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32 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS2023

Evaluation of the Interference of Tenax®TA Adsorbent With Dimethylformamide Dimethyl Acetal Reagent for Gas Chromatography-Dragonfly Mass Spectrometry and Future Gas Chromatography-Mass Spectrometry in Situ Analysis

Among future space missions, national aeronautics and space administration (NASA) selected two of them to analyze the diversity in organic content within Martian and Titan soil samples using a gas chromatograph – mass spectrometer (GC–MS) instrument. The Dragonfly space mission is planned to be launched in 2027 to Titan's surface and explore the Shangri-La surface region for years. One of the main goals of this mission is to understand the past and actual abundant prebiotic chemistry on Titan, which is not well characterized yet. The ExoMars space mission is planned to be launched in 2028 to Mars’ surface and explore the Oxia Planum and Mawrth Vallis region for years. The main objectives focus on the exploration of the subsurface soil samples, potentially richer in organics, that might be relevant for the search of past life traces on Mars where irradiation does not impact the matrices and organics. One recently used sample pre-treatment for gas chromatography – mass spectrometry analysis is planned on both space missions to detect refractory organic molecules of interest for astrobiology. This pre-treatment is called derivatization and uses a chemical reagent – called dimethylformamide dimethyl acetal (DMF-DMA) – to sublimate organic compounds keeping them safe from thermal degradation and conserving the chirality of the molecules extracted from Titan or Mars’ matrices. Indeed, the detection of building blocks of life or enantiomeric excess of some organics (e.g. amino acids) after DMF-DMA pre-treatment and GC–MS analyses would be both bioindicators. The main results highlighted by our work on DMF-DMA and Tenax®TA interaction and efficiency to detect organic compounds at ppb levels in a fast and single preparation are first that Tenax®TA did not show the onset of degradation until after 150 experiments – a 120 h at 300 °C experiment – which greatly exceeds the experimental lifetimes for the DraMS and GC-space in situ investigations. Tenax®TA polymer and DMF-DMA produce many by-products (about 70 and 46, respectively, depending on the activation temperature). Further, the interaction between the two leads to the production of 22 additional by-products from DMF-DMA degradation, but these listed by-products do not prevent the detection of trace-level organic molecules after their efficient derivatization and volatilization by DMF-DMA in the oven ahead the GC–MS trap and column.

DraMS-Dragonfly mission↗
NASA NTRS1985

High-Temperature Hall-Effect Apparatus

Compact furnace minimizes thermal gradients and electrical noise. Semiautomatic Hall-effect apparatus takes measurements on refractory semiconductors at temperatures as high as 1,100 degrees C. Intended especially for use with samples of high conductivity and low chargecarrier mobility that exhibit low signal-to-noise ratios, apparatus carefully constructed to avoid spurious electromagnetic and thermoelectric effects that further degrade measurements.

Wood, C.↗
NASA NTRS1991

Phase Transformations In Mullite-Precursor Xerogels

Report describes experimental study of phase transformations occurring in monophasic and diphasic xerogels of overall stoichiometric mullite composition during thermal treatment. Mullite valued as refractory material because of relatively high mechanical strength, excellent resistance to thermal shock, high resistance to creep, low density, low thermal conductivity, and stability at high temperature. Part of continuing effort to develop precursor materials transformed into mullite and sintered at temperatures low enough to avoid degradation of non-mullite reinforcing fibers in manufacture of mullite/fiber composites.

Hyatt, Mark J.↗
NASA NTRS1990

Lifetime studies of high power rhodium/tungsten and molybdenum electrodes for application to AMTEC (alkali metal thermal-to-electric converter)

A detailed and fundamental model for the electrochemical behavior of AMTEC electrodes is developed which can aid in interpreting the processes which occur during prolonged operation of these electrodes. Because the sintering and grain growth of metal particles is also a well-understood phenomenon, the changes in electrode performance which accompany its morphological evolution may be anticipated and modeled. The grain growth rate observed for porous Mo AMTEC electrodes is significantly higher than that predicted from surface diffusion data obtained at higher temperatures and incorporated into the grain growth model. The grain growth observed under AMTEC conditions is also somewhat higher than that measured for Mo films on BASE (beta-alumina solid electrolyte) substrates in vacuum or at similar temperatures. Results of modeling indicate that thin Mo electrodes may show significant performance degradation for extended operation (greater than 10,000 h) at higher operating temperatures (greater than 1150 K), whereas W/Rh and W/Pt electrodes are expected to show adequate performance at 1200 K for lifetimes greater than 10,000 h. It is pointed out that current collection grids and leads must consist of refractory metals such as Mo and W which do not accelerate sintering or metal migration.

Williams, R. M.↗
NASA NTRS1974

Development of a mercury electromagnetic centrifugal pump for the SNAP-8 refractory boiler development program

An electromagnetic pump, in which pressure is developed in mercury because of the interaction of the magnetic field and current which flows as a result of the voltage induced in the mercury contained in the pump duct, was developed for the SNAP-8 refractory boiler test facility. Pump performance results are presented for ten duct configurations and two stator sizes. These test results were used to design and fabricate a pump which met the SNAP-8 criteria of 530 psi developed pressure at 12,500 lb/hr. The pump operated continuously for over 13,000 hours without failure or performance degradation. Included in this report are descriptions of the experimental equipment, measurement techniques, all experimental data, and an analysis of the electrical losses in the pump.

Fuller, R. A.↗
NASA NTRS2005

Performance of Ceramics in Severe Environments

Ceramics are generally stable to higher temperatures than most metals and alloys. Thus the development of high temperature structural ceramics has been an area of active research for many years. While the dream of a ceramic heat engine still faces many challenges, niche markets are developing for these materials at high temperatures. In these applications, ceramics are exposed not only to high temperatures but also aggressive gases and deposits. In this chapter we review the response of ceramic materials to these environments. We discuss corrosion mechanisms, the relative importance of a particular corrodent, and, where available, corrosion rates. Most of the available corrosion information is on silicon carbide (SIC) and silicon nitride (Si3N4) monolithic ceramics. These materials form a stable film of silica (SO2) in an oxidizing environment. We begin with a discussion of oxidation of these materials and proceed to the effects of other corrodents such as water vapor and salt deposits. We also discuss oxidation and corrosion of other ceramics: precurser derived ceramics, ceramic matrix composites (CMCs), ceramics which form oxide scales other than silica, and oxide ceramics. Many of the corrosion issues discussed can be mitigated with refractory oxide coatings and we discuss the current status of this active area of research. Ultimately, the concern of corrosion is loss of load bearing capability. We discuss the effects of corrosive environments on the strength of ceramics, both monolithic and composite. We conclude with a discussion of high temperature wear of ceramics, another important form of degradation at high temperatures.

Jacobson, Nathan S.↗
NASA NTRS2006

Phase Stability of a Powder Metallurgy Disk Superalloy

Advanced powder metallurgy superalloy disks in aerospace turbine engines now entering service can be exposed to temperatures approaching 700 C, higher than those previously encountered. They also have higher levels of refractory elements, which can increase mechanical properties at these temperatures but can also encourage phase instabilities during service. Microstructural changes including precipitation of topological close pack phase precipitation and coarsening of existing gamma' precipitates can be slow at these temperatures, yet potentially significant for anticipated disk service times exceeding 1,000 h. The ability to quantify and predict such potential phase instabilities and degradation of capabilities is needed to insure structural integrity and air worthiness of propulsion systems over the full life cycle. A prototypical advanced disk superalloy was subjected to high temperature exposures, and then evaluated. Microstructural changes and corresponding changes in mechanical properties were quantified. The results will be compared to predictions of microstructure modeling software.

Gabb, Timothy P.↗
NASA NTRS1977

Development and evaluation of die materials for use in the growth of silicon ribbons by the inverted ribbon growth process, task 2, LSSA project

Silicon sessile drop experiments were performed on a variety of commercially available refractory carbides, nitrides, oxides, and borides to examine the potential of these materials for applications involving either direct contact with molten silicon or as substrates for CVD coatings in the fabrication of dies and crucibles for containing molten silicon. Simultaneous experiments were also conducted with CVD layers of SiC, Si3N4, and SiOxNy. Silicon nitride layers, deposited with NH3:SiH4 ratios ranging from 100:1 down to 5:1, were examined in sessile drop experiments to determine if the layers are degraded as a result of using lower reagent ratios. Preliminary experiments were undertaken on the stability of CVD Si3N4 near the melting point of silicon. Silicon ribbon segments were grown from vitreous carbon dies which had been coated with CVD Si3N4. Depending upon the purity of the die materials, ribbon resistivity values up to 40 Omega cm were obtained.

Duffy, M. T.↗
NASA NTRS1983

Stability of silica heat shield materials in the Space Shuttle environment

Sample tiles of Space Shuttle reusable surface insulation (RSI) and fibrous refractory composite insulation (FRCI) have been alternately exposed to simulated mission heating and the Kennedy Space Center launch-pad environment for up to 50 cycles. The two types of tiles were coated with an identical glass composition. The coating on RSI tiles was prone to cracking in the test environment while the same coating on FRCI was not. Absorption of water contaminated with environmental deposits resulted in accelerated devitrification in the RSI tiles. Devitrification in FRCI tiles was significantly less. The rate of environmental degradation of tiles appeared to be dependent on the amount of water absorption.

Ransone, P. O.↗
NASA NTRSDate not supplied

Microbial Pigments and Their Degradation Products as Biosignatures

Carotenoids are a class of vibrant biological pigments that have a characteristic chemical structure centered around a polyene core (Lu et al. 2018). Carotenoids and their derivatives are candidate biosignatures because they can persist in the terrestrial geologic record for up to 1.73 billion years (Vinnichenko et al. 2020), have specific structures that are likely the result of complex pathways, mediate the survival of many microorganisms in Mars and Ocean Worlds analog environments, and are detectable with multiple techniques, including Raman spectroscopy. In this project, we aim to investigate the detectability of carotenoid pigments with different spectroscopic methods to inform future instrument selection. We compare the spectra of five unaltered carotenoids, two model compounds, and carotenoid-forming archaeon with visible and deep UV Raman spectroscopy and UVVis absorption spectrophotometry. We then use one model pigment, beta-carotene, to evaluate the likelihood that unique spectral properties of carotenoids, or their refractory byproducts, would be preserved and detectable on a remote planetary surface by exposing it to simulated conditions for Mars. Sample Acquisition. Pigments betacarotene, lutein, zeaxanthin, astaxanthin, and lycopene were purchased from Sigma Aldrich. Halobacterium salinarum NRC-1 was acquired from Carlina Biological and grown in Halobacterium media. Mineral salts including sodium sulfate, sodium carbonate, and halite were used to form matrices in which the beta-carotene was embedded before exposure. Pigment-mineral mixes were at a 1:10 ratio in water. Analytical Techniques. Deep UV Raman data were collected on a custom laboratory mapping spectrometer called MOBIUS (Mineral and Organic Based Investigations using Ultraviolet Spectroscopy), which is an analog to the SHERLOC instrument on the Mars 2020 Perseverance rover (Bhartia et al. 2021). It features a 248.56 nm NeCu pulsed laser, liquid nitrogen-cooled detector, and tunable optical setup. Visible Raman data were collected using a Horiba Jobin Yvon LabRam HR spectrometer with a frequencydoubled Nd:YAG laser (532 nm) and a HeNe laser (633 nm). A VWR 6300 PC UV/Visible Spectrophotometer was used to collect absorption data for carotenoid solutions, model compounds, and solvents in UVpermissible capped cuvettes. Data were collected from 190-1100 nm at 1 nm increments. All spectral data were analyzed using Igor Pro 9 (Wavemetrics). Irradiation. We used a vacuum chamber equipped with a cryostat and a flood electron gun to simulate Martian surface temperatures, low pressures, and ionizing radiation (10keV, 10μA for 6h at 200K for our initial tests). The samples were prepared by drying the pigment-mineral mix onto polished metal tabs, then mounted on the cryostat for processing. Samples were then analyzed directly on the tabs after exposure. Results: In comparing the visible and deep UV Raman spectra of unaltered pigments, we found that they differed drastically. Carotenoids are often studied with visible Raman and typically have peaks at 1525 cm-1 and 1157 cm-1, due to the stretching of the C=C and C-C bonds in the polyene structure. However, in deep UV, the strongest feature is at ~1630 cm-1 and is broad, possibly indicating that multiple peaks are forming this feature. This stark difference is likely due to different preresonant enhancement effects. The UV-Vis results show that there is an absorption band in the deep UV <300 nm, which supports the hypothesis that the 248.6 nm excitation is interrogating another aspect of carotenoids than visible Raman. Our preliminary exposure tests indicated that pigments – even without minerals present - were largely unaltered in the applied conditions, with only a slight broadening in the primary polyene peaks apparent in the visible Raman data. Figure 1. A) Visible vs. deep UV Raman spectra of unaltered beta carotene. B) Schematic of exposure. Conclusions: Our results to date indicate that deep UV and visible Raman spectroscopy, both techniques with planetary mission heritage from Mars 2020 (Wiens et al. 2021, Bhartia et al. 2021), may be used in a complementary manner to observe carotenoids. In addition, we find that beta-carotene is largely resistant to our current exposure conditions, though there may be some amount of amorphization of the material which could cause the broadening of the peaks at 1525 and 1157 cm-1. As a next step, we aim to increase the dosage and duration of exposure to observe degradation of the parent pigment, possibly add UV as a factor via an Ar mini-arc UV lamp and use GC-MS to characterize possible degradation products.

pigments↗
NASA NTRS1991

A very low resistance, non-sintered contact system for use on indium phosphide concentrator/shallow junction solar cells

An investigation is made into the possibility of providing low resistance contacts to shallow junction InP solar cells which do not require sintering and which do not cause device degradation even when subjected to extended annealing at elevated temperatures. We show that the addition of In to Au contacts in amounts that exceed the solid solubility limit lowers the as-fabricated (unsintered) contact resistivity (R sub c) to the 10(exp -5) ohm cm(exp 2) range. We next consider the contact system Au/Au2P3, which has been shown to exhibit as-fabricated R sub c values in the 10(exp -6) ohm cm(exp 2) range, but which fails quickly when heated. We show that the substitution of a refractory metal (W, Ta) for Au preserves the low R sub c values while preventing the destructive reactions that would normally take place in this system at high temperatures. We show, finally, that R sub c values in the 10(exp -7) ohm cm(exp 2) range can be achieved without sintering by combining the effects of In or Ga additions to Au contacts with the effects of introducing a thin Au2P3 layer at the metal-InP interface.

Weizer, Victor G.↗
NASA NTRS1991

A very low resistance, non-sintered contact system for use on indium phosphide concentrator/shallow junction solar cells

An investigation is made into the possibility of providing low resistance contacts to shallow junction InP solar cells which do not require sintering and which do not cause device degradation even when subjected to extended annealing at elevated temperatures. We show that the addition of In to Au contacts in amounts that exceed the solid solubility limit lowers the as-fabricated (unsintered) contact resistivity (R sub c) to the 10(exp -5) ohm cm(exp 2) range. We next consider the contact system Au/Au2P3 which has been shown to exhibit as-fabricated R sub c values in the 10(exp -6) ohm cm(exp 2) range, but which fails quickly when heated. We show that the substitution of a refractory metal (W, Ta) for Au preserves the low R sub c values while preventing the destructive reactions that would normally take place in this system at high temperatures. We show, finally, that R sub c values in the 10(exp -7) ohm cm(exp 2) range can be achieved without sintering by combining the effects of In or Ga additions to Au contacts with the effects of introducing a thin Au2P3 layer at the metal-InP interface.

Weizer, Victor G.↗
NASA NTRS2013

Erosion, Transportation, and Deposition on Outer Solar System Satellites: Landform Evolution Modeling Studies

Mass movement and landform degradation reduces topographic relief by moving surface materials to a lower gravitational potential. In addition to the obvious role of gravity, abrasive mechanical erosion plays a role, often in combination with the lowering of cohesion, which allows disaggregation of the relief-forming material. The identification of specific landform types associated with mass movement and landform degradation provides information about local sediment particle size and abundance and transportation processes. Generally, mass movements can be classified in terms of the particle sizes of the transported material and the speed the material moved during transport. Most degradation on outer planet satellites appears consistent with sliding or slumping, impact erosion, and regolith evolution. Some satellites, such as Callisto and perhaps Hyperion and Iapetus, have an appearance that implies that some additional process is at work, most likely sublimation-driven landform modification and mass wasting. A variant on this process is thermally driven frost segregation as seen on all three icy Galilean satellites and perhaps elsewhere. Titan is unique among outer planet satellites in that Aeolian and fluvial processes also operate to erode, transport, and deposit material. We will evaluate the sequence and extent of various landform-modifying erosional and volatile redistribution processes that have shaped these icy satellites using a 3-D model that simulates the following surface and subsurface processes: 1) sublimation and re-condensation of volatiles; 2) development of refractory lag deposits; 3) disaggregation and downward sloughing of surficial material; 4) radiative heating/cooling of the surface (including reflection, emission, and shadowing by other surface elements); 5) thermal diffusion; and 6) vapor diffusion. The model will provide explicit simulations of landform development and thusly predicts the topographic and volatile evolution of the surface and final landscape form as constrained by DEMs. We have also simulated fluvial and lacustrine modification of icy satellites landscapes to evaluate the degree to which fluvial erosion of representative initial landscapes can replicate the present Titan landscape.

erosion↗
NASA NTRS2001

Effectiveness of Diffusion Barrier Coatings for Mo-Re Embedded in C/SiC and C/C

Advanced high-temperature cooling applications may often require the elevated-temperature capability of carbon/silicon carbide or carbon/carbon composites in combination with the hermetic capability of metallic tubes. In this paper, the effects of C/SiC and C/C on tubes fabricated from several different refractory metals were evaluated. Though Mo, Nb, and Re were evaluated in the present study, the primary effort was directed toward two alloys of Mo-Re, namely, arc cast Mo-41Re and powder metallurgy Mo-47.5Re. Samples of these refractory metals were subjected to either the PyC/SiC deposition or embedding in C/C. MoSi2(Ge), R512E, and TiB2 coatings were included on several of the samples as potential diffusion barriers. The effects of the processing and thermal exposure on the samples were evaluated by conducting burst tests, microhardness surveys, and scanning electron microscopic examination (using either secondary electron or back scattered electron imaging and energy dispersive spectroscopy). The results showed that a layer of brittle Mo-carbide formed on the substrates of both the uncoated Mo-41Re and the uncoated Mo-47.5Re, subsequent to the C/C or the PyC/SiC processing. Both the R512E and the MoSi2(Ge) coatings were effective in preventing not only the diffusion of C into the Mo-Re substrate, but also the formation of the Mo-carbides. However, none of the coatings were effective at preventing both C and Si diffusion without some degradation of the substrate.

Glass, David E.↗