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NASA NTRS1999

Flight Validation of Atomic Oxygen Resistant Resistant Polymers

Because of its high reactivity, atomic oxygen causes surface erosion on polymeric materials. although the reaction efficiency depends on the chemical structure of the polymer. We have found an organotin compound, bis(triphenyltin) oxide (BTO), which has an unusually high solubility in solutions of a number of commercial high performance polymers. Films of these polymers containing BTO showed a substantial reduction in erosion by atomic oxygen when compared with films of the pure material. Analysis has shown that in the presence of atomic oxygen, erosion of the exposed surfaces of the BTO-containing films leaves a residual protective tin oxide coating . Since the additive is uniformly distributed throughout the polymeric material, any break or puncture in the protective coating is "healed" by the material below. Samples were exposed to the environment of the low earth orbit (LEO) on two Space Shuttle flights, STS-46, in June of 1992, and STS-51 in September of 1993. The analysis of these samples has been reported previously. For both flights, the samples were small (1.3 cm and 1.9 cm respectively) thus limiting the scope of analysis. In the research under this cooperative agreement, films of a polyetherimide, were exposed to the LEO environment on Space Shuttle flight STS-85 in August of 1997 as part of the Evaluation of Space Environment and Effects on Materials (ESEM) experiment. The polyetherimide chosen is available commercially as Ultem, registered to the General Electric Company. Films of pure Ultem, Ultem with 10% BTO by mass, and Ultem with 20% BTO by mass were exposed in the ram direction for 40 hours during STS-85. Ultem has a Tg of 215 deg C and is soluble in common chlorinated solvents. Granules of the polymer were dried at 120 deg C, but otherwise were used as received. Films were cast on a glass plate from a solution of the polymer in a 60/40 (w/w) mixture of chloroform and 1,1,2,2-tetrachloroethane. The plate was placed in a dust-free box for at least 24 hours to allow much of the solvent to evaporate, and then was moved to a vacuum oven and slowly heated from 20 to 220 deg C over a period of two weeks to completely remove all solvent. Each exposed sample was 7.6 cm long and 2.2 cm wide and about 0.025 mm thick. The structures of Ultem and bis(triphenyltin) oxide are shown.

Kiefer, Richard L.↗

NASA NTRS1999

Nondestructive Superresolution Imaging of Defects and Nonuniformities in Metals, Semiconductors, Dielectrics, Composites, and Plants Using Evanescent Microwaves

We have imaged and mapped material nonuniformities and defects using microwaves generated at the end of a microstripline resonator with 0.4 micrometer lateral spatial resolution at 1 GHz. Here we experimentally examine the effect of microstripline substrate permittivity, the feedline-to-resonator coupling strength, and probe tip geometry on the spatial resolution of the probe. Carbon composites, dielectrics, semiconductors, metals, and botanical samples were scanned for defects, residual stresses, subsurface features, areas of different film thickness, and moisture content. The resulting evanescent microwave probe (EMP) images are discussed. The main objective of this work is to demonstrate the overall capabilities of the EMP imaging technique as well as to discuss various probe parameters that can be used to design EMPs for different applications.

Tabib-Azar, M.↗

NASA NTRS2004

Synchronized Electronic Shutter System and Method for Thermal Nondestructive Evaluation

The invention is a synchronized electronic shutter system (SESS) and method for same side and through transmission thermal analysis and inspection of a material for finding defects, corrosion, disbond defects, integrity of a weld and determination of paint thickness. The system comprises an infrared detector that acquires background images of the sample. A shutter then covers the detector and lamps rapidly heat the sample above ambient temperature. Shutters cover all lamps at the same time the shutter over the infrared detector is opened. The infrared detector acquires a series of temperature images over time radiated from the sample a s the sample cools down. After collecting a series of temperature images taken by the SESS, a processed image is developed using one of the group comprising time derivative calculation, temperature normalization data reduction routine, thermal diffusivity curve fitting and averaging the series of temperature images.

Joseph N Zalameda↗

NASA NTRS2020

Determination of the Complex Refractive Indices of Aerosol Analogs Formed at Low Temperatures with the NASA Ames Optical Constants Facility (OCF)

The NASA Ames COsmic SImulation Chamber (COSmIC) [1] is a unique experimental facility that allows: 1) cooling a gas mixture to low temperature (150 K) in a jet expansion before inducing chemistry by plasma; and 2) controlling the extent of the chemical reactions by employing a pulsed plasma discharge. This enables the study of the early stages of aerosol production, as well as specific chemical pathways in planetary environments (e.g. Titan’s and Pluto’s atmospheres). Both the gas and solid products can be studied. For a decade COSmIC has been used to simulate Titan’s atmospheric chemistry at low, Titan-like temperature [2]. New developments on the COSmIC facility are investigating formation of aerosols in tenuous, or transitory, atmospheres of other icy bodies [3-5], as well as cool exoplanets atmospheres having a hydrocarbon component, that results in formation of hazes and/or surface deposits of refractory materials. The new Ames Optical Constants Facility enables determination of the aerosol analogs' complex refractive indices, n and k, from 0.59 to 200 μm [2]. Here we report efforts of determining n and k from ex-situ transmission measurements of solid samples produced from binary N-CH and Ar-CH, and tertiary N-CH-CH and Ar-CH-CHgas mixtures in COSmIC, and deposited onto various substrates. A computational technique [6] that addresses interference fringes observed in the laboratory transmission data, particularly at wavelengths < 3 μm, has been implemented and applied to determine n and k for the samples. At visible and near-infrared wavelengths(0.4-1.6 μm) the deposit thickness, and its variation, as well as n and k were determined by a commercial entity. These data provide the ability to compare results, from independent methods, in the region of overlap between the two approaches.

Ella M Sciamma-O'Brien↗

NASA NTRS2022

Titan In-situ Resource Utilization (ISRU) Sample Return (TISR)

Titan is unique in the outer solar system in that it is the only moon with a thick atmosphere, and the only body in the solar system outside the Earth with liquid seas on its surface. The Titanian oceans, however, are seas of liquid hydrocarbons, and the rocks on the surface are solid water ice. Like other icy Moons of the outer solar system, beneath the ice crust, Titan also has a subsurface ocean. Rodriguez et al. refer to it as the “world with two oceans”, an organic-rich body with interior-surface-atmosphere interactions that are comparable in complexity to the Earth. [1] Titan is scientifically fascinating in many ways [2], [3], [4]. The Compass Team will emphasize just one here: Titan is a high priority target for astrobiology [4] [5] [6] [7] [8] [9] [10] [11]. It is a world with a surface and atmosphere rich in the complex organic compounds known as tholins. A detailed understanding of the nature of these complex compounds will require an analysis using a full laboratory on Earth. Because of its value to understanding the organic compounds of the outer solar system which may be the primordial building-blocks of life, return of samples from Titan to laboratories on Earth will be the primary goal of this mission. While this would give unprecedented science return, returning even a small sample from Titan using conventional technology would be tremendously difficult. Saturn is almost a billion miles from the Earth, about thirteen times farther than Mars. A return mission to Saturn requires such a large total-mission ∆V that, with conventional technology, the mass ratios required are prohibitive. Such a sample return would truly be “mission incredible.” But to date, a sample return mission from so distant a target has been assumed to be, not merely incredible, but mission impossible. The Compass Team has proposed [2] [12] that by manufacturing the propellant for the return to Earth using the resources available on Titan, such a mission becomes possible. The task of this report is to show that it is reasonable with credible space technology.

Titan↗

NASA NTRS2016

Application of Scanning-Imaging X-Ray Microscopy to Fluid Inclusion Candidates in Carbonates of Carbonaceous Chondrites

In order to search for such fluid inclusions in carbonaceous chondrites, a nondestructive technique using x-ray micro-absorption tomography combined with FIB sampling was developed and applied to a carbonaceous chondrite. They found fluid inclusion candidates in calcite grains, which were formed by aqueous alteration. However, they could not determine whether they are really aqueous fluids or merely voids. Phase and absorption contrast images can be simultaneously obtained in 3D by using scanning-imaging x-ray microscopy (SIXM). In refractive index, n=1-sigma+i(beta), in the real part, 1-sigma is the refractive index with decrement, sigma, which is nearly proportional to the density, and the imaginary part, beta, is the extinction coefficient, which is related to the liner attenuation coefficient, mu. Many phases, including water and organic materials as well as minerals, can be identified by SIXM, and this technique has potential availability for Hayabusa-2 sample analysis too. In this study, we examined quantitative performance of d and m values and the spatial resolution in SIXM by using standard materials, and applied this technique to carbonaceous chondrite samples. We used POM ([CH2O]n), silicon, quartz, forsterite, corundum, magnetite and nickel as standard materials for examining the sigma and mu values. A fluid inclusion in terrestrial quartz and bi-valve shell (Atrina vexillum), which are composed of calcite and organic layers with different thickness, were also used for examining the spatial resolution. The Ivuna (CI) and Sutter's Mill (CM) meteorites were used as carbonaceous chondrite samples. Rod- or cube-shaped samples 20-30 micron in size were extracted by using FIB from cross-sectional surfaces of the standard materials or polished thin sections of the chondrites, which was previously observed with SEM. Then, the sample was attached to a thin W-needle and imaged by SIXM system at beamline BL47XU, SPring-8, Japan. The slice thickness was 109.3 nm and the pixel size was mostly 100 nm.

Tsuchiyama, Akira↗

DOE OSTI2020

Chemical and bonding analysis of liquids using liquid cell electron microscopy

Liquid cell transmission electron microscopy (TEM) has become an essential tool for studying the structure and properties of both hard and soft condensed-matter samples, as well as liquids themselves. Liquid cell sample holders, often consisting of two thin window layers separating the liquid sample from the high vacuum of the microscope column, have been designed to control in situ conditions, including temperature, voltage/current, or flow through the window region. While high-resolution and time-resolved TEM imaging probes the structure, shape, and dynamics of liquid cell samples, information about the chemical composition and spatially resolved bonding is often difficult to obtain due to the liquid thickness, the window layers, the holder configuration, or beam-induced radiolysis. Here, we review different approaches to quantitative liquid cell electron microscopy, including recent developments to perform energy-dispersive x-ray and electron energy-loss spectroscopy experiments on samples in a liquid environment or the liquid itself. We also cover graphene liquid cells and other ultrathin window layer holders.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Field-dependent nonelectronic contributions to thermal conductivity in a metallic ferromagnet with low Gilbert damping

Heat conduction in metals is typically dominated by electron transport since electrons carry both charge and heat. In magnetic metals magnons, or spin waves, excitations of the magnetic order can be used to transport information. Heat conduction via magnons has been previously shown mostly for insulating magnets with low Gilbert damping and resulting long spin-wave lifetimes where conduction electrons cannot contribute. Here we show that thin films of properly optimized metallic ferromagnetic (FM) alloys show significant nonelectronic contributions to heat conduction, which furthermore depend on the direction of an applied magnetic field. These measurements are enabled by micromachined thermal isolation platforms optimized for thermal conductivity measurements of thin-film systems. Electrical conductivity measurements on exactly the same samples allow application of the Wiedemann-Franz relation, which shows large nonelectronic contributions to thermal conductivity for the cobalt-iron alloy with 25% Co. This composition has been shown to have exceptionally low damping for a metallic FM. The thermal conductivity of a 75-nm-thick film of the 25% Co alloy changes by more than 20% at some temperatures, while a reference sample with 50% cobalt that has much higher damping shows no field-direction dependence. Our measurements indicate that applied magnetic fields alter the magnon lifetimes in these films and that these magnons contribute to thermal conductivity in this metallic magnetic alloy with low Gilbert damping.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Role of p-GaN layer thickness in the degradation of InGaN-GaN MQW solar cells under 405 nm laser excitation

GaN-based solar cells with InGaN multiple quantum wells (MQWs) are promising devices for application in space environment, concentrator solar systems, wireless power transmission and multi-junction solar cells. It is therefore important to understand their degradation kinetics when submitted to high-temperature and high-intensity stress. We submitted three samples of GaN-InGaN MQW solar cells with p-AlGaN electron-blocking-layer with different thickness of the p-GaN layer to constant power stress at 310 W/cm 2 , 175 °C for several hundred hours. The main degradation modes are a reduction of open-circuit voltage, short-circuit current, external quantum efficiency, power conversion efficiency and electroluminescence. In particular, we observed that a thinner p-GaN layer results in a stronger degradation observed on the cell operating parameters. The analysis of the dark I-V characteristics showed an increase in low-forward bias current and the analysis of electroluminescence showed a decrease in the electroluminescene emitted by the (forward biased) cell, as a consequence of stress. This work highlights that the cause of degradation is possibly related to a diffusion mechanism, which results in an increase of defect density in the active region. Finally, the impurities involved in the diffusion processes possibly originate from the p-side of the devices, therefore a thicker p-GaN layer reduces the amount of defects reaching the active region.

14 SOLAR ENERGY↗

NASA NTRS1995

A microwave plasma cleaning apparatus

In a microwave electron cyclotron resonance plasma source, reactive plasmas of oxygen and its mixtures of argon have been used for evaluating plasma cleaning technologies. Small aluminum samples (0.95 x 1.9 cm) were coated with thin films (less than or equal to 20 micrometers in thickness) of Shell Vitrea oil and cleaned with reactive plasmas. The discharge parameters, such as gas pressure, magnetic field, substrate biasing, and microwave power, were varied to change cleaning conditions. A mass spectroscopy (or residual gas analyzer) was used to monitor the status of plasma cleaning. Mass loss of the samples after plasma cleaning was measured to estimate cleaning rates. Measured cleaning rates of low-pressure (0.5-m torr) argon/oxygen plasmas were as high as 2.7 micrometers/min. X-ray photoelectron spectroscopy was used to determine cleanliness of the sample surfaces. In this paper, significant results of the plasma cleaning are reported and discussed.

Tsai, C. C.↗

DOE OSTI2023

Optically Active Spin Defects in Few-Layer Thick Hexagonal Boron Nitride

Optically active spin defects in hexagonal boron nitride (hBN) are promising quantum systems for the design of two-dimensional quantum sensing units offering optimal proximity to the sample being probed. In this Letter, we first demonstrate that the electron spin resonance frequencies of boron vacancy centers ($V$$^{–}_{B}$) can be detected optically in the limit of few-atomic-layer thick hBN flakes despite the nanoscale proximity of the crystal surface that often leads to a degradation of the stability of solid-state spin defects. We then analyze the variations of the electronic spin properties of $V$$^{–}_{B}$ centers with the hBN thickness with a focus on (i) the zero-field splitting parameters, (ii) the optically induced spin polarization rate and (iii) the longitudinal spin relaxation time. Furthermore, this Letter provides important insights into the properties of $V$$^{–}_{B}$ centers embedded in ultrathin hBN flakes, which are valuable for future developments of foil-based quantum sensing technologies.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2024

Observation of tantalum deposition and growth on TiB2 and ZrB2 from PISCES-RF deuterium and helium plasma exposures

Deuterium and helium plasma exposures on bulk TiB2 and ZrB2 samples were performed using the PISCES-RF linear plasma device. 40 and 90 eV deuterium ion plasma exposures were performed at 240 and 800 °C sample temperatures, and 80 eV helium ion plasma exposures were performed at 800 °C sample temperatures. Following plasma exposures, it was discovered that two plasma conditions (90 eV deuterium and 80 eV helium at 800 °C) resulted in thick (>200 nm) tantalum-rich (>10 at%) surface features on the targets, presumably from tantalum sourced from a tantalum adapter mask or cap used as part of the target holder. This work aims to characterize these tantalum-rich features and examine the mechanisms of impurity deposition.Plasma-induced surface morphology of the tantalum-rich surface layers depends on plasma properties and target temperature and chemistry. Greater titanium sputtering compared to zirconium resulted in more distinct surface features in the TiB2 samples compared to the ZrB2 samples via increased, prompt deposition onto tantalum surface impurities. There is still uncertainty as to why thick tantalum deposition only occurred under some plasma exposure conditions but not others; it is likely due to tantalum sputtering by a combination of boron molecules from the targets and carbon-impurities in the tantalum mask or targets. Impurity driven surface features are a well-documented phenomena in samples exposed to plasma from linear plasma device facilities—this work confirms the occurrence of this and emphasizes the need for chemistry characterization of isolated post-mortem surface features in plasma-exposed samples.

Nuckols, Lauren↗

NASA NTRSDate not supplied

Correlated Changes in Retinal Thickness and Visuomotor Function in Asymptomatic Plaquenil Toxicity Patients

We have previously shown that a 5-minute eye-movement test can capture a number of largely independent “oculometric” parameters of human visual/visuomotor function (Liston & Stone, 2014). This test has been successfully used to characterize mild neural impairment due to traumatic brain injury, sleep and circadian disruption, and alcohol consumption (Liston et al., 2017; Stone et al, 2019; Tyson et al, 2021). Here, we extend this approach to study patients at risk of progressive posterior-segment illness to see how oculometrics relate to standard clinical ophthalmological measures. Five female patients (<20:40 BCVA, 34-60 years old) undergoing hydroxychloroquine treatment (2-7mg/kg/day for 10-23 years for rheumatologic illness) have participated thus far. Under monocular viewing conditions in randomized order, they tracked a moving spot undergoing radial step-ramp motion in one of 90 randomized directions, at one of 5 randomized speeds, starting at random times (for details, see Stone et al, 2019). We computed nine independent oculometrics (latency, initial acceleration, steady-state gain, proportion smooth, saccadic rate, saccadic amplitude, direction noise, speed responsiveness, and speed noise). Spectral-domain optical coherence tomography (Zeiss, Dublin, CA) was used to measure the average thickness of the nine Early Treatment Diabetic Retinopathy Study macular sectors from the internal limiting membrane to the retinal pigmented epithelium. We used Pearson’s correlation between retinal thickness and our oculometrics with t-statistics to test separate one-sided hypotheses across 10 retinae. Our preliminary analysis found significant changes in several different aspects of visuomotor performance. Most notably, latency increased, initial acceleration decreased, and steady-state pursuit gain decreased as retinal thickness decreased (r2 = 0.364, 0.579, and 0.692; one-tailed P = 0.032, 0.005, and 0.001, respectively). Speed responsiveness appeared to decrease, but this effect was marginal for our current sample (r2 = 0.253, P = 0.069). Lastly, direction discrimination and saccadic behavior appeared unchanged. We conclude that oculometrics may provide sensitive measures of changes in retinal thickness. More importantly, oculometrics have the potential to detect impairment before it becomes evident with standard clinical imaging tools, while also providing insight into the behavioral implications of any resulting deficits in visual/visuomotor function.

eye movements↗

NASA NTRS2003

Magnetic Analysis Techniques Applied to Desert Varnish

Desert varnish is a black or reddish coating commonly found on rock samples from arid regions. Typically, the coating is very thin, less than half a millimeter thick. Previous research has shown that the primary components of desert varnish are silicon oxide clay minerals (~60%), manganese and iron oxides (~20-30%), and trace amounts of other compounds [1]. Desert varnish is thought to originate when windborne particles containing iron and manganese oxides are deposited onto rock surfaces where manganese oxidizing bacteria concentrate the manganese and form the varnish [4,5]. If desert varnish is indeed biogenic, then the presence of desert varnish on rock surfaces could serve as a biomarker, indicating the presence of microorganisms. This idea has considerable appeal, especially for Martian exploration [6]. Magnetic analysis techniques have not been extensively applied to desert varnish. The only previous magnetic study reported that based on room temperature demagnetization experiments, there were noticeable differences in magnetic properties between a sample of desert varnish and the substrate sandstone [7]. Based upon the results of the demagnetization experiments, the authors concluded that the primary magnetic component of desert varnish was either magnetite (Fe3O4) or maghemite ( Fe2O3).

Schmidgall, E. R.↗

DOE OSTI2026

Superconducting Material Growth for Radio-Frequency (RF) Cavities

Superconducting radio-frequency (SRF) cavities, usually manufactured from Niobium (Nb), are vital components of modern particle accelerators because of their ability to achieve high acceleration gradients with little power dissipation. Naturally forming Nb surface oxides significantly alter cavity performance by changing surface resistance. A nondestructive characterization of oxide thickness is helpful for relating surface processing treatments to cavity performance. This work develops a protocol to measure Nb oxide thickness using Angle-Resolved X-ray Photoelectron Spectroscopy (ARXPS) while correcting instrumental errors. Using uniform bulk standard samples (Silver, Aluminum oxide, and Germanium), we determined a baseline correction factor to account for analyzer-related intensity evolution as the measurement angle increases. The correction factor was then applied to Nb 3d ARXPS data. Applying the Strohmeier equation to the corrected data yielded a Nb2O5 thickness of 6.04 nm, closely matching the 5.5 (±.05) nm value obtained from cross-sectional transmission electron microscopy. Our approach will bring a method to incorporate inherent errors in the thickness measurements using ARXPS and can be broadly applied to improve the accuracy of thickness measurements in a wide range of heterostructures.

Lambert, Nathan [Fermilab]↗

DOE OSTI2026

Superconducting Material Growth for Radio-Frequency (RF) Cavities

Lambert, Nathan [Fermilab]↗

DOE OSTI2021

Oxygen K -edge X-ray absorption spectra of liquids with minimization of window contamination

We report oxygen K-edge X-ray absorption spectroscopy is used routinely to study a range of solid materials. However, liquid samples are studied less frequently at the oxygen K-edge due to the combined challenges of high-vacuum conditions and oxygen contamination of window materials. A modular sample holder design with a twist-seal sample containment system that provides a simple method to encapsulate liquid samples under high-vacuum conditions is presented. This work shows that pure silicon nitride windows have lower oxygen contamination than both diamond- and silicon-rich nitride windows, that the levels of oxygen contamination are related to the age of the windows, and provides a protocol for minimizing the background oxygen contamination. Acid-washed 100 nm-thick silicon nitride windows were found to give good quality oxygen K-edge data on dilute liquid samples.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2024

Optimizing the spatial resolution and gamma discrimination of SiPM-based Anger cameras

SiPM Anger cameras have been designed for use as 2-dimensional thermal neutron detectors for scientific applications such as at single crystal diffraction instruments. These cameras utilize a neutron sensitive scintillator and an array of SiPM photosensors, separated by a light spreading glass. While this optics package is very effective at detecting and positioning neutrons, it is also sensitive to gamma rays, which are a source of unwanted noise. In this work, we underwent a search of scintillator and spreader glass thicknesses to determine the optimal combination for maximizing spatial resolution. Both experimental results and GEANT4 simulations are presented. Further, to address the issue of gamma ray detection, we have also designed and presented a multi-layer scintillator that reduces the amount of scintillation light produced via gamma-ray energy deposition, allowing for easier pulse-height discrimination. A sample of this geometry has been produced that results in a factor of 2 improvement over an equivalent thickness monolithic scintillator.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗