxygen surface functional groups. For fast-scan cyclic voltammetry detection of dopamine, oxygen plasma-etching increases the sensitivity from 21 nA/μM to 90 nA/μM after treatment. Fouling was tested by repeated injections of serotonin or tyramine, and both ND and plasma oxidized nanodiamond (NDO) microelectrodes maintain their currents better compared to CFMEs and therefore are more antifouling. Furthermore, a biofouling test in brain slices shows that ND microelectrodes barely have any current drop, while the more hydrophilic NDO microelectrodes decrease more, but still not as much as CFMEs. Overall, grown ND microelectrodes are promising in neurotransmitter detection with excellent fouling resistance, whereas oxygen plasma etching slightly lowers the fouling resistance but dramatically increases sensitivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High reliability sheathed, beryllia insulated, tungsten-rhenium alloy thermocouple assemblies; their fabrication and EMF stability

Tantalum sheathed, BeO insulated, W-3% Re/W-25% Re thermocouple assemblies were fabricated and their emf drift determined during 2059 hours of exposure at 2073 K in a gaseous helium environment. The sheathed thermocouple assemblies were constructed from aged thermoelements, specially heat-treated BeO insulators, and specially cleaned and etched tantalum sheaths. Their thermal emf drifts ranged from the equivalent of only -0.3 to -0.8 K drift per 1000 hours of exposure at 2073 K. No evidence of any gross chemical attack or degradation of the component materials was found. The emf drift and material behavior of some unsheathed, BeO insulated, W-3% Re/W-25% Re thermocouples at 2250 and 2400 K were also determined. Unsheathed thermocouples tested in an argon environment at 2250 K for 1100 hours and at 2400 K for 307 hours exhibited changes in thermal emf that typically ranged from the equivalent of a few degrees K to as much as +11 K. Post-test examinations of these thermocouples revealed some undesirable material degradation and interaction which included erosion of the BeO insulators and contamination of the thermoelements by tantalum from the tantalum blackbody enclosure in which the thermocouples were contained.

Burns, G. W.↗

Chemistry Modeling for Aerothermodynamics and TPS

Recent advances in supercomputers and highly scalable quantum chemistry software render computational chemistry methods a viable means of providing chemistry data for aerothermal analysis at a specific level of confidence. Four examples of first principles quantum chemistry calculations will be presented. Study of the highly nonequilibrium rotational distribution of a nitrogen molecule from the exchange reaction N + N2 illustrates how chemical reactions can influence rotational distribution. The reaction C2H + H2 is one example of a radical reaction that occurs during hypersonic entry into an atmosphere containing methane. A study of the etching of a Si surface illustrates our approach to surface reactions. A recently developed web accessible database and software tool (DDD) that provides the radiation profile of diatomic molecules is also described.

Wang, Dunyou↗

In Situ Analysis of Electron-Induced Chemical Transformations in Vapor-Phase-Synthesized Al-Based Inorganic–Organic Hybrid Thin Films for EUV Resist Platform

The rapid advancement and stringent requirements of extreme ultraviolet (EUV) lithography technology necessitate the development of advanced photoresist systems for next-generation microelectronics. Recent studies have demonstrated that inorganic-based hybrid photoresists offer notable improvements in EUV sensitivity, etch resistance, and greater insusceptibility to pattern collapse compared to their purely organic counterparts. However, variations in the synthesis/coating approaches and chemistry of inorganic–organic photoresists can result in distinct exposure mechanisms. In this work, an Al-based hybrid thin film resist system synthesized via molecular (atomic) layer deposition (MLD or MALD) is explored, focusing on its electron-beam and EUV patterning mechanisms. The Al-based hybrid thin films are deposited using trimethylaluminum (TMA) and the organic precursor hydroquinone, exhibiting a saturated growth rate within the temperature range of 150–200°C. In diluted tetramethylammonium hydroxide (TMAH)-based developer solutions, the electron-irradiated Al-based hybrid thin film system behaves as a negative tone resist, achieving a sensitivity of 10.4 mC/cm 2 at 0.1 kV electron beam lithography (EBL). Chemical changes induced by electron exposure are also analyzed in this study using X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and a unique infrared spectroscopy setup, revealing the potential cross-linking pathways. To further correlate the electron-induced chemical transformations with those mediated by EUV irradiations, a combination of X-ray photoemission electron microscopy/low-energy electron microscopy (XPEEM/LEEM) system is also employed. In conclusion, this study provides critical insights into the mechanisms underlying solubility switching and contributes to the design of advanced resist materials for EUV lithography.

36 MATERIALS SCIENCE↗

Partial analysis of experiment LDEF A-0114

Due to delays in manifesting the return of the Long Duration Exposure Facility from space, attention was concentrated on extracting the maximum information from the EIOM-2 (oxygen interaction with materials experiment) flown on STS-8 in September 1983. An analysis was made of the optical surfaces exposed during that flight and an assessment made of the effect of the 5 eV atomic oxygen upon their physical and chemical properties. The surfaces studied were of two types: high-purity thin films sputtered or evaporated onto 2.54-cm diam lambda/20 fused silica optical flats, and highly polished bulk samples. Rapid etching of carbon and carbonaceous surfaces was observed with polycarbonate CR-39 showing the largest etch of any substrate flown and measured. Of the metals tested, only osmium and silver showed large effects, the former being heavily etched and the later forming a very thick layer of oxide. The first measurable effects on iridium, aluminum, nickel, tungsten and niobium thin films are reported.

Gregory, J. C.↗

Chemistry Modeling for Aerothermodynamics and TPS

Recent advances in supercomputers and highly scalable quantum chemistry software render computational chemistry methods a viable means of providing chemistry data for aerothermal analysis at a specific level of confidence. Four examples of first principles quantum chemistry calculations will be presented. The study of the highly nonequilibrium rotational distribution of nitrogen molecule from the exchange reaction N + N2 illustrates how chemical reactions can influence the rotational distribution. The reaction C2H + H2 is one example of a radical reaction that occurs during hypersonic entry into a methane containing atmosphere. A study of the etching of Si surface illustrates our approach to surface reactions. A recently developed web accessible database and software tool (DDD) that provides the radiation profile of diatomic molecules is also described.

Wang, Dun-You↗

GaN vertical-channel junction field-effect transistors with regrown p-GaN by metal organic chemical vapor deposition (MOCVD)

Fabricating a vertical-channel junction field-effect transistor includes forming an unintentionally doped GaN layer on a bulk GaN layer by metalorganic chemical vapor deposition, forming a Cr/SiO 2 hard mask on the unintentionally doped GaN layer, patterning a fin by electron beam lithography, defining the Cr and SiO 2 hard masks by reactive ion etching, improving a regrowth surface with inductively coupled plasma etching, removing hard mask residuals, regrowing a p-GaN layer, selectively etching the p-GaN layer, forming gate electrodes by electron beam evaporation, and forming source and drain electrodes by electron beam evaporation. The resulting vertical-channel junction field-effect transistor includes a doped GaN layer, an unintentionally doped GaN layer on the doped GaN layer, and a p-GaN regrowth layer on the unintentionally doped GaN layer. Portions of the p-GaN regrowth layer are separated by a vertical channel of the unintentionally doped GaN layer.

Zhao, Yuji↗

Raman Laser-Induced Structural Modification in CVD-Grown Monolayer MoS 2 for Multi-Purposed Nanofabrication

Molybdenum disulfide (MoS 2 ) has been extensively explored to be utilized as an electronic material in a variety of device applications. In particular, the tunability of MoS 2 enhances its electrical properties making it an intriguing candidate for field-effect transistors (FETs), while also extending beyond electrical properties to structural phase engineering. Laser-induced modifications, particularly with Raman lasers, offer a straightforward method to modulate materials via thermal processes with precise patterning control and energy-level flexibility. However, most studies on the modification of MoS 2 have focused on multilayered structures or have been conducted under low-power laser conditions, leaving the feasibility of structural modifications in monolayer MoS 2 elusive. In this study, we fundamentally elucidated the effects of high-power Raman laser irradiation on the surface of chemical vapor deposition (CVD)-grown monolayer MoS 2 under ambient conditions and uncovered the underlying mechanisms of laser-induced modifications by applying intense photon energy with highly interactive reactions. Our results revealed both etching and deposition phenomena in two discernible regions, and it can be demonstrated by intensity regimes based on the spatial distribution of laser irradiance within the laser-irradiated spot. Furthermore, phase transition was found to be inhibited due to the promoted oxidation and the deposition of hydrogenated amorphous carbon (a-C:H), and p-type doping was observed, likely occurring in the region beneath the a-C:H deposition as substitutional doping on the 2H phase of MoS 2 . To compare the thermal effects, MoS 2 modifications were further analyzed using simplified heat transfer estimations. In conclusion, these findings deepen our understanding of how Raman laser irradiation modifies MoS 2 under ambient conditions, providing guidelines for optimizing its modification processes.

36 MATERIALS SCIENCE↗

Probing and controlling oxygen impurity diffusion in h -BN semi-bulk crystals

Combining its unique features of ultrawide bandgap (UWBG) and two-dimensional nature, h-BN has been explored for emerging applications such as deep ultraviolet optoelectronic devices and single photon emitters. One of the unusual applications of h-BN is for solid-state neutron detectors by utilizing the property of high thermal neutron capture cross section of B-10 as well as its UWBG properties. Although a record high detection efficiency of 59% has been attained by h-BN detectors, the understanding/minimization of defects and impurities is still needed to further advance the h-BN material and detector technologies. We report metal organic chemical vapor deposition growth and oxygen (O) impurity diffusion in thick h-BN. The diffusion coefficient (D) of O impurities has been measured via the evolution of an oxygen related emission with the etching depth, providing a value of D of ∼ 2 × 10−13 cm2/s at 1450 °C and supporting the interpretation that oxygen in h-BN is a substitutional donor. A multiple-buffer-layer approach was employed to mitigate to a certain degree the issue of oxygen diffusion from sapphire substrate during growth. It was demonstrated that the performance of h-BN neutron detectors fabricated from the wafer incorporating multiple buffer layers was significantly improved, as manifested by the enhanced thermal neutron detection efficiency. The advancement of the crystal growth technology of h-BN semi-bulk crystals creates applications in optoelectronic and power electronic devices utilizing the UWBG semiconductor properties of h-BN, while high efficiency h-BN neutron detectors have the potential to supplant the traditional He-3 gas detectors in various application areas by offering the obvious advantages of UWBG semiconductor technologies.

Physics↗

Fast Electromechanical Switches Based on Carbon Nanotubes

Electrostatically actuated nanoelectromechanical switches based on carbon nanotubes have been fabricated and tested in a continuing effort to develop high-speed switches for a variety of stationary and portable electronic equipment. As explained below, these devices offer advantages over electrostatically actuated microelectromechanical switches, which, heretofore, have represented the state of the art of rapid, highly miniaturized electromechanical switches. Potential applications for these devices include computer memories, cellular telephones, communication networks, scientific instrumentation, and general radiation-hard electronic equipment. A representative device of the present type includes a single-wall carbon nanotube suspended over a trench about 130 nm wide and 20 nm deep in an electrically insulating material. The ends of the carbon nanotube are connected to metal electrodes, denoted the source and drain electrodes. At bottom of the trench is another metal electrode, denoted the pull electrode (see figure). In the off or open switch state, no voltage is applied, and the nanotube remains out of contact with the pull electrode. When a sufficiently large electric potential (switching potential) is applied between the pull electrode and either or both of the source and drain electrodes, the resulting electrostatic attraction bends and stretches the nanotube into contact with the pull electrode, thereby putting the switch into the "on" or "closed" state, in which substantial current (typically as much as hundreds of nanoamperes) is conducted. Devices of this type for use in initial experiments were fabricated on a thermally oxidized Si wafer, onto which Nb was sputter-deposited for use as the pull-electrode layer. Nb was chosen because its refractory nature would enable it to withstand the chemical and thermal conditions to be subsequently imposed for growing carbon nanotubes. A 200- nm-thick layer of SiO2 was formed on top of the Nb layer by plasma-enhanced chemical vapor deposition. In the device regions, the SiO2 layer was patterned to thin it to the 20-nm trench depth. The trenches were then patterned by electron- beam lithography and formed by reactive- ion etching of the pattern through the 20-nm-thick SiO2 to the Nb layer.

Kaul, Anupama↗

Medicine Delivery Device with Integrated Sterilization and Detection

Sterile delivery devices can be created by integrating a medicine delivery instrument with surfaces that are coated with germicidal and anti-fouling material. This requires that a large-surface-area template be developed within a constrained volume to ensure good contact between the delivered medicine and the germicidal material. Both of these can be integrated using JPL-developed silicon nanotip or cryo-etch black silicon technologies with atomic layer deposition (ALD) coating of specific germicidal layers. The application of semiconductor processing techniques and technologies to the problems of fluid manipulation and delivery has enabled the integration of chemical, electrical, and mechanical manipulation of samples all within a single microfluidic device. This approach has been successfully applied at JPL to the automated processing, detection, and analysis of minute quantities (parts per trillion level) of biomaterials to develop instruments for in situ exploration or extraterrestrial bodies. The same nanofabrication techniques that are used to produce a microfluidics device are also capable of synthesizing extremely high-surface-area templates in precise locations, and coating those surfaces with conformal films to manipulate their surface properties. This methodology has been successfully applied at JPL to produce patterned and coated silicon nanotips (also known as black silicon) to manipulate the hydrophilicity of surfaces to direct the spreading of fluids in microdevices. JPL's ALD technique is an ideal method to produce the highly conformal coatings required for this type of application. Certain materials, such as TiO2, have germicidal and anti-fouling properties when they are illuminated with UV light. The proposed delivery device contacts medicine with this high-surface-area black silicon surface coated with a thin-film germicidal deposited conformally with ALD. The coating can also be illuminated with ultraviolet light for the purpose of sterilization or identification of the medicine itself. This constrained volume that is located immediately prior to delivery into a patient, ensures that the medicine delivery device is inherently sterile. An additional benefit to integrating a high-surface-area template within the fluid channel of a medicine delivery device is that one can envision a number of different functional coatings that could facilitate the capture and analysis of either microbial contaminants or the medicine itself. For example, one could attach antibodies or some other binding agent with a specific affinity to the silicon nanotip template. Once a target molecule or microbe is bound to the high-surface- area template, one could use an optical analytical technique such as fluorescence or adsorption to determine the identity and potentially the concentration of the species of interest. By illuminating the bound species from the back, it may also be possible to probe only the molecules with an evanescent wave, making detection of the species from the front side of the device much simpler.

Shearn, Michael J.↗

Electro-Chemically Enhanced Mechanical Polishing of Nickel Mandrels

Grinding and mechanical polishing techniques used for x-ray optics mandrel figuring lead to mid-frequency surface ripple. These small figure variations have to be addressed in order to improve the performance of the resulting x-ray mirrors. If the electrochemical etching is combined with mechanical polishing, the figuring and the surface finishing cm be done simultaneously and be used to correct the mid-frequency surface ripple. It is shown that the electrochemical mechanical polishing method allows selective removal of nickel alloy without mandrel surface microroughness degradation.

Gubarev, Mikhail↗

Stable electrospray signal on a microfabricated glass chip with three-dimensional open edge and tiered depth geometries

This paper presents the microfabrication and performance of a three-dimensional electrospray ionization (ESI) emitter tip made from glass, which achieves stable current signals important for chemical analysis. Our novel microfabrication process and custom-built signal conditioning hardware provides the advantage of providing accurate features and steady signals. The fabrication process relies on standard microfabrication techniques (i.e., deposition, photolithography, and wet etching). This fabrication method involves the novel application of two layers of positive and negative photoresists in addition to Parafilm® wax tape. Open edge and tiered depth details were successfully created from a multilayer planar mask. This is a benefit for integrated miniaturized and microfluidic systems that often require micro features for their functionality but relatively large millimeter size features for their physical periphery. We demonstrate the fundamental performance of electrospray with this microfluidic chip. The emitter tip was fixed on a linear axis stage with high resolution (10 μm) to finely control the tip distance from a metal counter electrode plate. Further, a custom printed circuit board system was built to safely control four voltages applied to the microchip ports from a single high voltage power supply. To readily form the electrospray, non-aqueous solvents were used for their low viscosity and a constant voltage of +2.7 kV was applied to the sheath electrospray microchannel. The liquid being sprayed was 80/20 (v/v) methanol/acetonitrile with 0.1% acetic acid in the sheath microchannel and with ammonium acetate (10–40 mM) in its remaining microchannels. The electrospray signal was measured in response to varying the distance (1.4 to 1.6mm) between the electrospray emitter tip and a metal counter electrode plate in addition to the varying concentration of the background electrolyte, ammonium acetate. Stable and repeatable electrospray signal showed linear relationships with emitter tip distance and concentration (r 2 ≥ 0.95).

42 ENGINEERING↗

Metal-Confined Synthesis of ZnS 2 Monolayer Catalysts for Dinitrogen Electroreduction

Atomically thin two-dimensional (2D) materials are of great significance in catalytic, energy storage, and electronic devices. So far, such materials are limited to several categories with layered structures. Herein, we predict an unusual atomically thin ZnS2 monolayer and exploit a metal-confined chemical vapor deposition strategy for the successful preparation of such an unprecedented 2D material, where a sulfide monolayer was first grown on metal nanosheets to form a sulfide/metal/sulfide sandwich structure, and then, the metal core was etched out to obtain freestanding sulfide monolayers. As shown in this work, the ZnS 2 monolayer possesses unique electron-deficient properties related to the atomic structure and exhibits high catalytic activity for dinitrogen electroreduction. Our work will enable creating 2D TMD materials that were previously inexistent or inaccessible.

2D Materials↗

The interactions of atmospheric cosmogenic radionuclides with spacecraft surfaces

The discovery of the cosmogenic radionuclide Be-7 on the front surface of the Long Duration Exposure Facility (LDEF) has opened new opportunities to study several unexplored regions of space science. The experiments have shown that the Be-7 found was concentrated in a thin surface layer of spacecraft material. The only reasonable source of the isotope is the atmosphere through which the spacecraft passed. It is expected that the uptake of Be in such circumstances will depend on the chemical form of the Be and the chemical nature of the substrate. It was found that the observed concentration of Be-7 does differ between metal surfaces and organic surfaces such as PTFE (Teflon). It is noted however, that (1) organic surfaces are etched by the atomic oxygen found under these orbital conditions, and (2) the relative velocity of the species is 8 km/s relative to the surface and the interaction chemistry and physics may differ from the norm. Be-7 is formed by disintegration of O and N nuclei under cosmic ray proton bombardment. Many other isotopes are produced by cosmic ray reactions, and some of these are suited to measurement by the extremely sensitive methods of accelerator mass spectrometry.

Gregory, John C.↗

Integrated Optical Interferometers with Micromachined Diaphragms for Pressure Sensing

Optical pressure sensors have been fabricated which use an integrated optical channel waveguide that is part of an interferometer to measure the pressure-induced strain in a micromachined silicon diaphragm. A silicon substrate is etched from the back of the wafer leaving a rectangular diaphragm. On the opposite side of the wafer, ring resonator and Mach-Zehnder interferometers are formed with optical channel waveguides made from a low pressure chemical vapor deposited film of silicon oxynitride. The interferometer's phase is altered by pressure-induced stress in a channel segment positioned over the long edge of the diaphragm. The phase change in the ring resonator is monitored using a link-insensitive swept frequency laser diode, while in the Mach-Zehnder it is determined using a broad band super luminescent diode with subsequent wavelength separation. The ring resonator was found to be highly temperature sensitive, while the Mach-Zehnder, which had a smaller optical path length difference, was proportionally less so. The quasi-TM mode was more sensitive to pressure, in accord with calculations. Waveguide and sensor theory, sensitivity calculations, a fabrication sequence, and experimental results are presented.

DeBrabander, Gregory N.↗

Integration of Multilevel Superconducting Buried Wiring Layers with Transition-Edge Sensor Detectors for Large Scale Arrays

Lynx, one of the four mission concepts under consideration for the next Astrophysics DecadalReview, will include a microcalorimeter array consisting of more than 100,000 pixels in a compact arrangement with absorber pitch as small as 25 microns. In order to realize the desired array scale, fine-pitch multi-level superconducting wiring with high yield, compatible with rapid expansion of our hydra absorber designs, is essential. We have demonstrated a method of integrating transition edge sensor (TES) microcalorimeters with suitable multilevel buried wiring, fabricated at MIT Lincoln Laboratory using advanced tools dedicated to superconducting circuit fabrication. The TES Mo/Au bilayer is deposited on a high-quality oxide surface created by chemical-mechanical polishing, allowing tight specifications on the TES superconducting transition and link conductivity to be achieved even though the process order has been inverted. The TESs contact the top-level niobium wiring through vias etched through silicon dioxide down to the topmost wiring layer. The article discusses the overall fabrication process, as wellas the behavior of sensors with different via designs, proximity structures, and lateral sizes. An initial iteration of the integrated fabrication process indicates that microcalorimeters fabricated in this way should meet mission specifications using a Mo/Au bilayer with a reasonable critical temperature below 100 mK.

Detector↗