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NASA NTRS2000

The Effect of Low Earth Orbit Atomic Oxygen Exposure on Phenylphosphine Oxide-Containing Polymers

Thin films of phenylphosphine oxide-containing polymers were exposed to low Earth orbit aboard a space shuttle flight (STS-85) as part of flight experiment designated Evaluation of Space Environment and Effects on Materials (ESEM). This flight experiment was a cooperative effort between the NASA Langley Research Center (LaRC) and the National Space Development Agency of Japan (NASDA). The thin film samples described herein were part of an atomic oxygen exposure experiment (AOE) and were exposed to primarily atomic oxygen (~1 X 1019 atoms/cm2). The thin film samples consisted of three phosphine oxide containing polymers (arylene ether, benzimidazole and imide). Based on post-flight analyses using atomic force microscopy, X-ray photoelectron spectroscopy, and weight loss data, it was found that atomic oxygen exposure of these materials efficiently produces a phosphate layer at the surface of the samples. This layer provides a barrier towards further attack by AO. Consequently, these materials do not exhibit linear erosion rates which is in contrast with most organic polymers. Qualitatively, the results obtained from these analyses compare favorably with those obtained from samples exposed to atomic oxygen and or oxygen plasma in ground based exposure experiments. The results of the low Earth orbit atomic oxygen exposure on these materials will be compared with those of ground based exposure to AO.

Connell, John W.↗

NASA NTRS2004

The Influence of Sizings on the Durability of High-Temperature Polymer Composites

To increase performance and durability of high-temperature composites for potential rocket engine components, it is necessary to optimize wetting and interfacial bonding between high modulus carbon fibers and high-temperature polyimide resins. Sizings commercially supplied on most carbon fibers are not compatible with polyimides. In this study, the chemistry of sizings on two high-modulus carbon fibers (M40J and M60J, Toray) was characterized as was the chemistry of PMR-II-50 fluorinated polyimide resin. The carbon fibers were characterized using single filament wetting, scanning electron microscopy, fourier transform infrared spectroscopy, and x-ray photoelectron spectroscopic measurements. The polyimide matrix resins were coated onto glass filaments for characterization by wetting measurements. Surface energy components were obtained by wetting with nondispersive (methylene iodide), acidic (ethylene glycol), and basic (formamide) probes. A continuous desizing system that uses an environmentally friendly chemical-mechanical process was developed for tow level fiber. Composites were fabricated with fibers containing the manufacturer's sizing, desized, and further treated with a reactive finish. Results of room-temperature tests after thermal aging show that the reactive finish produces a higher strength and more durable interface compared to the manufacturer's sizing. When exposed to moisture blistering tests, however, the better bonded composite displayed a tendency to delaminate, presumably due to trapping of volatiles.

Allred, Ronald E.↗

NASA NTRS2019

Secondary Ion Mass Spectroscopy

Secondary Ion mass Spectroscopy (SIMS), as the name suggests, involves characterizing metallic and other materials trough the spectroscopic analysis of secondary ions emanating from the surface of the material to be characterized by the impact of the high energy primary ions. The primary ion source including the choice of its gun, voltage and current can be selected and used depending on the purpose of the analysis. In most instruments more than one primary ion gun is lined up to the sample stage and can be activated with selected accelerating parameters (voltage and beam intensity). The impingement of primary ions on to the sample surface generates positive, negative or neutral ions, electrons, atoms and atomic clusters. Majority of these sample fragments being neutral, could not be utilized as such fragments cannot be manipulated through the use of electromagnetic or electrostatic lenses. Secondary ions that are positively or negatively charged possess large variation in velocity, charge, and mass. These ionic fragments eventually travel through a system of several lenses in very high vacuum to reach detector/counter. Relative amounts of alloying elements or impurities in an alloy can be calculated from the counts of related ions accumulated in the detector/counter.

Panda, Binayak↗

NASA NTRSDate not supplied

Using Holey Graphene for Improved Interfacial Contact in Solid Electrolyte Ionic Conductivity Measurements

Solid-state batteries (SSBs) are poised to become the batteries of the future with advantages such as higher energy density, lighter weight, versatile geometry, and greater safety due to low flammability risk. An important parameter of the solid electrolyte (SE) used is its ionic conductivity. The ionic conductivity is generally calculated from the bulk resistance of a SE pellet, measured from the electrochemical impedance spectroscopy data. The SE pellet is typically prepared from the electrolyte powder by dry compression and is sandwiched between two blocking current collectors to obtain the impedance spectroscopy data. One of the challenges in conducting this measurement is poor interfacial contacts between the SE pellet and the current collector surfaces. Therefore, measurements reported in the literature may underestimate the true ionic conductivity of a given electrolyte. Holey graphene is a carbon nanomaterial with high electrical conductivity and unique dry compressibility, which is unusual for carbon materials but similar to many oxide and sulfide SEs. In this work, it is demonstrated that adding a thin layer of holey graphene between the electrolyte and the stainless steel current collectors significantly improves the interfacial contact. The ionic conductivity values obtained in the effort were sometimes several times higher than the data measured for SEs without the holey graphene layers. This work calls for more standardized measurement procedures to reduce the discrepancies in reported ionic conductivity values.

Solid state battery↗

NASA NTRS2015

Asteroid (90) Antiope: Another Icy Member of the Themis Family?

Many members of the Themis family show evidence of hydration in the form of oxidized iron in phyllosilicates (Florczak, M. et al. [1999]. Astron. Astrophys. Suppl. Ser. 134, 463–471), and OH-bearing minerals (Takir, D., Emery, J.P. [2012]. Icarus 219, 641–654). The largest member, (24) Themis, has H2O ice covering its surface (Campins, H. et al. [2010]. Nature 464, 1320–1321; Rivkin, A.S., Emery, J.P. [2010]. Nature 464, 1322–1323). We have investigated the second largest Themis-family asteroid, (90) Antiope, which Castillo-Rogez and Schmidt (Castillo-Rogez, J.C., Schmidt, B.E. [2010]. Geophys. Res. Lett. 37, L10202) predict to have a composition that includes water ice and organics. We obtained 2–4-lm spectroscopy of (90) Antiope in 2006 and 2008, and we find an absorption in the 3-lm region clearly present in our 2008 spectrum and likely in our 2006 spectrum. Both spectra have rounded, bowl-shaped absorptions consistent with those ascribed to water ice as in the spectrum of Asteroid (24) Themis. We also present and compare Spitzer 8–12-lm mid-infrared spectra of (24) Themis and (90) Antiope. We find that (90) Antiope is lacking a ‘‘fairy castle’’ dusty surface, which is in contrast to (24) Themis, other Themis family members (Licandro, J. et al. [2012]. Astron. Astrophys. 537, A73), and Jupiter Trojans (e.g. Emery, J.P., Cruikshank, D.P., Van Cleve, J. [2006]. Icarus 182, 496–512). We conclude that the surface structure of (90) Antiope is most similar to Cybele Asteroid (121) Hermione (Hargrove, K.D. et al. [2012]. Icarus 221, 453–455).

Asteroids↗

NASA NTRSDate not supplied

Recent Advances in Soft Matter Characterization Capabilities Developed at NASA GRC for Lunar Exploration: Differential Dynamic Microscopy to Spectroscopy to Computer Vision

In 1991, famous French scientist Pierre-Gilles de Genes was awarded Nobel prize for his impactful research in soft matter, more specifically polymers. He is defined as the founding father of soft matter. In his Nobel lecture (https://www.nobelprize.org/uploads/2018/06/gennes-lecture.pdf ) he described soft matter aka complex fluids as materials with two primary features – (a) complexity and (b) flexibility. The sub-categories of soft matter (e.g.- granular materials, polymers, foams, colloids etc.) are defined on the basis of Pierre-Gilles de Gennes’ definition. At NASA GRC, we are pushing the boundaries for fundamental study of soft matter on Lunar Surface. With regard to Lunar surface science, we are focusing on developing capabilities pertaining to granular materials and bio-soft/active matter to facilitate future efforts in ISRU and bio-ISRU capabilities. In order to achieve fundamental goals of soft matter research within the limitations of Lunar environment, the scientific capabilities need to be small, flexible, modular, off the shelf and the focus needs to be more on developing an interdisciplinary capability that leverages the recent growth in AI/ML and Computer Vision to augment our understanding of fundamental science. This strategy would allow us to reduce our resource requirement during launch, installation, and occupied real estate footprint on Lunar surface In this talk, we will go over 3 different capabilities that we have developed in house and in close collaboration – (a) Differential Dynamic Microscopy (DDM), (b) Portable In-situ Chemical Spectroscopy (PICS) and (c) Computer Vision Enabled Observation. At very high level, Differential Dynamic Microscopy (DDM) allows us to study the structure-property-process relation (microrheology) of bio-soft/active matter using optical microscope and improved image analysis capabilities. PICS uses AI/ML-based advanced signal deconvolution and analysis technique that can work with existing portable spectroscopy tools to perform materials analysis (e.g.- granular materials and bio-soft/active matter) inspection on the go. Finally, computer vision enabled analysis allows us to use simple camera images for 3D reconstruction of experimental process and tracking of objects of interest in an experiment. We expect that this detailed process will allow us reach a thorough understanding of soft matter in Lunar environment. The capabilities developed by us will help to validate and establish fundamental understanding in Lunar environment. This will, in turn, allow us to guide future space exploration missions and expand the knowledge base of the scientific and engineering communities.

Suman Sinha Ray↗

NASA NTRSDate not supplied

Recent Advances in Soft Matter Characterization Capabilities Developed at NASA GRC for Lunar Exploration: Differential Dynamic Microscopy to Spectroscopy to Computer Vision

In 1991, famous French scientist Pierre-Gilles de Genes was awarded Nobel prize for his impactful research in soft matter, more specifically polymers. He is defined as the founding father of soft matter. In his Nobel lecture (https://www.nobelprize.org/uploads/2018/06/gennes-lecture.pdf ) he described soft matter aka complex fluids as materials with two primary features – (a) complexity and (b) flexibility. The sub-categories of soft matter (e.g.- granular materials, polymers, foams, colloids etc.) are defined on the basis of Pierre-Gilles de Gennes’ definition. At NASA GRC, we are pushing the boundaries for fundamental study of soft matter on Lunar Surface. With regard to Lunar surface science, we are focusing on developing capabilities pertaining to granular materials and bio-soft/active matter to facilitate future efforts in ISRU and bio-ISRU capabilities. In order to achieve fundamental goals of soft matter research within the limitations of Lunar environment, the scientific capabilities need to be small, flexible, modular, off the shelf and the focus needs to be more on developing an interdisciplinary capability that leverages the recent growth in AI/ML and Computer Vision to augment our understanding of fundamental science. This strategy would allow us to reduce our resource requirement during launch, installation, and occupied real estate footprint on Lunar surface. In this talk, we will go over 3 different capabilities that we have developed in house and in close collaboration – (a) Differential Dynamic Microscopy (DDM), (b) Portable In-situ Chemical Spectroscopy (PICS) and (c) Computer Vision Enabled Observation. At very high level, Differential Dynamic Microscopy (DDM) allows us to study the structure-property-process relation (microrheology) of bio-soft/active matter using optical microscope and improved image analysis capabilities. PICS uses AI/ML-based advanced signal deconvolution and analysis technique that can work with existing portable spectroscopy tools to perform materials analysis (e.g.- granular materials and bio-soft/active matter) inspection on the go. Finally, computer vision enabled analysis allows us to use simple camera images for 3D reconstruction of experimental process and tracking of objects of interest in an experiment. We expect that this detailed process will allow us reach a thorough understanding of soft matter in Lunar environment. The capabilities developed by us will help to validate and establish fundamental understanding in Lunar environment. This will, in turn, allow us to guide future space exploration missions and expand the knowledge base of the scientific and engineering communities.

Suman Sinha-Ray↗

NASA NTRSDate not supplied

Recent Advances in Soft Matter Characterization Capabilities Developed at NASA GRC for Lunar Exploration: Differential Dynamic Microscopy to Spectroscopy to Computer Vision

Suman Sinha Ray↗

NASA NTRS1991

XPS study of the effect of hydrocarbon contamination on polytetrafluoroethylene (teflon) exposed to atomic oxygen

The presence of hydrocarbon contamination on the surface of polytetrafluoroethylene (PTFE) markedly affects the oxygen uptake, and hence the wettability, of this polymer when exposed to an oxygen plasma. As revealed by X-ray photoelectron spectroscopy (XPS) analysis, the oxygen-to-carbon ratio (O/C) for such a polymer can increase sharply, and correspondingly the fluorine-to-carbon ratio (F/C) can decrease sharply, at very short exposure times; at longer times, however, such changes in the O/C and F/C ratios reverse direction, and these ratios then assume values similar to those of the unexposed PTFE. The greater the extent of hydrocarbon contamination in the PTFE, the larger are the amplitudes of the 'spikes' in the O/C- and F/C-exposure time plots. In contrast, a pristine PTFE experiences a very small, monotonic increase of surface oxidation or O/C ratio with time of exposure to oxygen atoms, while the F/C ratio is virtually unchanged from that of the unexposed polymer (2.0). Unless the presence of adventitious hydrocarbon is taken into account, anomalous surface properties relating to polymer adhesion may be improperly ascribed to PTFE exposed to an oxygen plasma.

Golub, Morton A.↗

NASA NTRS1973

The Nimbus 4 infrared spectroscopy experiment. 2: Comparison of observed and theoretical radiance from 425-1450 cm(minus 1)

The Nimbus 4 infrared interferometer spectrometer (IRIS) measured the thermal emission of the earth's atmosphere and surface from 400-1600/cm with an apodized spectral resolution of 2.8/cm. A comparison of theoretical radiances, computed from in-situ measurements and using a direct integration slant path atmospheric transmittance model, with the observed IRIS radiances has been made to verify the radiometeric and spectral performance of the instrument and to assess the accuracy of the atmospheric transmittances. The radiance comparison has indicated a relatively constant difference of less than 5% in the water vapor continuum in the 425-550/cm and 750-1200/cm atmospheric window regions while in the 667/cm CO2 band the difference was 5-10%. The absolute accuracy was found to be approximately 5-10% for each of the parameters; measured radiances, in-situ measurements, and the atmospheric transmittances, thus it is not possible to uniquely specify the degree of error arising from each parameter in the total resultant difference.

Kunde, V. G.↗

NASA NTRS1998

Reflectance Spectroscopy and Lunar Sample Science: Finally a Marriage After Far Too Long an Engagement

Inferences about the igneous and impact evolution of planetary bodies are based upon spectral remote sensing of their surfaces. However, it is not the rocks of a body that are seen by the remote sensing, but rather the regolith, that may contain small pieces of rock but also many other phases as well. Indeed, recent flybys of objects even as small as asteroid Ida have shown that these objects are covered by a regolith. Thus, spectral properties cannot be directly converted into information about the igneous history of the object. It is imperative to fully understand the nature of the regolith, particularly its finer fraction termed "soil," to appreciate the possible effects of "space weathering" on the reflectance spectra. We have initiated a study of our nearest, regolith-bearing body, the Moon, as "ground truth" for further probes of planetary and asteroidal surfaces. the foundation for remote chemical and mineralogical analyses lies in the physics underlying optical absorption and the linking of spectral properties of materials measured in the laboratory to well understood mineral species and their mixtures. From this statement, it is obvious that there should be a thorough integration of the material science of lunar rocks and soils with the remote-sensing observations. That is, the lunar samples returned by the Apollo missions provide a direct means for evaluation of spectral characteristics of the Moon. However, this marriage of the remote-sensing and lunar sample communities has suffered from a prolonged unconsummated betrothal, nurtured by an obvious complacency by both parties. To make more direct and quantitative links between soil chemistry/mineralogy and spectral properties, we have initiated a program to (1) obtain accurate characterization of the petrography of lunar soils (in terms relevant to remote analyses), coupled with (2) measurement of precise reflectance spectra, with testing and use of appropriate analytical tools that identify and characterize individual mineral and glass components. It is the finest-sized fractions of the bulk lunar soil that dominate the observed spectral signatures.

Taylor, Lawrence A.↗

NASA NTRS2001

Estimating Expressed Temperature and Fractional Area of Hot Lava at the Kilauea Vent with AVIRIS Spectral Measurements

Imaging spectroscopy offers a framework based in physics and chemistry for scientific investigation of a wide range of phenomena of interest in the Earth environment. In the scientific discipline of volcanology knowledge of lava temperature and distribution at the surface provides insight into the volcano status and subsurface processes. A remote sensing strategy to measure surface lava temperatures and distribution would support volcanology research. Hot targets such as molten lava emit spectral radiance as a function of temperature. A figure shows a series of Planck functions calculated radiance spectra for hot targets at different temperatures. A maximum Lambertian solar reflected radiance spectrum is shown as well. While similar in form, each hot target spectrum has a unique spectral shape and is distinct from the solar reflected radiance spectrum. Based on this temperature-dependent signature, imaging spectroscopy provides an innovative approach for the remote-sensing-based measurement of lava temperature. A natural site for investigation of the measurement of lava temperature is the Big Island of Hawaii where molten lava from the Kilauea vent is present at the surface. In the past, Airborne Visible/Infrared Imaging Spectrometer (AVIRIS) data sets have been used for the analysis of hot volcanic targets and hot burning fires. The research presented here builds upon and extends this earlier work. The year 2000 Hawaii AVIRIS data set has been analyzed to derive lava temperatures taking into account factors of fractional fill, solar reflected radiance, and atmospheric attenuation of the surface emitted radiance. The measurements, analyses, and current results for this research are presented here.

Green, Robert O.↗

NASA NTRS2004

Mars Mineral Spectroscopy Web Site: A Resource for Remote Planetary Spectroscopy

A web site dedicated to Mars Mineral Spectroscopy has been established at http://www.mtholyoke.edu/go/mars. Its goal is to provide an easily accessible data set of Mossbauer spectra of minerals collected over a range of temperatures, to provide suitable analog spectra for data acquired on remote surfaces such as Mars. Complementing these data (eventually) will be both reflectance FTIR data, collected at Brown University's RELAB facility, and Raman spectra to be collected by Jill Pasteris at Washington University St. Louis. Through our Education link, we provide information for those wishing to learn about how Mossbauer and other types of spectroscopy work. Our emphasis is to study only well-characterized mineral samples that represent typical rock-forming occurrences such as might exist on Mars and other terrestrial bodies in our solar system.

Dyar, M. D.↗

NASA NTRS1986

Simulation experiments for gamma-ray mapping of planetary surfaces: Scattering of high-energy neutrons

The concentration and distribution of certain elements in surface layers of planetary objects specify constraints on models of their origin and evolution. This information can be obtained by means of remote sensing gamma-ray spectroscopy, as planned for a number of future space missions, i.e., Mars, Moon, asteroids, and comets. To investigate the gamma-rays made by interactions of neutrons with matter, thin targets of different composition were placed between a neutron-source and a high-resolution germanium spectrometer. Gamma-rays in the range of 0.1 to 8 MeV were accumulated. In one set of experiments a 14-MeV neutron generator using the T(d,n) reaction as neutron-source was placed in a small room. Scattering in surrounding walls produced a spectrum of neutron energies from 14 MeV down to thermal. This complex neutron-source induced mainly neutron-capture lines and only a few scattering lines. As a result of the set-up, there was a considerable background of discrete lines from surrounding materials. A similar situation exists under planetary exploration conditions: gamma-rays are induced in the planetary surface as well as in the spacecraft. To investigate the contribution of neutrons with higher energies, an experiment for the measurement of prompt gamma radiation was set up at the end of a beam-line of an isochronous cyclotron.

Brueckner, J.↗

NASA NTRS2014

Spectroscopy of Pluto, 380-930 Nm at Six Longitudes

We have obtained spectra of the Pluto-Charon pair (unresolved) in the wavelength range 380-930 nm with resolution approx..450 at six roughly equally spaced longitudes. The data were taken in May and June, 2014, with the 4.2-m Isaac Newton Telescope at Roque de Los Muchachos Observatory in the Canary Islands, using the ACAM (auxiliary-port camera) in spectrometer mode, and using two solar analog stars. The new spectra clearly show absorption bands of solid CH4 at 620, 728, and 850-910 nm, which were known from earlier work. The 620-nm CH4 band is intrinsically very weak, and its appearance indicates a long optical path-length through the ice. This is especially true if it arises from CH4 dissolved in N2 ice. Earlier work (Owen et al. Science 261, 745, 1993) on the near-infrared spectrum of Pluto (1-2.5 microns) has shown that the CH4 bands are shifted to shorter wavelengths because the CH4 occurs as a solute in beta-phase crystalline N2. The optical path-length through the N2 crystals must be on the order of several cm to produce the N2 band observed at 2.15 microns. The new spectra exhibit a pronounced red slope across the entire wavelength range; the slope is variable with longitude, and differs in a small but significant way from that measured at comparable longitudes by Grundy & Fink (Icarus 124, 329, 1996) in their 15-year study of Pluto's spectrum (500-1000 nm). The new spectra will provide an independent means for calibrating the color filter bands on the Multispectral Visible Imaging Camera (MVIC) (Reuter et al. Space Sci. Rev. 140, 129, 2008) on the New Horizons spacecraft, which will encounter the Pluto-Charon system in mid-2015. They will also form the basis of modeling the spectrum of Pluto at different longitudes to help establish the nature of the non-ice component(s) of Pluto's surface. It is presumed that the non-ice component is the source of the yellow-red coloration of Pluto, which is known to be variable across the surface.

Spectroscopy↗

NASA NTRS1983

The X-ray photoelectron spectroscopy depth profiling and tribological characterization of ion-plated gold on various metals

For the case of ion-plated gold, the graded interface between gold and a nickel substrate and a nickel substrate, such tribological properties as friction and microhardness are examined by means of X-ray photoelectron spectroscopy analysis and depth profiling. Sliding was conducted against SiC pins in both the adhesive process, where friction arises from adhesion between sliding surfaces, and abrasion, in which friction is due to pin indentation and groove-plowing. Both types of friction are influenced by coating depth, but with opposite trends: the graded interface exhibited the highest adhesion, but the lowest abrasion. The coefficient of friction due to abrasion is inversely related to hardness. Graded interface microhardness values are found to be the highest, due to an alloying effect. There is almost no interface gradation between the vapor-deposited gold film and the substrate.

Miyoshi, K.↗

NASA NTRS1988

Scanning Tunneling Microscopy methods for spectroscopic imaging of subsurface interfaces

A new method for spatially-resolved, spectroscopic investigation of subsurface interface structure has been developed. The method, Ballistic Electron Emission Microscopy (BEEM), is based on Scanning Tunneling Microscopy (STM) techniques. BEEM combines STM vacuum tunneling with unique ballistic electron spectroscopy capabilities. BEEM enables, for the first time, direct imaging of subsurface interface electronic properties with nanometer spatial resolution. STM topographic images of surface structure and BEEM images of subsurface properties are obtained simultaneously. BEEM capabilities are demonstrated by investigation of important metal-semiconductor interfaces.

Bell, L. D.↗

NASA NTRS1991

Selective and low temperature synthesis of polycrystalline diamond

Polycrystalline diamond thin films have been deposited on single-crystal silicon substrates at low temperatures (not above 600 C) using a mixture of hydrogen and methane gases by high-pressure microwave plasma-assisted chemical vapor deposition. Low-temperature deposition has been achieved by cooling the substrate holder with nitrogen gas. For deposition at reduced substrate temperature, it has been found that nucleation of diamond will not occur unless the methane/hydrogen ratio is increased significantly from its value at higher substrate temperature. Selective deposition of polycrystalline diamond thin films has been achieved at 600 C. Decrease in the diamond particle size and growth rate and an increase in surface smoothness have been observed with decreasing substrate temperature during the growth of thin films. As-deposited films are identified by Raman spectroscopy, and the morphology is analyzed by scanning electron microscopy.

Ramesham, R.↗